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1. Exploring the response to a new range of ethanol reductions in Chardonnay and Syrah wines using a Consumer Rejection Threshold approach

Author

Olivier Geffroy, Grégory Pasquier, Marielle Pagès, and Frédéric Violleau

Subjects
ethanol perception, difference threshold, consumer rejection threshold, Chardonnay wine, Syrah wine, spinning cone column, Agriculture, Botany, QK1-989
Abstract

Ethanol is one of the major components of wine, which has a substantial impact on its sensory characteristics. However, data concerning consumer response to ethanol or changes in ethanol remains limited. The aim of this study was to determine the threshold ethanol concentrations beyond which ethanol lowering becomes undesirable in Chardonnay and Syrah wines using the consumer rejection threshold (CRT) methodology. Base wines from these two cultivars were first dearomatised and fully dealcoholised using spinning cone column technology. Then, control wines with a similar ethanol content to the base wines (13.8 and 13.5 % v/v for Chardonnay and Syrah respectively) and wines with lower ethanol contents were reconstituted by mixing the final beverage, the aroma fraction, food grade ethanol and distilled water. CRT values were determined as 2.8 % v/v for Chardonnay and at 7.0 % v/v for Syrah. These particularly low and unexpected concentrations indicate that consumer sensory liking might not be necessarily driven by ethanol concentration, especially for white wines. However, the post-evaluation questionnaire showed that consumers were expecting a high minimal ethanol content for quality wines (10.9 % v/v ± 1.2 and 11.7 % v/v ± 1.5 for white and red wines respectively) and had a limited experience with low and dealcoholised wines. Overall, our data, which are still preliminary and deserve to be validated using different base wines with a larger number of consumers, show that consumers would not necessarily be refractory from a sensory standpoint to the consumption of low ethanol beverages made from wine. Our findings strongly encourage professionals from the wine industry and public authorities to raise awareness about the increase in quality of such products and their benefits for human health.

Published
2022
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2. Characterization of Non-Derivatized Cellulose Samples by Size Exclusion Chromatography in Tetrabutylammonium Fluoride/Dimethylsulfoxide (TBAF/DMSO)

Author

Jérémy Rebière, Antoine Rouilly, Vanessa Durrieu, and Frédéric Violleau

Subjects
cellulose, molar mass, SEC analysis, conventional calibration, Organic chemistry, QD241-441
Abstract

This paper deals with the use of tetrabutylammonium fluoride/dimethylsulfoxide (TBAF/DMSO) to characterize the molar mass distribution of non-derivatized cellulosic samples by size exclusion chromatography (SEC). Different cellulose samples with various average degree of polymerization (DP) were first solubilized in this solvent system, with increasing TBAF rates, and then analyzed by SEC coupled to a refractive index detector (RID), using DMSO as mobile phase. The Molar Masses (MM) obtained by conventional calibration were then discussed and compared with suppliers’ data and MM determined by viscosimetry measurements. By this non-classic method, molar mass of low DP samples (Avicel® and cotton fibers) have been determined. For high DP samples (α-cellulose and Vitacel®), dissolution with TBAF concentration of 10 mg/mL involved elution of cellulose aggregates in the exclusion volume, related to an incomplete dissolution or the dilution of TBAF molecules in elution solvent, preventing the correct evaluation of their molar mass.

Published
2017
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3. Drug Release by Direct Jump from Poly(ethylene-glycol-b-ε-caprolactone) Nano-Vector to Cell Membrane

Author

Ugo Till, Laure Gibot, Anne-Françoise Mingotaud, Jérôme Ehrhart, Luc Wasungu, Christophe Mingotaud, Jean-Pierre Souchard, Alix Poinso, Marie-Pierre Rols, Frédéric Violleau, and Patricia Vicendo

Subjects
polymer micelles, pheophorbide-a, cellular penetration, uptake mechanism, Organic chemistry, QD241-441
Abstract

Drug delivery by nanovectors involves numerous processes, one of the most important being its release from the carrier. This point still remains unclear. The current work focuses on this point using poly(ethyleneglycol-b-ε-caprolactone) micelles containing either pheophorbide-a (Pheo-a) as a fluorescent probe and a phototoxic agent or fluorescent copolymers. This study showed that the cellular uptake and the phototoxicity of loaded Pheo-a are ten times higher than those of the free drug and revealed a very low cellular penetration of the fluorescence-labeled micelles. Neither loaded nor free Pheo-a displayed the same cellular localization as the labeled micelles. These results imply that the drug entered the cells without its carrier and probably without a disruption, as suggested by their stability in cell culture medium. These data allowed us to propose that Pheo-a directly migrates from the micelle to the cell without disruption of the vector. This mechanism will be discussed.

Published
2016
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4. Assessment of structures in phosphocaseinate dispersions by A4F, NMR and SAXS: The impact of demineralization and heat treatment on viscosity

Author

Márcio H. Nogueira, Luisa A. Scudeler, Lucile Humblot, Bertrand Doumert, Marie Hennetier, Frédéric Violleau, Celine Lesur, Guillaume Delaplace, Paulo.P.S. Peixoto, Unité Matériaux et Transformations - UMR 8207 (UMET), Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT), Chimie Agro-Industrielle (CAI), Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques (ENSIACET), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), INGREDIA SA, F-62000 Arras, France, Partenaires INRAE, This study started with the phD Thesis of Marcio Nogueira (These Cifre financed by ANRT) within the frame of the project 'Proteinolab', a partnership between the Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE) and Ingredia Dairy Experts . Hence, this work has allowed some funds from French National Research Agency (ANR) allocated to the project 'Proteinolab' but also from the ANR-financed 'ProteinoPeps' project, which enable us to strenghten scientific discussion and to consolidate the results through acceding to other experimental facilitie, and ANR-17-LCV2-0005,Proteinolab,Laboratoire commun de caractérisation des structures-fonctions d'isolats protéiques différenciés(2017)

Subjects
Dense dispersions, Viscosity, General Chemical Engineering, [SDV]Life Sciences [q-bio], Ultra-high-temperature, General Chemistry, Demineralization, Casein micelles, Food Science
Abstract

International audience; The present work aims to better understand the relation between heat treatment (Ultra High Temperature - UHT), partial demineralization of casein micelles (CMs) dispersions and their corresponded rheological properties. A multiscale analysis (SAXS, solid state NMR and Asymmetrical Flow Field Flow Fractionation (A4F)), has been used. Different samples with different levels of calcium/phosphorous demineralization (up to −30% of calcium content) have been studied before and after UHT treatment. The present data show that CM dispersions, displaying a mild demineralization, display an important decrease in viscosity after UHT. NMR shows that, during UHT, mild demineralized samples display stronger calcium/phosphorus intake than both, the non-demineralized and the strong demineralized ones. SAXS and A4F show that UHT-dependent calcium intake, in mild demineralization dispersions, seems to be responsible for a transformation of large casein aggregates into small and denser ones. This decrease of the large aggregates is probably the main reason of the UHT-dependent decrease in viscosity. These data show that a sample with a rather small amount of demineralization can have a quite important susceptibility to UHT in terms of viscosity.

Published
2023

5. Ozone Dissolved in Water: An Innovative Tool for the Production of Young Plants in Grapevine Nurseries?

Author

Ana Romeo-Oliván, Frédéric Violleau, Alban Jacques, Hubert Cros, Olivier Yobregat, Coralie Breton, Fabien Lagarde, Marielle Pagès, Physiologie, Pathologie et Génétique Végétales (PPGV), INP-PURPAN, Université Fédérale Toulouse Midi-Pyrénées, Pépinères Daydé, Institut Français de la Vigne et du Vin (IFV), Chimie Agro-Industrielle (CAI), Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National Polytechnique (Toulouse) (Toulouse INP), and Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)

Subjects
0106 biological sciences, P. minimum, 0303 health sciences, Environmental Engineering, Ozone, [SDV]Life Sciences [q-bio], fungi, food and beverages, 01 natural sciences, Trunk, Fungicide, 03 medical and health sciences, Horticulture, Plant development, chemistry.chemical_compound, chemistry, fungicide, Environmental Chemistry, Environmental science, grapevine trunk diseases, plant development, P. chlamydospora, 030304 developmental biology, 010606 plant biology & botany
Abstract

International audience; Grapevine trunk diseases can infect nursery plants at different stages of propagation. Here, we evaluated the efficiency of aqueous ozone against two fungi associated with trunk diseases (Phaeoacremonium minimum and Phaeomoniella chlamydospora). The effect of ozone on the plant growth is also studied. Aqueous ozone completely suppressed spore germination in vitro. In planta fungal development was reduced six weeks post-inoculation. In the nursery, ozone treatment was comparable to the usual chemical treatment. Irrigation with aqueous ozone had no negative effects on plant growth. These anti-fungal properties and the absence of phytotoxicity make ozone a promising alternative for controlling microbial infection in nurseries.

Published
2021

6. High and low pathogenicity avian influenza virus discrimination and prediction based on volatile organic compounds signature by SIFT-MS: a proof-of-concept study

Author

Fabien Filaire, Aurélie Sécula, Pierre Bessière, Marielle Pagès-Homs, Jean-Luc Guérin, Frederic Violleau, and Ugo Till

Subjects
Volatile organic compounds, Avian influenza, Multivariate analysis, Virus, Infection, SIFT-MS, Medicine, Science
Abstract

Abstract High and low pathogenicity avian influenza viruses (HPAIV, LPAIV) are the primary causes of poultry diseases worldwide. HPAIV and LPAIV constitute a major threat to the global poultry industry. Therefore, early detection and well-adapted surveillance strategies are of the utmost importance to control the spread of these viruses. Volatile Organic Compounds (VOCs) released from living organisms have been investigated over the last decades as a diagnostic strategy. Mass spectrometry instruments can analyze VOCs emitted upon viral infection. Selected ion flow tube mass spectrometry (SIFT-MS) enables direct analysis of cell headspace in less than 20 min. As a proof-of-concept study, we investigated the ability of a SIFT-MS coupled sparse Partial Least Square-Discriminant Analysis analytical workflow to discriminate IAV-infected cells. Supernatants of HPAIV, LPAIV, and control cells were collected from 1 to 72 h post-infection and analyzed using our analytical workflow. At each collection point, VOCs' signatures were first identified based on four independent experiments and then used to discriminate the infectious status of external samples. Our results indicate that the identified VOCs signatures successfully discriminate, as early as 1-h post-infection, infected cells from the control cells and differentiated the HPAIV from the LPAIV infection. These results suggest a virus-dependent VOCs signature. Overall, the external samples' status was identified with 96.67% sensitivity, 100% specificity, and 97.78% general accuracy.

Published
2024
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7. Ozonation of three different fungal conidia associated with apple disease: Importance of spore surface and membrane phospholipid oxidation

Author

Didier Kleiber, Frédéric Violleau, Marielle Pagès, Ecole d'Ingénieurs de Purpan (INPT - EI Purpan), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées, Chimie Agro-Industrielle (CAI), Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), and BPIFrance, Grant/Award Number: F1206003M

Subjects
Ozone, [SDV]Life Sciences [q-bio], lcsh:TX341-641, [SDV.TOX.TCA]Life Sciences [q-bio]/Toxicology/Toxicology and food chain, 010501 environmental sciences, 01 natural sciences, 040501 horticulture, chemistry.chemical_compound, Spore germination, 0105 earth and related environmental sciences, Botrytis cinerea, Original Research, biology, Ascomycota, Chemistry, fungi, Venturia inaequalis, 04 agricultural and veterinary sciences, biology.organism_classification, Spore, Fungicide, Horticulture, Germination, 0405 other agricultural sciences, lcsh:Nutrition. Foods and food supply, Food Science
Abstract

Although ozone (O3) is a well‐known bactericide and fungicide, the required dose of ozone can depend significantly on the targeted pathogens. The present research evaluates the variation in sensibility to ozone of three fungal species from a single fungal group. The three fungal species selected, Venturia inaequalis, Botrytis cinerea, and Neofabreae alba, belong to the Ascomycota group and attack apples. The fungi were exposed to ozone by bubbling directly into the spore solutions (treatment period ranged from 0.5 to 4 min, ozone concentration in inlet gas ranged from 1 to 30 g/m3). The rates of germination were determined, and the level of peroxidation of the lipid membrane was quantified based on the malondialdehyde (MDA) production. The results indicate that ozone effectively reduces spore development and suggest that the fungi differ in sensitivity. To reduce by 50% the spore germination rate of N. alba, B. cinerea, and V. inaequalis requires ozone doses of 0.01, 0.03, and 0.07 mg/ml, respectively. Spore sensitivity seems to be directly linked to spore surface. For all the fungal species, the MDA level and the level of spore inactivation both increase with ozone dose, which confirms that ozone alters the cell membrane., Although ozone (O3) is a well‐known bactericide and fungicide, the required dose of ozone can depend significantly on the targeted pathogens. Thanks our results, spore sensitivity seems to be directly linked to spore surface. For all the fungal species, the MDA level and the level of spore inactivation both increase with ozone dose, which confirms that ozone alters the cell membrane.

Published
2020

8. Study of the relationship between red wine colloidal fraction and astringency by asymmetrical flow field-flow fractionation coupled with multi-detection

Author

Cecile Levasseur-Garcia, Véronique Cheynier, Kevin Pascotto, Coline Leriche, Jean-Claude Boulet, Frédéric Violleau, Olivier Geffroy, Soline Caillé, Chimie Agro-Industrielle (CAI), Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Unité Expérimentale de Pech-Rouge (PECH ROUGE), Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Sciences Pour l'Oenologie (SPO), Université de Montpellier (UM)-Institut national d’études supérieures agronomiques de Montpellier (Montpellier SupAgro), Institut national d'enseignement supérieur pour l'agriculture, l'alimentation et l'environnement (Institut Agro)-Institut national d'enseignement supérieur pour l'agriculture, l'alimentation et l'environnement (Institut Agro)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Ecole d'Ingénieurs de Purpan (INPT - EI Purpan), Institut National Polytechnique (Toulouse) (Toulouse INP), and Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées

Subjects
AF4-UV-MALS-dRI, Astringency, [SDV]Life Sciences [q-bio], Fraction (chemistry), Wine, 01 natural sciences, Analytical Chemistry, Chemometrics, Absorbance, Colloid, 0404 agricultural biotechnology, Polysaccharides, [CHIM]Chemical Sciences, Proanthocyanidins, Colloids, Chromatography, Chemistry, 010401 analytical chemistry, Polyphenols, 04 agricultural and veterinary sciences, General Medicine, 040401 food science, Fractionation, Field Flow, 0104 chemical sciences, Proanthocyanidin, Macromolecules, Polyphenol, Taste, Principal component analysis, [SDV.AEN]Life Sciences [q-bio]/Food and Nutrition, Food Science
Abstract

International audience; Macromolecules including condensed tannins and polysaccharides impact wine taste and especially astringency. Asymmetrical Flow-Field-Flow-Fractionation (AF4) coupled to UV detection (UV), multi-angle light scattering (MALS) and refractive index detection (dRI) has been proposed to separate red wine colloids. The present work aimed at relating AF4-mutidetection profiles with red wine astringency. Fifty commercial red wines characterized by a trained sensory panel were analysed by AF4-UV-MALS-dRI and UV & ndash;visible spectroscopy. The analytical data set was built by selecting the three variables most predictive of the astringency score from each table (UV, dRI, MALS, Mw distribution, and UV & ndash;visible spectra of whole wine, permeate and retentate A4F fractions) and analysed by principal component analysis. Red wine astringency was more related to variables extracted from the AF4 data than to UV- absorbance of the wine or permeate, confirming the relevance of AF4-multidetection for analysis of the colloidal fraction involved in this perception.

Published
2021

9. Ozonized 2-hydroxypropyl-β-cyclodextrins as novel materials with oxidative and bactericidal properties

Author

Elsi, Haddad, Marielle, Pagès, Frédéric, Violleau, Olivier, Marsan, Marie-Hélène, Manero, Romain, Richard, and Jean-Philippe, Torré

Subjects
Cyclodextrins, Oxidative Stress, Polymers and Plastics, beta-Cyclodextrins, Organic Chemistry, Materials Chemistry, Oxidation-Reduction, 2-Hydroxypropyl-beta-cyclodextrin
Abstract

Ozonized (2-Hydroxypropyl)-β-cyclodextrins (Oz-HPbCDs) were produced by direct gas/solid reaction between gaseous ozone (O

Published
2022

10. Iodine and Peroxide Index Rapid Determination by Mid- and Near-infrared Spectroscopy in Ozonated Sunflower Oil and Ozonated Fats

Author

A. Calmon, Cecile Levasseur-Garcia, S. Tréguier, Julien Vinet, Frédéric Violleau, Chimie Agro-Industrielle (CAI), Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Terres Inovia, Ecole d'Ingénieurs de Purpan (INPT - EI Purpan), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées, and Occitanie Region and the EI Purpan for funding by Grant No. 15066413.

Subjects
ozonated sunflower oil, Environmental Engineering, food.ingredient, Ozone, [SDV]Life Sciences [q-bio], Infrared spectroscopy, chemistry.chemical_element, 02 engineering and technology, 010501 environmental sciences, Iodine, 01 natural sciences, Peroxide, Chemometrics, chemistry.chemical_compound, food, 020401 chemical engineering, Environmental Chemistry, iodine index, 0204 chemical engineering, infrared spectroscopy, 0105 earth and related environmental sciences, ozonated fat compounds, Chemistry, Sunflower oil, Near-infrared spectroscopy, food and beverages, chemometrics, quantification, peroxide index, 13. Climate action, Antibacterial activity, Nuclear chemistry
Abstract

International audience; Ozone can react with fatty species such as vegetable oils to form oxidized compounds with interesting antibacterial activity. The iodine and peroxide indexes of these ozonated products are two crucial antibacterial characteristics. Currently, these two parameters are determined by chemical methods, which is disadvantageous because it requires long handling time, sample destruction and the use of toxic products. Spectroscopic analyses coupled with chemometric evaluations have already shown their usefulness for characterizing virgin oils via rapid, chemical-free methods. In addition, infrared spectroscopy is widely used to characterize ozonated compounds. The present study evaluates the possibility of coupling infrared spectroscopy with chemical analyses of ozonated compounds. We subjected 187 fat samples of varying compositions to different ozonation conditions to determine their chemical parameters. We analyzed the samples by infrared spectroscopy and modeled the results by combining chemical data with spectral analysis. The model results are quantified by the coefficient of determination R-2, the root-mean-square error, and the residual predictive deviation (RPD). The model produces RPDs greater than 3.5 for the mid-infrared spectral range, which means that they may be used to estimate indexes. In addition, with RPDs between 2 and 3, partial least squares near-infrared models demonstrate a capacity for rough screening of ozonated fats.

Published
2021

11. Prediction and detection of human epileptic seizures based on SIFT-MS chemometric data

Author

Frédéric Violleau, Hugo Cousillas, Amélie Catala, Martine Hausberger, Cecile Levasseur-Garcia, Jean-Luc Schaff, Marine Grandgeorge, Ugo Till, Leticia Vitola Pasetto, Marielle Pagès, Association Nationale d'Education de Chiens d'Assistance pour Handicapés (Handi'chiens), Ethologie animale et humaine (EthoS), Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Normandie Université (NU)-Université de Rennes 1 (UR1), Université de Rennes (UNIV-RENNES)-Université de Rennes (UNIV-RENNES)-Centre National de la Recherche Scientifique (CNRS), Chimie Agro-Industrielle (CAI), Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Physiologie Pathologie et Génétique Végétales (PPGV), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées, Centre Hospitalier Régional Universitaire de Nancy (CHRU Nancy), 2016/1171, Association Nationale de la Recherche et de la Technologie, Normandie Université (NU)-Normandie Université (NU)-Université de Rennes (UR)-Centre National de la Recherche Scientifique (CNRS), Handi'Chiens, Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques (ENSIACET), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Physiologie, Pathologie et Génétique Végétales (PPGV), Ecole d'Ingénieurs de Purpan (INP - PURPAN), Université de Toulouse (UT)-Université de Toulouse (UT), and Centre Hospitalier de Laval (CH Laval)

Subjects
[SDV]Life Sciences [q-bio], Scale-invariant feature transform, lcsh:Medicine, Electroencephalography, Sensitivity and Specificity, 01 natural sciences, Article, 03 medical and health sciences, Epilepsy, 0302 clinical medicine, Seizures, medicine, Humans, lcsh:Science, Volatile Organic Compounds, Multidisciplinary, medicine.diagnostic_test, Mass spectrometry, business.industry, 010401 analytical chemistry, lcsh:R, Reproducibility of Results, Ethology, Pattern recognition, medicine.disease, 3. Good health, 0104 chemical sciences, Breath Tests, Odorants, lcsh:Q, Artificial intelligence, business, 030217 neurology & neurosurgery, Biomarkers, [SDV.MHEP]Life Sciences [q-bio]/Human health and pathology
Abstract

Although epilepsy is considered a public health issue, the burden imposed by the unpredictability of seizures is mainly borne by the patients. Predicting seizures based on electroencephalography has had mixed success, and the idiosyncratic character of epilepsy makes a single method of detection or prediction for all patients almost impossible. To address this problem, we demonstrate herein that epileptic seizures can not only be detected by global chemometric analysis of data from selected ion flow tube mass spectrometry but also that a simple mathematical model makes it possible to predict these seizures (by up to 4 h 37 min in advance with 92% and 75% of samples correctly classified in training and leave-one-out-cross-validation, respectively). These findings should stimulate the development of non-invasive applications (e.g., electronic nose) for different types of epilepsy and thereby decrease of the unpredictability of epileptic seizures.

Published
2020

12. Structural characterization of heat-induced protein aggregates in model infant milk formulas

Author

Amélie Deglaire, Thomas Croguennec, Marie Hennetier, Amira Halabi, Didier Dupont, Frédéric Violleau, Agnès Burel, Saïd Bouhallab, Science et Technologie du Lait et de l'Oeuf (STLO), Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-AGROCAMPUS OUEST, Institut national d'enseignement supérieur pour l'agriculture, l'alimentation et l'environnement (Institut Agro)-Institut national d'enseignement supérieur pour l'agriculture, l'alimentation et l'environnement (Institut Agro), Ecole d'Ingénieurs de Purpan (INPT - EI Purpan), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées, Biosit : biologie, santé, innovation technologique (SFR UMS CNRS 3480 - INSERM 018), Université de Rennes 1 (UR1), Université de Rennes (UNIV-RENNES)-Université de Rennes (UNIV-RENNES)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Structure Fédérative de Recherche en Biologie et Santé de Rennes ( Biosit : Biologie - Santé - Innovation Technologique ), ARED 17-032Institut National de Recherche en Sciences et Technologies pour l'Environnement et l'Agriculture, IRSTEA, AGROCAMPUS OUEST, Institut national d'enseignement supérieur pour l'agriculture, l'alimentation et l'environnement (Institut Agro)-Institut national d'enseignement supérieur pour l'agriculture, l'alimentation et l'environnement (Institut Agro)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-INSTITUT AGRO Agrocampus Ouest, Université de Toulouse (UT)-Université de Toulouse (UT), and Université de Rennes (UR)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Structure Fédérative de Recherche en Biologie et Santé de Rennes ( Biosit : Biologie - Santé - Innovation Technologique )

Subjects
Whey protein, animal structures, General Chemical Engineering, [SDV]Life Sciences [q-bio], Multiangle light scattering, Fractionation, Protein aggregation, Casein micelles, 01 natural sciences, Micelle, 0404 agricultural biotechnology, Protein structure, Casein, 0103 physical sciences, [SDV.IDA]Life Sciences [q-bio]/Food engineering, Denaturation (biochemistry), Chromatography, 010304 chemical physics, Chemistry, food and beverages, 04 agricultural and veterinary sciences, General Chemistry, 040401 food science, Lactoferrin, Heat-induced modifications, Infant formula, Whey proteins, [SDV.AEN]Life Sciences [q-bio]/Food and Nutrition, Food Science
Abstract

International audience; Heat treatments induce structural modifications of bovine milk proteins. In this study, we aimed to investigate how these structural modifications are affected by the whey protein profile of infant milk formulas (IMFs) and heat treatment parameters. Three model IMFs (1.3% of proteins; caseinwhey protein ratio 4060) differing by the whey protein profile (13.37 α-lactalbumin (α-LA)β-lactoglobulin (β-LG), 13.261.80 α-LAβ-LGlactoferrin (LF) or 10.130.40 α-LAβ-LGLF), were heated at 67.5 °C or 80 °C to reach an akin whey protein denaturation extent of 65%. Protein structures were analyzed by asymmetrical flow field-flow fractionation coupled with multiangle light scattering and differential refractometer, transmission electron microscopy and electrophoresis. The unheated IMFs were used as reference. The results showed that LF addition in IMFs induced partial casein micelle disintegration before heating. In the absence of added LF, the heat-denatured whey proteins either formed soluble whey protein aggregates or casein micelle-bound whey protein aggregates. The latter were favored at the expense of soluble aggregates in the heated IMFs with the LF content increase and the concomitant β-LG content decrease. Consequently, the casein micelle structure was strongly dependent on the β-LG and LF amounts in IMFs and on the heating temperature. In the IMFs containing β-LG and LF and at temperature greater than the β-LG denaturation temperature, the casein micelles exhibited filamentous appendages on its surface after heating. Below the denaturation temperature of β-LG and in IMFs containing trace β-LG amount, the heated casein micelles were perfectly spherical with a smooth surface. © 2020 Elsevier Ltd

Published
2020

13. Sudden Decrease of the Dissolved Ozone Concentration in Sprays: A Mass Transfer Phenomenon?

Author

Wilfried Remus-Borel, Axel Canado, Marielle Pagès, Marine Tournois, Michel Roustan, Gilles Hébrard, Nicolas Dietrich, Frédéric Violleau, Chimie Agro-Industrielle (CAI), Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques (ENSIACET), Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Toulouse Biotechnology Institute (TBI), Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Physiologie, Pathologie et Génétique Végétales (PPGV), Ecole d'Ingénieurs de Purpan (INP - PURPAN), Université de Toulouse (UT)-Université de Toulouse (UT), Belchim Crop Protection France, This research belongs to the SOLSTICE project supported by the French state within the framework of 'Programme d'Investissements d'Avenir'., Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Physiologie, Pathologie et Génétique Végétales (PPGV), INP-PURPAN, Université Fédérale Toulouse Midi-Pyrénées, Ecole d'Ingénieurs de Purpan (INPT - EI Purpan), and Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées

Subjects
Ozone, [SDV.BIO]Life Sciences [q-bio]/Biotechnology, Ozone concentration, General Chemical Engineering, 02 engineering and technology, General Chemistry, 021001 nanoscience & nanotechnology, Industrial and Manufacturing Engineering, Persistence (computer science), chemistry.chemical_compound, 020401 chemical engineering, chemistry, 13. Climate action, Mass transfer, Environmental chemistry, [SPI.GPROC]Engineering Sciences [physics]/Chemical and Process Engineering, 0204 chemical engineering, 0210 nano-technology
Abstract

International audience; Ozone is known to be a powerful oxidant with low persistence and has been shown to possess biocidal activity against a wide number of fungi and bacteria. These properties make ozone a good candidate as a substitute for chemical phytosanitary products in agriculture. However, when water containing dissolved ozone is sprayed, the concentration of ozone decreases dramatically with spraying distance. This study aims to better understand this ozone loss during spraying and, in particular, to identify whether mass transfer occurs. Identification was performed by dioxygen absorption and comparison of its concentration profiles with those for ozone desorption. Droplets were collected at different heights in the spray to measure the dissolved concentrations. Image analysis was used to determine the diameters and velocities of the droplets. Ozone self-decomposition kinetics were not able to explain the experimental concentration variation obtained in the droplets. The decrease of dissolved ozone in the liquid is then only caused by mass transfer. Most of the mass transfer seems to take place in the liquid sheet that leaves the nozzle. Volumetric mass transfer coefficients have been assessed for different regions of the spray. From mass transfer correlations, a model has been made to predict the concentration profile in droplets of the spray.

Published
2020

14. Insight into gluten structure in a mild chaotropic solvent by asymmetrical flow field-flow fractionation (AsFlFFF) and evidence of non-covalent assemblies between glutenin and ω-gliadin

Author

Marie-Hélène Morel, Ameur Louhichi, Frédéric Violleau, Paul Menut, Laurence Ramos, Amélie Banc, Justine Pincemaille, Edouard Chauveau, Ingénierie des Agro-polymères et Technologies Émergentes (UMR IATE), Centre de Coopération Internationale en Recherche Agronomique pour le Développement (Cirad)-Université Montpellier 2 - Sciences et Techniques (UM2)-Centre international d'études supérieures en sciences agronomiques (Montpellier SupAgro)-Université de Montpellier (UM)-Institut national d’études supérieures agronomiques de Montpellier (Montpellier SupAgro)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Laboratoire Charles Coulomb (L2C), Centre National de la Recherche Scientifique (CNRS)-Université de Montpellier (UM), Ecole d'Ingénieurs de Purpan (INPT - EI Purpan), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées, Paris-Saclay Food and Bioproduct Engineering (SayFood), AgroParisTech-Université Paris-Saclay-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Centre de Coopération Internationale en Recherche Agronomique pour le Développement (Cirad)-Centre international d'études supérieures en sciences agronomiques (Montpellier SupAgro)-Université de Montpellier (UM)-Institut national d’études supérieures agronomiques de Montpellier (Montpellier SupAgro), Institut national d'enseignement supérieur pour l'agriculture, l'alimentation et l'environnement (Institut Agro)-Institut national d'enseignement supérieur pour l'agriculture, l'alimentation et l'environnement (Institut Agro)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Université de Montpellier (UM)-Centre National de la Recherche Scientifique (CNRS), Chimie Agro-Industrielle (CAI), Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Doctoral School GAIA and the Labex Numev (ANR-10-LAB-20) for the funding of the PhD Grant, scientific council of Montpellier SupAgro, and ANR-18-CE06-0012,ELASTOBIO,Gels élastomériques de biopolymères soumis à des déformations extrêmes(2018)

Subjects
chemistry.chemical_classification, Molar mass, 010304 chemical physics, biology, General Chemical Engineering, Size-exclusion chromatography, food and beverages, 04 agricultural and veterinary sciences, General Chemistry, Polymer, 040401 food science, 01 natural sciences, Gluten, [CHIM.THEO]Chemical Sciences/Theoretical and/or physical chemistry, Chaotropic agent, 0404 agricultural biotechnology, Glutenin, chemistry, Dynamic light scattering, Chemical engineering, 0103 physical sciences, biology.protein, Gliadin, [SDV.AEN]Life Sciences [q-bio]/Food and Nutrition, Food Science
Abstract

International audience; Wheat gluten, one of the most complex viscoelastic protein networks in nature, is unique to get the specific texture of bread. Due to its complex protein composition, its insolubility in most solvents and the very high molar mass of half of the proteins (glutenin, the other half being gliadin), the architecture of the network is still not well understood. In this work, we have investigated model gluten protein extracts with contrasted compositions in glutenin and gliadin solubilized in a mild chaotropic solvent: ethanol/water (50/50 v/v). The samples display a liquid-liquid phase separation with an upper critical solution temperature that depends on the protein composition. The phase diagrams are consistent with the presence of supramolecular assemblies of proteins. To confirm the presence of these assemblies and fully characterize the objects dispersed in ethanol/water, we have used an asymmetrical flow field-flow fractionation (AsFlFFF) setup coupled with differential refractive index, multi-angle light scattering and dynamic light scattering detections to probe very dilute protein suspensions. We have identified three classes of objects, with distinctive molar mass, characteristic size and conformation: protein monomers, polymeric structures, and very loose protein assemblies with molar mass larger than 2.10 6 g/mol. A molecular characterization of the species by size exclusion chromatography in a denaturing solvent shows that polymers and assemblies are mainly composed of glutenin and ω-gliadin. The high content of ω-gliadin, devoid of cysteines, indicates the importance of non-covalent interactions involved in protein assemblies and might play a major role in gluten rheology

Published
2020

15. A catalyst-free process for gas ozonation of reduced sulfur compounds

Author

Leticia Vitola Pasetto, Jean-Stéphane Pic, Frédéric Violleau, Romain Richard, Valérie Simon, Marie-Hélène Manero, Centre National de la Recherche Scientifique - CNRS (FRANCE), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Institut National de la Recherche Agronomique - INRA (FRANCE), Institut National des Sciences Appliquées de Toulouse - INSA (FRANCE), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), Chimie Agro-Industrielle (CAI), Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Laboratoire de Génie Chimique (LGC), Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS), Toulouse Biotechnology Institute (TBI), Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Agro Innovation International CIFRE 2015/1233, French National Agency for Research and Technology, Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques (ENSIACET), Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Université de Toulouse (UT)-Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT), and Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)

Subjects
Ozone, SIFT/MS, Sulfide, General Chemical Engineering, Hydrogen sulfide, Inorganic chemistry, chemistry.chemical_element, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, Industrial and Manufacturing Engineering, Catalysis, chemistry.chemical_compound, [CHIM.GENI]Chemical Sciences/Chemical engineering, Homogenous ozonation, Environmental Chemistry, Génie chimique, Dimethyl disulfide, [SPI.GPROC]Engineering Sciences [physics]/Chemical and Process Engineering, Génie des procédés, Sulfur dioxide, chemistry.chemical_classification, Gas treatment, General Chemistry, Doehlert design, 021001 nanoscience & nanotechnology, Sulfur, 0104 chemical sciences, chemistry, 13. Climate action, Reagent, Odor compounds, 0210 nano-technology
Abstract

International audience; The feasibility of homogenous gas ozonation process was investigated in order to reduce the negative environmental impact caused by reduced sulfur compounds (RSCs). Emitted from a variety of industrial plants, this class of compounds are known by their odor properties. Selecting hydrogen sulfide (H2S), methyl ethyl sulfide (MES) and dimethyl disulfide (DMDS) as representative odorous RSCs, the influence of four gas ozonation process parameters (ozone concentration, humidity level, reactor temperature and residence time) on their removal efficiencies was evaluated using a Doehlert experimental design in an experimental domain compatible with industrial constraints. Ozone concentration was the only process parameter that has resulted in a positive – but limited – effect on the removal efficiency of the mix of RSCs. However, even if ozone was present in large excess (20 times the RSCs concentration), MES and DMDS were slightly consumed (around 30%). Only H2S has shown interesting removal efficiencies (up to 80%). In addition to the measurement of reagent concentrations, Selected Ion Flow Tube coupled with Mass Spectrometry (SIFT/MS) was applied to identify and quantify the potential products of RSCs-ozone reaction. Methyl ethyl sulfone (MESO2) was found to be the primary product of MES, whereas methyl methanethiosulfinate (DMSOS) and sulfur dioxide (SO2) for DMDS, suggesting that the organic monosulfide and disulfides would not follow the same reaction mechanism with ozone in gas phase. In addition, SO2 and H2O may not be the only end products for H2S ozonation, since additional peaks were detected in SIFT/MS spectra

Published
2020

16. Hydrogen sulphide quantification by SIFT/MS: highlighting the influence of gas moisture

Author

Marie-Hélène Manero, Romain Richard, Jean-Stéphane Pic, Leticia Vitola Pasetto, Frédéric Violleau, Valérie Simon, Chimie Agro-Industrielle (CAI), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National de la Recherche Agronomique (INRA), Laboratoire de Génie Chimique (LGC), Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS), Toulouse Biotechnology Institute (TBI), Institut National de la Recherche Agronomique (INRA)-Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), French National Agency for Research and Technology and Agro Innovation International, Institut National de la Recherche Agronomique (INRA)-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques (ENSIACET), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Université de Toulouse (UT), Université de Toulouse (UT)-Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS), Laboratoire de Chimie Agro-Industrielle (LCA), Institut National de la Recherche Agronomique (INRA)-Ecole Nationale Supérieure de Chimie de Toulouse, Centre National de la Recherche Scientifique - CNRS (FRANCE), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Institut National de la Recherche Agronomique - INRA (FRANCE), Institut National des Sciences Appliquées de Toulouse - INSA (FRANCE), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), and Institut National Polytechnique de Toulouse - INPT (FRANCE)

Subjects
Materials science, Health, Toxicology and Mutagenesis, Analytical chemistry, Soil Science, chemistry.chemical_element, Selected ion flow tube mass spectrometry, 010501 environmental sciences, Mass spectrometry, 01 natural sciences, Analytical Chemistry, Chemical ionisation mass spectrometry, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, Hydrogen sulphide, Génie chimique, Environmental Chemistry, Génie des procédés, Waste Management and Disposal, Water content, 0105 earth and related environmental sciences, Water Science and Technology, Moisture, [SDE.IE]Environmental Sciences/Environmental Engineering, 010401 analytical chemistry, Public Health, Environmental and Occupational Health, Water interference, equipment and supplies, Pollution, Nitrogen, 0104 chemical sciences, chemistry, 13. Climate action, Measurement uncertainty, Selected-ion flow-tube mass spectrometry, Saturation (chemistry), Water vapor
Abstract

International audience; The quantification of hydrogen sulphide (H2S) by Selected Ion Flow Tube coupled with Mass Spectrometry (SIFT/MS) was investigated for application in industrial emission context, usually faced with concentrations of water vapour higher than the saturation at room condition. H2S concentrations measured by SIFT/MS (using nitrogen as carrier gas and flow tube temperature at 119°C) were affected by water content, reducing the sensibility for H2S measurements. Accurate concentrations were obtained when the influence of water was considered on SIFT/MS analysis, requiring although the information about water content in the sample. In addition, the association of low concentration of H2S (around 50 ppbv) and high humidity level (4.0 %vol of water) was highlighted as a critical point for measuring H2S by SIFT/MS, due to the sensibility reduction as function of water content and the measurement uncertainty enhancement at low signal intensity.

Published
2020

17. Using near-infrared spectroscopy to determine moisture content, gel strength, and viscosity of gelatin

Author

Cecile Levasseur-Garcia, Frédéric Violleau, Didier Kleiber, Carlos Vaca-Garcia, Christine Raynaud, Satoru Tsuchikawa, Simon Duthen, Jean Daydé, Ecole d'Ingénieurs de Purpan (INPT - EI Purpan), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées, Chimie Agro-Industrielle (CAI), Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Physiologie, Pathologie et Génétique Végétales (PPGV), INP-PURPAN, Université Fédérale Toulouse Midi-Pyrénées, Graduate School of Bioagricultural Sciences, Nagoya University, Centre d’Application et de Traitement des AgroRessources [Toulouse] (CRT CATAR), and This work was supported by Région Midi-Pyrénées (France) [Grant No. DESR/12050967 ] and by Université Fédérale de Toulouse Midi-Pyrénées (funding for international mobility) .

Subjects
Materials science, food.ingredient, [SDV]Life Sciences [q-bio], General Chemical Engineering, engineering.material, 01 natural sciences, Gelatin, Viscosity, 0404 agricultural biotechnology, food, [SDV.IDA]Life Sciences [q-bio]/Food engineering, 0103 physical sciences, Gel strength, Spectroscopy, Infrared spectroscopy, Water content, Moisture, 010304 chemical physics, Near-infrared spectroscopy, Analytical technique, 04 agricultural and veterinary sciences, General Chemistry, 040401 food science, Regression, Integrating sphere, Chemical engineering, engineering, Biopolymer, Food Science
Abstract

International audience; Gelatin is a natural biopolymer obtained by denaturation and partial hydrolysis of fibrous collagen, which is a fibrous protein present in the connective tissues of all species in the animal kingdom. Gelatin is used in many different industries, such as food, pharmaceuticals, photography, and cosmetics. The control of its physical properties is therefore of primary economic and technical importance for the gelatin industry, in particular because drying gelatin is the most expensive step in the manufacturing process and because customers demand products with well-controlled moisture content, gel strength, and viscosity. Consequently, a tool that provides rapid and nondestructive, real time analysis of gelatin would provide a definite competitive advantage. One such tool may be near-infrared (NIR) spectroscopy, which is a well-known analytical technique to determine the moisture content of complex matrices. We therefore use this technique to determine the moisture content, gel strength, and viscosity of 135 industrial gelatins. NIR spectra were acquired by using in reflectance mode a Fourier-transform NIR spectrometer with an integrating sphere to make a chemometric study of the industrial gelatins to determine the accuracy with which this technique can estimate moisture content, gel strength, and viscosity. The predictive accuracy for these parameters is quantified by using the ratio of performance of deviation (RPD), which gives 8.8, 3.7, and 2.1 in cross-validation, and 3.9, 1.8, and 1.9 in testing, respectively. Finally, we discuss the use of this technique in industrial conditions.

Published
2021

18. Tackling the question of specific interactions in a complex blend of proteins: the gluten case

Author

Amélie Banc, Justine Pincemaille, Frédéric Violleau, Paul Menut, Laurence Ramos, Marie Helene Morel, Laboratoire Charles Coulomb (L2C), Université de Montpellier (UM)-Centre National de la Recherche Scientifique (CNRS), Chimie Agro-Industrielle (CAI), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National de la Recherche Agronomique (INRA), Paris-Saclay Food and Bioproduct Engineering (SayFood), AgroParisTech-Université Paris-Saclay-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Ingénierie des Agro-polymères et Technologies Émergentes (UMR IATE), Institut national d’études supérieures agronomiques de Montpellier (Montpellier SupAgro), Institut national d'enseignement supérieur pour l'agriculture, l'alimentation et l'environnement (Institut Agro)-Institut national d'enseignement supérieur pour l'agriculture, l'alimentation et l'environnement (Institut Agro)-Centre de Coopération Internationale en Recherche Agronomique pour le Développement (Cirad)-Centre international d'études supérieures en sciences agronomiques (Montpellier SupAgro)-Université Montpellier 2 - Sciences et Techniques (UM2)-Université de Montpellier (UM)-Institut National de la Recherche Agronomique (INRA), Centre National de la Recherche Scientifique (CNRS)-Université de Montpellier (UM), Laboratoire de Chimie Agro-Industrielle (LCA), Ecole Nationale Supérieure de Chimie de Toulouse-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Institut national d’études supérieures agronomiques de Montpellier (Montpellier SupAgro)-Centre de Coopération Internationale en Recherche Agronomique pour le Développement (Cirad)-Centre international d'études supérieures en sciences agronomiques (Montpellier SupAgro)-Université Montpellier 2 - Sciences et Techniques (UM2)-Université de Montpellier (UM)-Institut National de la Recherche Agronomique (INRA), and Aigle, L2c

Subjects
[SDV.AEN] Life Sciences [q-bio]/Food and Nutrition, nutritional and metabolic diseases, food and beverages, [PHYS.COND.CM-SCM]Physics [physics]/Condensed Matter [cond-mat]/Soft Condensed Matter [cond-mat.soft], [SDV.AEN]Life Sciences [q-bio]/Food and Nutrition, [PHYS.COND.CM-SCM] Physics [physics]/Condensed Matter [cond-mat]/Soft Condensed Matter [cond-mat.soft]
Abstract

International audience; Natural protein sources often display a huge complexity, being composed of a blend of polypeptides of various molecular weight, pHi and charge density. Gluten, the proteins extracted from wheat flour is one of such. Gluten is widely used for its viscoelastic properties as an improver of cereal products (bread, pastry, etc.). It is composed of two classes of proteins, named gliadin and glutenin, similar in their amounts in glutamine (30%) and proline (10%). The more than 25 different polypeptides belonging to the gliadin class are hard to fractionate into individual components because of high redundancy in the primary sequences. Glutenin are in the form of polymers made from several distinct polypeptides concatenated through inter-chain disulfide bonds. Their molecular weights are evenly distributed from 100 kg/mol to 7,000 kg/mol.While it is well established that gliadin confers viscosity to gluten whereas glutenin polymers are at the origin of its elastic resistance, the interactions existing between both classes of gluten protein remain unknown. We previously showed by SLS and multi-angle DLS that gluten proteins suspended in ethanol/water (50/50, v/v), a theta solvent, includes large proteins assemblies (26,000 kg/mol, Rh 100nm) displaying an internal dynamic1. To get a better insight of the composition of those assemblies, we combined biochemical and physicochemical approaches. On the one hand, gluten proteins suspended in ethanol/water were fractionated by Asymmetrical- Flow-Field-Flow Fractionation (A4F) coupled to UV, SLS and QELS detectors. On the other hand, gluten proteins were partitioned by liquid-phase decomposition in respect with temperature. Protein composition of partitioned phases and eluting fractions recovered from A4F were characterized by size-exclusion chromatography. A specific interaction between omega-gliadin and glutenin polymers was evidenced.This result strengthens a very recent study that demonstrates a significant positive correlation between glutenin polymeric proteins, the ω‐gliadin fraction, and dough properties.

Published
2019

19. Ozone quantification by Selected Ion Flow Tube Mass Spectrometry: influence of humidity and manufacturing gas of ozone generator

Author

Marie-Hélène Manero, Jean-Stéphane Pic, Frédéric Violleau, Romain Richard, Leticia Vitola Pasetto, Valérie Simon, Simon, Valérie, Chimie Agro-Industrielle (CAI), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National de la Recherche Agronomique (INRA), Laboratoire de Génie Chimique (LGC), Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS), Toulouse Biotechnology Institute (TBI), Institut National de la Recherche Agronomique (INRA)-Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), Laboratoire de Chimie Agro-Industrielle (LCA), Institut National de la Recherche Agronomique (INRA)-Ecole Nationale Supérieure de Chimie de Toulouse, Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées, Centre National de la Recherche Scientifique - CNRS (FRANCE), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Institut National de la Recherche Agronomique - INRA (FRANCE), Institut National des Sciences Appliquées de Toulouse - INSA (FRANCE), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), Institut National Polytechnique de Toulouse - INPT (FRANCE), Institut National de la Recherche Agronomique (INRA)-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques (ENSIACET), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Université de Toulouse (UT), Université de Toulouse (UT)-Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT), and Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Ozone, Atmospheric chemistry, Analytical chemistry, chemistry.chemical_element, 010402 general chemistry, 01 natural sciences, Oxygen, Analytical Chemistry, Ion, chemistry.chemical_compound, [CHIM.GENI]Chemical Sciences/Chemical engineering, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, Génie chimique, Génie des procédés, Milieux et Changements globaux, Ions, 010401 analytical chemistry, Humidity, Precursors, 0104 chemical sciences, chemistry, 13. Climate action, Selected-ion flow-tube mass spectrometry, Nitrogen oxide, Saturation (chemistry)
Abstract

International audience; The quantification of ozone by SIFT-MS was investigated in conditions suitable with an industrial emission context (high ozone demand, dry air/oxygen as the manufacturing gas of the ozone generator, and high humidity levels beyond saturation at room conditions). Ozone reacts with four negative precursor ions available in the SIFT-MS device (NO2–, O2–, HO–, and O–), each precursor ion having its specific domain of linearity. For a high ozone concentration range, only NO2– and O2– have resulted in a linear behavior (between 1 and 100 ppmv of O3 for NO2–, between 1 and 50 ppmv of O3 for O2–). No water interference was identified during ozone measurements by SIFT-MS using NO2– and O2– precursor ions, even with extreme humidity levels. The presence of nitrogen oxide contaminants (due to the use of dry air as the manufacturing gas of the ozone generator) affected the ozone quantification by SIFT-MS. It is critical for NO2– precursor ions, whose rate constant varied as a function of NO2 concentrations. With O2– precursor ion, ozone was successfully measured in the presence of nitrogen oxides; however, the secondary chemistry must be taken into account.

Published
2019

20. Aldehydes gas ozonation monitoring: Interest of SIFT/MS versus GC/FID

Author

Frédéric Violleau, Marie-Hélène Manero, Leticia Vitola Pasetto, Jean-Stéphane Pic, Romain Richard, Valérie Simon, Laboratoire de Génie Chimique (LGC), Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées, Laboratoire de Chimie Agro-industrielle, LCA, INRA, INPT-ENSIACET, Université de Toulouse, Laboratoire d'Ingénierie des Systèmes Biologiques et des Procédés (LISBP), Centre National de la Recherche Scientifique (CNRS)-Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Institut National de la Recherche Agronomique (INRA), Chimie Agro-Industrielle (CAI), Institut National de la Recherche Agronomique (INRA)-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées, Institut National de la Recherche Agronomique (INRA)-Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), Centre National de la Recherche Scientifique - CNRS (FRANCE), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Institut National de la Recherche Agronomique - INRA (FRANCE), Institut National des Sciences Appliquées de Toulouse - INSA (FRANCE), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), Institut National Polytechnique de Toulouse - INPT (FRANCE), Université de Toulouse (UT)-Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT), Institut National de la Recherche Agronomique (INRA)-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques (ENSIACET), Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Université de Toulouse (UT), and Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)

Subjects
ozone artifacts, aldehydes, GC/FID, SIFT/MS, gas treatment, VOC, [SDV.BIO]Life Sciences [q-bio]/Biotechnology, Agronomie, Health, Toxicology and Mutagenesis, gas chromatography, 0208 environmental biotechnology, 02 engineering and technology, 010501 environmental sciences, 01 natural sciences, Mass Spectrometry, law.invention, chemistry.chemical_compound, law, Flame Ionization, Gas treatment, tropospheric ozone, General Medicine, Injector, Pollution, Ozone artifacts, Environmental Engineering, Ozone, chromatographie en phase gazeuse, Biotechnologies, Mass spectrometry, Gas Chromatography-Mass Spectrometry, Catalysis, Environmental Chemistry, Flame ionization detector, Génie chimique, Tropospheric ozone, Génie des procédés, 0105 earth and related environmental sciences, Volatile Organic Compounds, Aldehydes, Chromatography, Public Health, Environmental and Occupational Health, Reproducibility of Results, VOCs, General Chemistry, 020801 environmental engineering, ozone, chemistry, 13. Climate action, Gas chromatography, Gas chromatography–mass spectrometry
Abstract

Accepted manuscrit; Two analytical techniques – online gas chromatography coupled with flame ionization detector (often used method for VOCs monitoring) versus selected ion flow tube coupled with mass spectrometry (a more recent technique based on direct mass spectrometry) – were compared in association to an ozone-based gas treatment. Selecting aldehydes as the representative VOCs, their concentrations were monitored during ozonation experiments by both techniques in parallel. Contradictory results were obtained in the presence of ozone. Aldehydes were up to 90% removed due to a reaction with ozone according to GC/FID analysis, whereas with SIFT/MS, aldehydes concentration remained at the same level during the experiments regardless of the ozone presence. In addition, it was demonstrated that the apparent aldehydes removal was affected by GC injector temperature, varying from 90% (when it was at 250 °C) to 60% (at 100 °C). Meanwhile, even when the ozonation reactor was heated to 100 °C, no aldehydes conversion was evidenced by SIFT/MS, suggesting that the GC injector temperature was not the only interference-causing parameter. The ozone-aldehyde reaction is probably catalyzed by some material of GC injector and/or column. An ozone-GC interference was therefore confirmed, making unsuitable the use of GC/FID with silicone stationary phase to monitor aldehydes in presence of high concentrations of ozone (at least 50 ppmv). On the other hand, SIFT/MS was validated as a reliable technique, which can be employed in order to measure VOC concentrations in ozonation processes.

Published
2019

21. Fractionation and characterization of polyphenolic compounds and macromolecules in red wine by asymmetrical flow field-flow fractionation

Author

Kevin Pascotto, Pascale Williams, Frédéric Violleau, Olivier Geffroy, Véronique Cheynier, Chimie Agro-Industrielle (CAI), Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Sciences Pour l'Oenologie (SPO), Université de Montpellier (UM)-Institut national d’études supérieures agronomiques de Montpellier (Montpellier SupAgro), Institut national d'enseignement supérieur pour l'agriculture, l'alimentation et l'environnement (Institut Agro)-Institut national d'enseignement supérieur pour l'agriculture, l'alimentation et l'environnement (Institut Agro)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Région Occitanie , France, and Ecole d'ingénieurs Purpan, Toulouse, France

Subjects
Time Factors, Macromolecular Substances, [SDV]Life Sciences [q-bio], Wine, Fractionation, 010402 general chemistry, Polysaccharide, 01 natural sciences, Biochemistry, Analytical Chemistry, Colloid, Polysaccharides, [CHIM]Chemical Sciences, chemistry.chemical_classification, AF4, Chromatography, Chemistry, digestive, oral, and skin physiology, 010401 analytical chemistry, Organic Chemistry, Red wine, Polyphenols, food and beverages, Regenerated cellulose, General Medicine, Fractionation, Field Flow, 0104 chemical sciences, Molecular Weight, Proanthocyanidin, Polyphenol, Macromolecular complexes, Hydrodynamics, Tannins, Macromolecule
Abstract

Red wine is a complex matrix containing macromolecules such as condensed tannins and polysaccharides. Wine macromolecular components and their interactions have been reported to impact taste properties such as astringency but the colloidal systems formed in wine are not well known. A key prerequisite to characterize these systems is the ability to work under analytical conditions as close as possible to the colloid environment, preserving the sample structure and limiting the denaturation of macromolecular complexes. A method of Asymmetric Flow Field-Flow Fractionation (AF4) coupled with UV detection, multi-angle light scattering (MALS), and differential refractometer index (dRI) (AF4-UV-MALS-dRI) has been developed to analyse macromolecules, including tannins and polysaccharides, and macromolecular complexes, in red wine. This method separates objects according to their hydrodynamic radius and does not require calibration to determine molecular weight (Mw). AF4 can provide native separation of wine colloidal matter while working with simulated wine as mobile phase. The channel was equipped with a 350-µm spacer and the membrane made in regenerated cellulose had a cut-off of 5kDa. Different parameters of crossflow rate were investigated using a generic red wine to optimize separation conditions. Then, purified fractions of polysaccharides and tannins were analysed using the selected AF4 parameters. The comparison of the peaks obtained for these fractions and for the wine sample allowed us to determine the retention time associated with these macromolecules. The AF4 fractogram of wine was divided into four fractions. The first three were assigned to higher Mw tannins coeluted with lower Mw polysaccharides such as rhamnogalacturonan II (F1), to intermediate Mw polysaccharides (F2), and to higher Mw mannoproteins (F3) whereas the last fraction (F4) was not identified. Furthermore, our results have shown that AF4-UV-MALS-dRI could be an efficient technique to separate large size tannins as well as polysaccharides and macromolecular complexes.

Published
2020

22. Modulating analytical characteristics of thermovinified Carignan musts and the volatile composition of the resulting wines through the heating temperature

Author

Frédéric Violleau, Ricardo López, Carole Feilhes, Didier Kleiber, Olivier Geffroy, Jean-Luc Favarel, Vicente Ferreira, Ecole d'Ingénieurs de Purpan - EIP (FRANCE), Institut National Polytechnique de Toulouse - INPT (FRANCE), Institut National de la Recherche Agronomique - INRA (FRANCE), Institut Français de la Vigne et du Vin (FRANCE), Pera-Pellenc (FRANCE), Universidad Zaragoza (SPAIN), Laboratoire d'Agro-Physiologie (Toulouse, France), Laboratory for Flavor Analysis and Enology (Zaragoza, Spain), Institut Français de la Vigne et du Vin (IFV), Ecole d'Ingénieurs de Purpan (INPT - EI Purpan), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées, University of Zaragoza - Universidad de Zaragoza [Zaragoza], Laboratoire de Chimie Agro-Industrielle (LCA), Institut National de la Recherche Agronomique (INRA)-Ecole Nationale Supérieure de Chimie de Toulouse, Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Chimie Agro-Industrielle (CAI), and Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National de la Recherche Agronomique (INRA)

Subjects
Thermovinification, Hot Temperature, Aroma composition, Wine, Laboratory scale, 01 natural sciences, Heating temperature, Analytical Chemistry, chemistry.chemical_compound, 0404 agricultural biotechnology, Two temperature, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, [SDV.IDA]Life Sciences [q-bio]/Food engineering, Vitis, Food science, Volatile Organic Compounds, Chemistry, 010401 analytical chemistry, Extraction (chemistry), 04 agricultural and veterinary sciences, General Medicine, 040401 food science, 0104 chemical sciences, Fruit and Vegetable Juices, Pre-fermentation heat treatment, Composition (visual arts), Heating time, Geraniol, Biologie végétale, Food Science
Abstract

International audience; The impact of two temperature levels (50 °C and 75 °C) and heating times (30 min and 3 h) on the composition of thermovinified musts and wines from Carignan was investigated at the laboratory scale in 2014 and 2015. The heating temperature had a significant impact on the extraction of amino acids and a probable thermal degradation of anthocyanins was noted at 75 °C. In 2014, musts from grapes that underwent a heat treatment at 50 °C for 3 h had a similar level of phenolic compounds as those treated at 75 °C for 30 min. This indicates that the reduction of the heating temperature in some vintages can be compensated for through an extension of the heating period. Several grape-derived molecules were impacted by the rise in temperature and wines made from grapes treated at 50 °C in most cases contained larger concentrations of geraniol, β-citronellol, β-damascenone and 3-mercaptohexanol.

Published
2018

23. Mechanistic Insights into Polyion Complex Associations

Author

Anne-Françoise Mingotaud, Debora Berti, Baptiste Amouroux, Jean-Daniel Marty, Frédéric Violleau, Michael Sztucki, Emanuela Di Cola, Giacomo Parigi, Claudio Luchinat, Stéphanie Balor, Christophe Mingotaud, Stéphane Gineste, Ugo Till, Barbara Lonetti, Interactions moléculaires et réactivité chimique et photochimique (IMRCP), Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut de Chimie de Toulouse (ICT-FR 2599), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD), European Synchrotron Radiation Facility (ESRF), Laboratoire de Chimie des Polymères Organiques (LCPO), Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC), Chimie Agro-Industrielle (CAI), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National de la Recherche Agronomique (INRA), Centre de Microscopie Électronique Appliquée à la Biologie (CMEAB), Hôpital de Rangueil, CHU Toulouse [Toulouse]-CHU Toulouse [Toulouse]-Toulouse Réseau Imagerie-Genotoul ( TRI-Genotoul), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), This work was funded by the Midi-Pyrenees region and University of Toulouse, Centre National de la Recherche Scientifique (CNRS)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Institut de Recherche pour le Développement (IRD)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées, Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Centre National de la Recherche Scientifique (CNRS), Institut National de la Recherche Agronomique (INRA)-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées, Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Hôpital de Rangueil, CHU Toulouse [Toulouse]-CHU Toulouse [Toulouse], Centre National de la Recherche Scientifique - CNRS (FRANCE), Ecole d'Ingénieurs de Purpan - EIP (FRANCE), European Synchrotron Radiation Facility - ESRF (FRANCE), Institut National Polytechnique de Toulouse - INPT (FRANCE), Institut National de la Recherche Agronomique - INRA (FRANCE), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), Università degli Studi di Milano (ITALY), Organisation Européenne pour la Recherche Nucléaire - CERN (SWITZERLAND), Università degli Studi di Firenze (ITALY), Laboratoire de Chimie Agro-Industrielle - LCA (Toulouse, France), Centre de biologie Intégrative (Toulouse, france), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Institut de Recherche pour le Développement (IRD)-Centre National de la Recherche Scientifique (CNRS), Institut de Chimie de Toulouse (ICT), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Institut Ecologie et Environnement (INEE), Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS)-Fédération de Recherche Fluides, Energie, Réacteurs, Matériaux et Transferts (FERMAT), Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS), IDeAS - Interfaces Dynamiques et Assemblages Stimulables (IDeAS), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie de Toulouse (ICT), Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut National de la Recherche Agronomique (INRA)-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques (ENSIACET), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Université de Toulouse (UT), Toulouse Réseau Imagerie-Genotoul ( TRI-Genotoul), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), and Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE)

Subjects
Relaxometry, Polymers and Plastics, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, Micelle, Light scattering, Inorganic Chemistry, Dynamic light scattering, Autre, Materials Chemistry, Polyion Complex, chemistry.chemical_classification, Chemistry, Small-angle X-ray scattering, Organic Chemistry, technology, industry, and agriculture, Polymer, biochemical phenomena, metabolism, and nutrition, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Ingénierie biomédicale, Chemical engineering, Macromolecules, [SDV.IB]Life Sciences [q-bio]/Bioengineering, Self-assembly, 0210 nano-technology, Drug carrier, [CHIM.OTHE]Chemical Sciences/Other
Abstract

International audience; Polyion complex (PIC) micelles formed from the electrostatic interaction between oppositely charged polymers have been studied for their promising applications in the biomedical field as drug carriers or vectors for gene delivery. In spite of their asset of possible high drug loading, their formation process remains poorly studied. In this work, we investigate the properties of a series of PICs based on poly(ethylene oxide-b-acrylic acid) (PEO–PAA)/dendrigraft poly(L-lysine) (DGL3), using PEO–PAA with different compositions and average molecular weights. For each PEO–PAA/DGL3 pair, the complexes were characterized as a function of the ratios between acid and amine moieties combining different techniques: dynamic light scattering (DLS), flow field-flow fractionation (FlFFF), small-angle X-ray scattering (SAXS), and relaxometry. The coupling of batch techniques, i.e., DLS, SAXS, and relaxometry, together with a soft separation technique like FlFFF enabled a finer analysis to elucidate subtle details of the association process and of the polydispersity of the complexes. We show that the formation of PICs is more complex than previously described. In particular, we demonstrate that PICs with stoichiometry 1:1 may form at low ratios provided that the acidic block is long enough to neutralize the cationic dendrigraft with few polymer chains. Moreover, in such conditions, PICs with stoichiometry 1:1 often coexist with free dendritic polymers and other associated complex species.

Published
2018

24. Polymeric self-assemblies for photodynamic therapy: A critical approach

Author

Marie-Pierre Rols, Laure Gibot, Anne-Françoise Mingotaud, Frédéric Violleau, Mireille Gaucher, Christophe Mingotaud, Ugo Till, Patricia Vicendo, Centre National de la Recherche Scientifique - CNRS (FRANCE), Ecole d'Ingénieurs de Purpan - EIP (FRANCE), Institut National Polytechnique de Toulouse - INPT (FRANCE), Institut National de la Recherche Agronomique - INRA (FRANCE), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), Laboratoire de Chimie Agro-Industrielle - LCA (Toulouse, France), Interactions moléculaires et réactivité chimique et photochimique (IMRCP), Institut de Chimie de Toulouse (ICT), Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Institut Ecologie et Environnement (INEE), Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS)-Fédération de Recherche Fluides, Energie, Réacteurs, Matériaux et Transferts (FERMAT), Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS), Ecole d'Ingénieurs de Purpan (INP - PURPAN), Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Université de Toulouse (UT), Institut de pharmacologie et de biologie structurale (IPBS), Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS), IDeAS - Interfaces Dynamiques et Assemblages Stimulables (IDeAS), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie de Toulouse (ICT), Chimie Agro-Industrielle (CAI), Institut National de la Recherche Agronomique (INRA)-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques (ENSIACET), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National Polytechnique (Toulouse) (Toulouse INP), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), and Ecole d'Ingénieurs de Purpan (INPT - EI Purpan)

Subjects
Materials science, Critical approach, medicine.medical_treatment, Biophysics, Nanotechnology, Photodynamic therapy, [SDV.CAN]Life Sciences [q-bio]/Cancer, 02 engineering and technology, Dermatology, Neutron scattering, 01 natural sciences, Light scattering, medicine, Zeta potential, Photodynamic, Pharmacology (medical), Polymeric, Cancer, Atomic force microscopy, 010401 analytical chemistry, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Characterization (materials science), Oncology, 0210 nano-technology, Refractometry
Abstract

International audience; The work presented here suggests a new approach in the critical development of polymeric nanovectors for photodynamic therapy (PDT) against cancer. Whereas hundreds of studies quickly jump forward from formation of self-assemblies to biological application without having a thorough examination of the vector solution, we suggest having a parallel assessment of formation/characterization of the nanovectors and biological activity [1]. This is possible by first using a careful physical chemistry characterization of the vectors by both batch techniques (light and neutron scattering, electron microscopy, atomic force microscopy) and Asymmetrical Flow Field-Flow Fractionation (AsFlFFF) coupled to adequate detectors (refractometry, light scattering) [2]. This enables us to fully characterize the vectors regarding purity, size and zeta potential.

Published
2017

25. Frit inlet field-flow fractionation techniques for the characterization of polyion complex self-assemblies

Author

S. Kim Ratanathanawongs Williams, Baptiste Amouroux, Ugo Till, Christophe Mingotaud, Frédéric Violleau, Jean-Daniel Marty, Anne-Françoise Mingotaud, Mireille Gaucher, Stéphane Gineste, Carmen R.M. Bria, Barbara Lonetti, Interactions moléculaires et réactivité chimique et photochimique (IMRCP), Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut de Chimie de Toulouse (ICT-FR 2599), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD), Centre National de la Recherche Scientifique (CNRS), Département Sciences Agronomiques et Agroalimentaires - EI Purpan, Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole d'Ingénieurs de Purpan (INPT - EI Purpan), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées, Department of Chemistry, Laboratory for Advanced Separations Technologies, Colorado School of Mines, Chimie Agro-Industrielle (CAI), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National de la Recherche Agronomique (INRA), This work was funded by the Midi-Pyrenees region and University of Toulouse. National Science Foundation Grant CHE-1508827 for support., Centre National de la Recherche Scientifique (CNRS)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Institut de Recherche pour le Développement (IRD)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Institut National de la Recherche Agronomique (INRA)-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées, Centre National de la Recherche Scientifique - CNRS (FRANCE), Colorado School of Mines (USA), Ecole d'Ingénieurs de Purpan - EIP (FRANCE), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Institut National de la Recherche Agronomique - INRA (FRANCE), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), Laboratoire de Chimie Agro-Industrielle - LCA (Toulouse, France), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Institut de Recherche pour le Développement (IRD)-Centre National de la Recherche Scientifique (CNRS), Institut National Polytechnique de Toulouse - INPT (FRANCE), Ecole d'Ingénieurs de Purpan (INPT - EI Purpan), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Institut de Chimie de Toulouse (ICT), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Institut Ecologie et Environnement (INEE), Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS)-Fédération de Recherche Fluides, Energie, Réacteurs, Matériaux et Transferts (FERMAT), Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS), Ecole d'Ingénieurs de Purpan (INP - PURPAN), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Université de Toulouse (UT), Université de Toulouse (UT), and Institut National de la Recherche Agronomique (INRA)-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques (ENSIACET)

Subjects
[SDV.SA]Life Sciences [q-bio]/Agricultural sciences, Polymers, Proton Magnetic Resonance Spectroscopy, Acrylic Resins, Analytical chemistry, Fractionation, Chemical Fractionation, Sodium Chloride, 010402 general chemistry, Frit inlet flow field-flow fractionation, 01 natural sciences, Biochemistry, Dissociation (chemistry), Analytical Chemistry, chemistry.chemical_compound, polymère, Autre, Dynamic light scattering, Acrylic resin, Acrylic acid, Ions, chemistry.chemical_classification, Field flow fractionation, Chromatography, Elution, Lysine, 010401 analytical chemistry, Organic Chemistry, General Medicine, Polymer, Self-assembly, Dynamic Light Scattering, Fractionation, Field Flow, 0104 chemical sciences, Molecular Weight, Solutions, Refractometry, Bays, chemistry, Polyion complex micelles, visual_art, Chromatography, Gel, visual_art.visual_art_medium, [CHIM.OTHE]Chemical Sciences/Other, Flow field-flow fractionation, Sciences agricoles
Abstract

International audience; Polymer self-assemblies joining oppositely charged chains, known as polyion complexes (PICs), have been formed using poly(ethyleneoxide – b – acrylic acid)/poly(l-lysine), poly(ethyleneoxide-b-acrylic acid)/dendrigraft poly(l-lysine) and poly[(3-acrylamidopropyl) trimethylammonium chloride – b – N – isopropyl acrylamide]/poly(acrylic acid). The self-assemblies have been first characterized in batch by Dynamic Light Scattering. In a second step, their analysis by Flow Field-Flow Fractionation techniques (FlFFF) was examined. They were shown to be very sensitive to shearing, especially during the focus step of the fractionation, and this led to an incompatibility with asymmetrical FlFFF. On the other hand, Frit Inlet FlFFF proved to be very efficient to observe them, either in its symmetrical (FI-FlFFF) or asymmetrical version (FI-AsFlFFF). Conditions of elution were found to optimize the sample recovery in pure water. Spherical self-assemblies were detected, with a size range between 70–400nm depending on the polymers. Compared to batch DLS, FI-AsFlFFF clearly showed the presence of several populations in some cases. The influence of salt on poly(ethyleneoxide-b-acrylic acid) (PEO-PAA) 6000-3000/dendrigraft poly(l-lysine) (DGL 3) was also assessed in parallel in batch DLS and FI-AsFlFFF. Batch DLS revealed a first process of swelling of the self-assembly for low concentrations up to 0.8M followed by the dissociation. FI-AsFlFFF furthermore indicated a possible ejection of DGL3 from the PIC assembly for concentrations as low as 0.2M, which could not be observed in batch DLS.

Published
2017

26. Gradual disaggregation of the casein micelle improves its emulsifying capacity and decreases the stability of dairy emulsions

Author

Marie-Noelle Madec, Fanny Lazzaro, Mireille Gaucher-Delmas, Christelle Lopez, Arnaud Saint-Jalmes, Frédéric Violleau, Frédéric Gaucheron, Eric Beaucher, Science et Technologie du Lait et de l'Oeuf (STLO), Institut National de la Recherche Agronomique (INRA)-AGROCAMPUS OUEST, Institut national d'enseignement supérieur pour l'agriculture, l'alimentation et l'environnement (Institut Agro)-Institut national d'enseignement supérieur pour l'agriculture, l'alimentation et l'environnement (Institut Agro), Centre National Interprofessionnel de l'Economie Laitière [Paris] (CNIEL), Institut de Physique de Rennes (IPR), Université de Rennes 1 (UR1), Université de Rennes (UNIV-RENNES)-Université de Rennes (UNIV-RENNES)-Centre National de la Recherche Scientifique (CNRS), Chimie Agro-Industrielle (CAI), Institut National de la Recherche Agronomique (INRA)-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées, Département Sciences Agronomiques et Agroalimentaires - EI Purpan, Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole d'Ingénieurs de Purpan (INPT - EI Purpan), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées, The authors thank the French Dairy Interbranch Organization (CNIEL) for their financial support, Rachel Boutrou for assistance with writing the manuscript and Anne-Laure Chapeau for proof reading the article., Centre National Interprofessionnel de l'Economie Laitière - CNIEL (FRANCE), Centre National de la Recherche Scientifique - CNRS (FRANCE), Ecole d'Ingénieurs de Purpan - EIP (FRANCE), Institut National Polytechnique de Toulouse - INPT (FRANCE), Institut National de la Recherche Agronomique - INRA (FRANCE), Université de Rennes 1 (FRANCE), Institut de Physique de Rennes - IPR (Rennes, France), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National de la Recherche Agronomique (INRA), Ecole d'Ingénieurs de Purpan (INPT - EI Purpan), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université de Rennes (UR)-Centre National de la Recherche Scientifique (CNRS), Institut National de la Recherche Agronomique (INRA)-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques (ENSIACET), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Université de Toulouse (UT), Ecole d'Ingénieurs de Purpan (INP - PURPAN), and Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE)

Subjects
Flocculation, General Chemical Engineering, Sodium, chemistry.chemical_element, Micelle, chemistry.chemical_compound, Colloid, 0404 agricultural biotechnology, Casein, Sodium citrate, [SDV.IDA]Life Sciences [q-bio]/Food engineering, Functionality, Mineral, [PHYS]Physics [physics], Chromatography, 0402 animal and dairy science, Casein aggregate, Foams, 04 agricultural and veterinary sciences, General Chemistry, Phosphate, 040401 food science, 040201 dairy & animal science, [CHIM.THEO]Chemical Sciences/Theoretical and/or physical chemistry, Creaming, Milk, chemistry, Chemical engineering, Calcium phosphate, Alimentation et Nutrition, Citrate, [PHYS.COND.CM-SCM]Physics [physics]/Condensed Matter [cond-mat]/Soft Condensed Matter [cond-mat.soft], Food Science
Abstract

International audience; The casein micelle is a highly aggregated colloid consisting of phosphoproteins and minerals, in particular calcium and phosphate. Its properties are affected by physico-chemical changes which provide possibilities for the development of new casein aggregates (CAs) with novel functionalities. The aim of this study was to investigate the emulsifying and emulsion-stabilizing capacity of gradually demineralized CAs in model dairy emulsions. Tri sodium citrate (TSC) was used to remove calcium and inorganic phosphate from pure casein micelles in order to produce four suspensions of differently demineralized CAs. Two types of milkfat-in-suspension (30:70 v/v) emulsions were then prepared to study the emulsifying and emulsion-stabilizing capacity of these CAs separately. Casein micelles were progressively demineralized (from 24 to 81% calcium reduction) and dissociated with the increase in TSC concentration. Three distinct populations of particles (micelle-like aggregates, sodium caseinate-like aggregates and casein monomers) were present in every suspension in different proportions. The smaller CAs had better emulsifying capacity and similar surface activity according to interfacial studies. The state of aggregation of the CAs was thus the main factor that controlled their emulsifying capacity. However, the emulsions formed with these smaller aggregates were less stable against creaming and flocculation, but still resisted coalescence under our storage conditions (21 days at 50 °C). The properties of the interfacial casein layers did not depend on the aggregation state of the CAs used to form the emulsions. The differences in instability were attributed to the nature of the non-adsorbed CAs and storage conditions.

Published
2017

27. A new way of valorizing biomaterials: The use of sunflower protein for α-tocopherol microencapsulation

Author

Alla Nesterenko, Françoise Silvestre, Isabelle Alric, Vanessa Durrieu, and Frédéric Violleau

Subjects
0106 biological sciences, Chromatography, Chemistry, 04 agricultural and veterinary sciences, Fractionation, engineering.material, 040401 food science, 01 natural sciences, Acylation, Hydrolysis, 0404 agricultural biotechnology, 010608 biotechnology, Spray drying, Enzymatic hydrolysis, Emulsion, engineering, Biopolymer, Microparticle, Food Science
Abstract

Biopolymer based microparticles were efficiently prepared from sunflower protein (SP) wall material and α-tocopherol (T) active core using a spray-drying technique. Protein enzymatic hydrolysis and/or N-acylation were carried out to make some structural modifications to the vegetable protein. Native and hydrolyzed SP were characterized by Asymmetrical Flow Field-Flow Fractionation (AsFlFFF). Results of AsFlFFF confirmed that size of proteinic macromolecules was influenced by degree of hydrolysis. The effect of protein modifications and the influence of wall/core ratio on both emulsions and microparticle properties were evaluated. Concerning emulsion properties, enzymatic hydrolysis involved a decrease in viscosity, whereas acylation did not significantly affect emulsion droplet size and viscosity. Microparticles obtained with hydrolyzed SP wall material showed lower retention efficiency (RE) than native SP microparticles (62–80% and 93% respectively). Conversely, acylation of both hydrolyzed SP and native SP allowed a higher RE to be reached (up to 100%). Increasing T concentration increased emulsion viscosity, emulsion droplet size and microparticle size, and enhanced RE. These results demonstrated the feasibility of highly loaded (up to 79.2% T) microparticles.

Published
2013

28. Structural modifications of cellulose samples after dissolution into various solvent systems

Author

Vanessa Durrieu, Frédéric Violleau, Marianne Gaborieau, Jérémy Rebière, Patrice Castignolles, Antoine Rouilly, Maelie Heuls, Ecole d'Ingénieurs de Purpan - EIP (FRANCE), Institut National Polytechnique de Toulouse - INPT (FRANCE), Institut National de la Recherche Agronomique - INRA (FRANCE), University of Western Sydney - UWS (AUSTRALIA), Chimie Agro-Industrielle (CAI), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National de la Recherche Agronomique (INRA), School of Science and Health, Molecular Medicine Research Group, Western Sydney University, School of Science and Health, Australian Centre for Research on Separation Science, Institut National de la Recherche Agronomique (INRA)-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées, Western Sydney University (UWS), and Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE)

Subjects
Thermogravimetric analysis, degré de polymérisation, Agronomie, Scanning electron microscope, état cristallin, [SDV.SA.AGRO]Life Sciences [q-bio]/Agricultural sciences/Agronomy, solvant, 02 engineering and technology, Degree of polymerization, 010402 general chemistry, 01 natural sciences, Biochemistry, Analytical Chemistry, chemistry.chemical_compound, Crystallinity, dissolving, Crystallinity index, Structural effects, Cellulose, Dissolution, Molar mass, 021001 nanoscience & nanotechnology, crystalline state, 0104 chemical sciences, chemistry, Chemical engineering, Polymerization, 0210 nano-technology, Underivatizing solvent
Abstract

International audience; This work deals with the modifications resulting from the dissolution of four commercial cellulosic samples, with different crystallinity rates and degrees of polymerization (DPs), in four solvent systems, known and used to dissolve cellulose. The dissolution conditions were optimized for the 16 various systems and followed by turbidity measurements. After regeneration, the samples were analyzed by thermal gravimetric analysis (TGA), scanning electron microscopy (SEM), and X-ray diffractometry (XRD) to study their modification. Viscosimetry measurements were used to evaluate the potential decrease of the DP after dissolution. The observed structural modifications established that, for low DP, all the solvent systems were efficient in dissolving the cellulose without altering the DP, except BMIM [Cl], which provoked a decrease of up to 40 % and a decrease of around 20 % of the degradation temperature (onset temperature, T o). For high molecular weight (MW) celluloses, DMSO/TBAF was the only system to allow a complete dissolution without any molar mass loss and degradation temperature modification.

Published
2016

29. Influence of Storage Temperature on the Composition and the Antibacterial Activity of Ozonized Sunflower Oil

Author

Sophie Moureu, A. Calmon, Frédéric Violleau, Djamila Ali Haimoud-Lekhal, Ecole d'Ingénieurs de Purpan - EIP (FRANCE), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Institut National de la Recherche Agronomique - INRA (FRANCE), Laboratoire de Chimie Agro-Industrielle (LCA), Institut National de la Recherche Agronomique (INRA)-Ecole Nationale Supérieure de Chimie de Toulouse, Ecole d'Ingénieurs de Purpan (INPT - EI Purpan), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées, Institut National Polytechnique de Toulouse - INPT (FRANCE), Chimie Agro-Industrielle (CAI), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National de la Recherche Agronomique (INRA), and Midi-Pyrenees Region [12050572]

Subjects
0301 basic medicine, 030103 biophysics, Environmental Engineering, food.ingredient, Ozonized Oil, 010501 environmental sciences, 01 natural sciences, Peroxide, 03 medical and health sciences, chemistry.chemical_compound, food, Ozone, Storage Temperature, Environmental Chemistry, Food science, 0105 earth and related environmental sciences, [SDV.EE]Life Sciences [q-bio]/Ecology, environment, Ecologie, Environnement, Chemistry, Sunflower oil, Antibacterial Activity, Environmental chemistry, Composition (visual arts), Gas chromatography, Antibacterial activity, Stability
Abstract

International audience; The use of ozonized vegetable oils as drugs or cosmetics requires having data on their stability over the time. In this study, ozonized sunflower oil was stored under different temperatures for up to 1 year. Peroxide index, acidity value, gas chromatography profile, infrared profile and antibacterial activity (against Streptococcus uberis) of this ozonized oil were followed. The results highlight the fact that the better way to preserve the initial composition of ozonized oil is to keep it at low temperature. However, the antibacterial activity is not diminished by the changes occurring to the composition.

Published
2016

30. Multimodal Dispersion of Nanoparticles: A Comprehensive Evaluation of Size Distribution with 9 Size Measurement Methods

Author

Frédéric Violleau, Christine Vauthier, Fanny Varenne, Ali Makky, Mireille Gaucher-Delmas, Centre National de la Recherche Scientifique - CNRS (FRANCE), Ecole d'Ingénieurs de Purpan - EIP (FRANCE), Institut National Polytechnique de Toulouse - INPT (FRANCE), Institut National de la Recherche Agronomique - INRA (FRANCE), Université Paris-Sud 11 (FRANCE), Laboratoire de Chimie Agro-Industrielle - LCA (Toulouse, France), Institut Galien Paris-Sud (IGPS), Université Paris-Sud - Paris 11 (UP11)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), École nationale supérieure agronomique de Toulouse [ENSAT], Ecole d'Ingénieurs de Purpan (INPT - EI Purpan), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées, BPI-France: Projet Nice, and Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE)

Subjects
Tunable resistive pulse sensing, Materials science, Analytical chemistry, Pharmaceutical Science, Nanoparticle tracking analysis, 02 engineering and technology, 010402 general chemistry, Microscopy, Atomic Force, 01 natural sciences, light scattering, Light scattering, Dynamic light scattering, Dispersion (optics), nanoparticle tracking analysis, Pharmacology (medical), Static light scattering, tunable resistive pulse sensing, particle size distribution, Particle Size, Pharmacology, Microscopy, Organic Chemistry, [SDV.SP]Life Sciences [q-bio]/Pharmaceutical sciences, 021001 nanoscience & nanotechnology, Particle size distribution, Dynamic Light Scattering, Fractionation, Field Flow, 0104 chemical sciences, Microscopy, Electron, [CHIM.POLY]Chemical Sciences/Polymers, [SDV.SP.PG]Life Sciences [q-bio]/Pharmaceutical sciences/Galenic pharmacology, Particle-size distribution, microscopy, Molecular Medicine, Particle, Nanoparticles, Particle size, 0210 nano-technology, Sciences agricoles, Biotechnology
Abstract

International audience; PURPOSE: Evaluation of particle size distribution (PSD) of multimodal dispersion of nanoparticles is a difficult task due to inherent limitations of size measurement methods. The present work reports the evaluation of PSD of a dispersion of poly(isobutylcyanoacrylate) nanoparticles decorated with dextran known as multimodal and developed as nanomedecine.METHODS: The nine methods used were classified as batch particle i.e. Static Light Scattering (SLS) and Dynamic Light Scattering (DLS), single particle i.e. Electron Microscopy (EM), Atomic Force Microscopy (AFM), Tunable Resistive Pulse Sensing (TRPS) and Nanoparticle Tracking Analysis (NTA) and separative particle i.e. Asymmetrical Flow Field-Flow Fractionation coupled with DLS (AsFlFFF) size measurement methods.RESULTS: The multimodal dispersion was identified using AFM, TRPS and NTA and results were consistent with those provided with the method based on a separation step prior to on-line size measurements. None of the light scattering batch methods could reveal the complexity of the PSD of the dispersion.CONCLUSIONS: Difference between PSD obtained from all size measurement methods tested suggested that study of the PSD of multimodal dispersion required to analyze samples by at least one of the single size particle measurement method or a method that uses a separation step prior PSD measurement.

Published
2016

31. Crosslinked polymeric self-assemblies as an efficient strategy for photodynamic therapy on a 3D cell culture

Author

Frédéric Violleau, Marie-Pierre Rols, Patricia Vicendo, Laure Gibot, Mireille Gaucher, Ugo Till, Anne-Françoise Mingotaud, Centre National de la Recherche Scientifique - CNRS (FRANCE), Ecole d'Ingénieurs de Purpan - EIP (FRANCE), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Institut National de la Recherche Agronomique - INRA (FRANCE), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), Laboratoire des Interactions Moléculaires et de la Réactivité Chimique et Photochimique – IMRCP (Toulouse, France), Ecole d'Ingénieurs de Purpan (INPT - EI Purpan), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées, Interactions moléculaires et réactivité chimique et photochimique (IMRCP), Centre National de la Recherche Scientifique (CNRS)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Institut de Recherche pour le Développement (IRD)-Centre National de la Recherche Scientifique (CNRS), Institut de pharmacologie et de biologie structurale (IPBS), Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS), Laboratoire de Chimie Agro-Industrielle (LCA), Institut National de la Recherche Agronomique (INRA)-Ecole Nationale Supérieure de Chimie de Toulouse, Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Institut de Recherche pour le Développement (IRD)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées, Département Sciences Agronomiques et Agroalimentaires - EI Purpan, Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), French ANR P2N COPOPDT, Midi-Pyrenees region, University of Toulouse, Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD), Chimie Agro-Industrielle (CAI), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National de la Recherche Agronomique (INRA), Université de Toulouse (UT)-Université de Toulouse (UT), Institut de Chimie de Toulouse (ICT), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Institut Ecologie et Environnement (INEE), Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS)-Fédération de Recherche Fluides, Energie, Réacteurs, Matériaux et Transferts (FERMAT), Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS), Université de Toulouse (UT)-Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS), IDeAS - Interfaces Dynamiques et Assemblages Stimulables (IDeAS), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie de Toulouse (ICT), Institut National de la Recherche Agronomique (INRA)-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques (ENSIACET), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National Polytechnique (Toulouse) (Toulouse INP), Institut National Polytechnique de Toulouse - INPT (FRANCE), and Ecole d'Ingénieurs de Purpan (INP - PURPAN)

Subjects
ph, General Chemical Engineering, PhotoDynamic Therapy (PDT), Radical polymerization, 02 engineering and technology, [SDV.BC]Life Sciences [q-bio]/Cellular Biology, macromolecular substances, in-vitro, 010402 general chemistry, 01 natural sciences, Micelle, triggered release, doxorubicin, chemistry.chemical_compound, paclitaxel, Dynamic light scattering, Polymer chemistry, [CHIM]Chemical Sciences, Photosensitizer, block-copolymer micelles, intracellular drug-delivery, polymers, chemistry.chemical_classification, Acrylate, technology, industry, and agriculture, General Chemistry, Polymer, 021001 nanoscience & nanotechnology, Ethyleneglycoldimethacrylate (EGDMA), 0104 chemical sciences, chemistry, Polymerization, Chemical engineering, Pheophorbide A, facile preparation, nanoparticles, Biologie cellulaire, 0210 nano-technology, reactive micelles
Abstract

International audience; In order to compare the efficiency of crosslinked nano-vectors in the field of photodynamic therapy (PDT) both on 2D and 3D cell cultures, various polymeric crosslinked self-assemblies based on poly-(ethyleneoxide-b-epsilon-caprolactone) have been synthesized by radical polymerization of acrylate end-functionalized polymers. Crosslinked self-assemblies obtained from the reaction of the functionalized polymers with ethyleneglycoldimethacrylate (EGDMA) were compared to chain-end polymerized and to unreacted ones. Polymeric micelles with a size between 10 and 20 nm were obtained, as well as an elongated system with a length close to 100 nm. They all have been characterized by Transmission Electron Microscopy and Dynamic Light Scattering but also by Asymmetrical Flow Field-Flow Fractionation in order to prove that they consisted of pure self-assemblies. Chain-end polymerization or crosslinking did not induce any change in morphology nor strong size modification. After post-encapsulation of a photosensitizer, namely Pheophorbide a, the systems have been examined for their potential use in PDT on HCT-116 and FaDu human tumor cell lines both in 2D and 3D cultures. The crosslinked vectors were observed to be the most efficient on both cell lines cultivated in 3D spheroids, whereas unreacted or chain-end polymerized ones presented a lower activity. This was different from the trend observed in 2D cell cultures where an uncrosslinked micelle was observed to be efficient at a lower concentration compared to its chain-end polymerized or crosslinked analogue. The different synthesized self-assemblies also allowed assessing the influence of polymer chain length and shape on PDT efficiency. The molecular weight of the polymer did not lead in our case to efficiency change, for similar size and surface characteristics. As for the shape effect, the elongated self-assembly was not observed in our case to be more efficient than spherical micelles. Crosslinked polymeric vectors are therefore promising vectors for 3D tumor treatment.

Published
2016

32. Self-assembled polymeric vectors mixtures: characterization of the polymorphism and existence of synergistic effects in photodynamic therapy

Author

Christophe Mingotaud, Mireille Gaucher, Laure Gibot, Marie-Pierre Rols, Patricia Vicendo, Anne-Françoise Mingotaud, Ugo Till, Frédéric Violleau, Interactions moléculaires et réactivité chimique et photochimique (IMRCP), Institut de Chimie de Toulouse (ICT), Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Institut Ecologie et Environnement (INEE), Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS)-Fédération de Recherche Fluides, Energie, Réacteurs, Matériaux et Transferts (FERMAT), Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS), Institut de pharmacologie et de biologie structurale (IPBS), Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS), IDeAS - Interfaces Dynamiques et Assemblages Stimulables (IDeAS), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie de Toulouse (ICT), Département Sciences Agronomiques et Agroalimentaires - EI Purpan, Ecole d'Ingénieurs de Purpan (INPT - EI Purpan), Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Université de Toulouse (UT), Chimie Agro-Industrielle (CAI), Institut National de la Recherche Agronomique (INRA)-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques (ENSIACET), French ANR P2N COPOPDT, Midi-Pyrenees region, University of Toulouse, Centre National de la Recherche Scientifique - CNRS (FRANCE), Ecole d'Ingénieurs de Purpan - EIP (FRANCE), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Institut National de la Recherche Agronomique - INRA (FRANCE), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), Laboratoire des Interactions Moléculaires et de la Réactivité Chimique et Photochimique – IMRCP (Toulouse, France), Institut National Polytechnique de Toulouse - INPT (FRANCE), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD), Centre National de la Recherche Scientifique (CNRS)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées, Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole d'Ingénieurs de Purpan (INPT - EI Purpan), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées, Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National de la Recherche Agronomique (INRA), and Ecole d'Ingénieurs de Purpan (INP - PURPAN)

Subjects
Polymersomes, Materials science, Polymers, Asymmetrical flow field flow fractionation, Bioengineering, Nanotechnology, Asymmetrical flow fieldflow fractionation, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, Micelle, Photodynamic therapy, chemistry.chemical_compound, Dynamic light scattering, Amphiphile, General Materials Science, Photosensitizer, Vesicles, Electrical and Electronic Engineering, Micelles, Field flow fractionation, Photosensitizing Agents, Mechanical Engineering, Vesicle, General Chemistry, Self-assembly, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Ingénierie biomédicale, Chemical engineering, chemistry, Photochemotherapy, Mechanics of Materials, Pheophorbide A, Polymersome, Polymeric micelles, [SDV.IB]Life Sciences [q-bio]/Bioengineering, Spheroids, 0210 nano-technology
Abstract

International audience; The objective of this work was to assess the relation between the purity of polymeric self-assemblies vectors solution and their photodynamic therapeutic efficiency. For this, several amphiphilic block copolymers of poly(ethyleneoxide-b-ε-caprolactone) have been used to form self-assemblies with different morphologies (micelles, worm-like micelles or vesicles). In a first step, controlled mixtures of preformed micelles and vesicles have been characterized both by dynamic light scattering and asymmetrical flow field flow fractionation (AsFlFFF). For this, a custom-made program, STORMS, was developed to analyze DLS data in a thorough manner by providing a large set of fitting parameters. This showed that DLS only sensed the larger vesicles when the micelles/vesicles ratio was 80/20 w/w. On the other hand, AsFlFFF allowed clear detection of the presence of micelles when this same ratio was as low as 10/90. Subsequently, the photodynamic therapy efficiency of various controlled mixtures was assessed using multicellular spheroids when a photosensitizer, pheophorbide a, was encapsulated in the polymer self-assemblies. Some mixtures were shown to be as efficient as monomorphous systems. In some cases, mixtures were found to exhibit a higher PDT efficiency compared to the individual nano-objects, revealing a synergistic effect for the efficient delivery of the photosensitizer. Polymorphous vectors can therefore be superior in therapeutic applications.

Published
2016

33. Ozone Effects on Botrytis cinerea Conidia using a Bubble Column: Germination Inactivation and Membrane Phospholipids Oxidation

Author

Frédéric Violleau, Didier Kleiber, Romain J. G. Pierron, Marielle Pagès, Laboratoire de Chimie Agro-Industrielle (LCA), Institut National de la Recherche Agronomique (INRA)-Ecole Nationale Supérieure de Chimie de Toulouse, Ecole d'Ingénieurs de Purpan (INPT - EI Purpan), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées, Ecole d'Ingénieurs de Purpan - EIP (FRANCE), Institut National Polytechnique de Toulouse - INPT (FRANCE), Institut National de la Recherche Agronomique - INRA (FRANCE), Chimie Agro-Industrielle (CAI), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National de la Recherche Agronomique (INRA), and Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE)

Subjects
Bubble Column, [SDV.SA]Life Sciences [q-bio]/Agricultural sciences, Environmental Engineering, Ozone, Germination, 010501 environmental sciences, Biology, 01 natural sciences, 040501 horticulture, Conidium, Lipid peroxidation, Conidia, chemistry.chemical_compound, Botrytis cinerea, Environmental Chemistry, LipidPeroxidation, 0105 earth and related environmental sciences, Chromatography, fungi, 04 agricultural and veterinary sciences, biology.organism_classification, Malondialdehyde, Spore, Membrane, chemistry, Biochemistry, 13. Climate action, 0405 other agricultural sciences, Sciences agricoles
Abstract

International audience; Ozone treatments were applied on conidia aqueous suspensions in order to determine theminimal applied ozone dose to limit conidia germination and to observe the mechanismsinvolved in the spores inactivation. Conidia germination was significantly reduced, bubbling forat least 0.5 min as a gas with a minimal ozone concentration of 1 g.m−3. The applied ozone dosesinduce the membrane phospholipids oxidation, determined by the malondialdehyde quantifica-tion. Membrane phospholipids oxidation and inactivation rate are correlated. So, lipid peroxida-tion and consequently the alteration of the membrane integrity are involved in the antifungalaction of ozone.

Published
2016

34. Decrease of available lysine in thermally treated gelatin followed by LC–UV: Influence on molar mass and ability to helixes’ formation

Author

Khalid Rbii, Noëlle Brambati, Olivier Surel, Anne-Marie Buchert, and Frédéric Violleau

Subjects
Chromatography, food.ingredient, Molar mass, Chemistry, General Chemical Engineering, Al content, Intermolecular force, Lysine, General Chemistry, Thermal treatment, Gelatin, Protein chain, food, Food Science, Nuclear chemistry
Abstract

Available lysine (AL) content, weight-average molar mass (M w ) and kinetic of α helixes’ formation have been determined in thermally treated gelatin (75 °C) during 2, 6 and 8 days. Quantification of available lysine in gelatin sample by LC–UV has been developed. Thermal treatment during 8 days led to a decrease of AL content from 3.1 g/100 g of gelatin to 2.3 g/100 g of gelatin. In the same time, M w increased from 6.7 × 10 5 g mol −1 to more than 2.0 × 10 6 g mol −1 and α helixes’ formation ability was strongly affected. Thermal treatment led to the reaction of available lysine group with other functions present in its environment. Intermolecular cross-links led to a high molar mass compounds’ formation and limited protein chain unfolding which is an essential step for helixes’ formation.

Published
2011

35. Study of gelatin renaturation in aqueous solution by AFlFFF–MALS: Influence of a thermal pre-treatment applied on gelatin

Author

Anne-Marie Buchert, Khalid Rbii, Frédéric Violleau, Olivier Surel, and Noëlle Brambati

Subjects
Pre treatment, Molar mass, Aqueous solution, food.ingredient, Chromatography, Chemistry, General Chemical Engineering, Asymmetrical Flow Field-Flow Fractionation, Multiangle light scattering, General Chemistry, Fractionation, Gelatin, food, Food Science
Abstract

Asymmetrical Flow Field-Flow Fractionation coupled to Multi-Angle Light Scattering has been applied to study and understand the renaturation phenomenon of gelatin in dilute aqueous solutions. Renaturation behaviour has been studied on a native gelatin powder and compared to the same gelatin, pre-heated at 75 °C. An increase of molar mass, due to gelatin chains association at room temperature was observed for native gelatin. AFlFFF–MALS analysis allowed to follow α, β, γ chains association and the occurrence of other fractions with high molar mass. This process was absent in pre-heated gelatin which suggested that pre-heating process could lead to interactions between gelatin chains which limited renaturation process in aqueous solutions. For pre-heated gelatin samples, the average initial molar mass was higher and hardly changed during incubation of a dilute solution.

Published
2011

36. Physicochemical characterization and study of molar mass of industrial gelatins by AsFlFFF-UV/MALS and chemometric approach

Author

Chloé Rochat, Simon Duthen, Frédéric Violleau, Christine Raynaud, Jean Daydé, Didier Kleiber, Cecile Levasseur-Garcia, Ecole d'Ingénieurs de Purpan - EIP (FRANCE), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Institut National de la Recherche Agronomique - INRA (FRANCE), Ecole d'Ingénieurs de Purpan (INPT - EI Purpan), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées, Chimie Agro-Industrielle (CAI), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National de la Recherche Agronomique (INRA), Region Midi-Pyrenees (France) [DESR/12050967], Laboratoire de Chimie Agro-Industrielle (LCA), Institut National de la Recherche Agronomique (INRA)-Ecole Nationale Supérieure de Chimie de Toulouse, Institut National Polytechnique de Toulouse - INPT (FRANCE), and Levasseur-Garcia, Cécile

Subjects
[SDV.SA]Life Sciences [q-bio]/Agricultural sciences, Light, Polymers, Analytical chemistry, lcsh:Medicine, Physical Chemistry, Biochemistry, Gelatin, Scattering, Physicochemical, Viscosity, Animal Products, Materials Physics, Scattering, Radiation, Polymer, lcsh:Science, Materials, chemistry.chemical_classification, Multidisciplinary, Molar mass, Gelatins, Chemistry, Physics, Electromagnetic Radiation, Classical Mechanics, Agriculture, 04 agricultural and veterinary sciences, 040401 food science, Fractionation, Field Flow, Separation Processes, Physicochemical Properties, Macromolecules, Physical Sciences, Molar mass distribution, Research Article, food.ingredient, Materials Science, Multiangle light scattering, Fraction (chemistry), Fluid Mechanics, Research and Analysis Methods, Continuum Mechanics, 0404 agricultural biotechnology, food, lcsh:R, Extraction (chemistry), Light Scattering, Biology and Life Sciences, Proteins, Fluid Dynamics, Elution, Polymer Chemistry, Flow Field, Physical Properties, Molecular Weight, Condensed Matter::Soft Condensed Matter, Chemical Properties, lcsh:Q, Collagens, Sciences agricoles
Abstract

International audience; Industrial gelatins have different physicochemical properties that mainly depend of the raw materials origin and the extraction conditions. These properties are closely related to the molar mass distribution of these gelatins. Several methods exist to characterize molar mass distribution of polymer, including the Asymmetrical Flow Field Flow Fractionation method. The goal of this study is to analyze the relationship between physicochemical properties and the gelatins molar mass distribution obtained by Asymmetrical Flow Field Flow Fractionation. In this study, 49 gelatins samples extracted from pig skin are characterized in terms of gel strength and viscosity and their molar mass distribution are analyzed by Asymmetrical Flow Field Flow Fractionation coupled to an Ultraviolet and Multi Angle Light Scattering detector. This analytical method is an interesting tool for studying, simultaneously, the primary chains and the high-molar-mass fraction corresponding to the polymer chains. Correlation analysis between molar mass distribution data from the different fractions highlights the importance of high molar mass polymer chains to explain the gel strength and viscosity of gelatins. These results are confirmed by an additional chemometric approach based on the UV absorbance of gelatin fractograms to predict gel strength (r2Cal = 0.85) and viscosity (r2Cal = 0.79).

Published
2018

37. Analysis of aged gelatin by AFlFFF-MALS: Identification of high molar mass components and their influence on solubility

Author

Frédéric Violleau, Olivier Surel, Khalid Rbii, and Sylviane Guedj

Subjects
food.ingredient, Chromatography, Molar mass, Chemistry, General Chemical Engineering, Multiangle light scattering, General Chemistry, Fractionation, Food chemistry, Gelatin, Colloid, food, Solubility, Chemical composition, Food Science
Abstract

Gelatin is an important product for several industries and its solubility dramatically influences its functional properties. In order to be able to predict the gelatin behaviour, a new technique for its analysis has been developed with an Asymmetrical Flow Field-Flow Fractionation coupled to a multi-angle light scattering. The AFlFFF-MALS analysis showed the gelatin molar mass ranging from 5 × 10 4 to 2 × 10 7 g mol −1 . This technique also permitted to follow aggregation of gelatin samples after process in an oven at 75 °C. Between 0 and 4 days, some huge aggregates appeared. Their size and density increased without changing gelatin solubility. From 8 to 30 days, the molar mass and density of these aggregates increased leading to partial gelatin insolubilisation in water. This phenomenon is supposed to be due to cross-linking of the gelatin macromolecules.

Published
2009

38. Monomeric pheophorbide(a)-containing poly(ethyleneglycol-b-ε-caprolactone) micelles for photodynamic therapy

Author

Frédéric Violleau, Jean-Pierre Souchard, Naram El-Akra, Katrin Knop, Anne-Françoise Mingotaud, Interactions moléculaires et réactivité chimique et photochimique (IMRCP), Institut de Chimie de Toulouse (ICT), Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Institut Ecologie et Environnement (INEE), Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS)-Fédération de Recherche Fluides, Energie, Réacteurs, Matériaux et Transferts (FERMAT), Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS), IDeAS - Interfaces Dynamiques et Assemblages Stimulables (IDeAS), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie de Toulouse (ICT), Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT), Laboratoire d'Ecologie Microbienne - UMR 5557 (LEM), Institut National de la Recherche Agronomique (INRA)-Université Claude Bernard Lyon 1 (UCBL), and Université de Lyon-Université de Lyon-Ecole Nationale Vétérinaire de Lyon (ENVL)-VetAgro Sup - Institut national d'enseignement supérieur et de recherche en alimentation, santé animale, sciences agronomiques et de l'environnement (VAS)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Chlorophyll, Drug Compounding, Polyesters, Photochemistry, Micelle, Fluorescence spectroscopy, chemistry.chemical_compound, Microscopy, Electron, Transmission, Dynamic light scattering, Cell Line, Tumor, Humans, [CHIM]Chemical Sciences, Photosensitizer, Particle Size, Physical and Theoretical Chemistry, Micelles, Photosensitizing Agents, Singlet Oxygen, Asymmetric flow field flow fractionation, [CHIM.POLY]Chemical Sciences/Polymers, Monomer, Photochemotherapy, chemistry, Pheophorbide A, Nanoparticles, Ethylene Glycols, Nanocarriers
Abstract

Incorporation of unaggregated monomeric molecules of pheophorbide(a) into micelles of poly(ethyleneoxide-b-epsilon-caprolactone) has been characterized by fluorescence spectroscopy, dynamic light scattering, transmission electron microscopy and asymmetric flow field flow fractionation. It was shown that the method used leads to 20 nm micelles, corresponding to approximately 200 molecules of polymer and 4 molecules of monomeric pheophorbide(a) per nano-object which was able to generate (1)O(2) in the medium. They have been used thereafter as nanocarriers for photosensitizers in photodynamic therapy against cancer cells. The encapsulation of photosensitizer has been verified and in vitro tests on human cancerous cells have revealed a ca. 2-fold enhanced photocytotoxicity and cellular uptake compared to free pheophorbide(a).

Published
2009

39. Effect of Oxidative Treatment on Corn Seed Germination Kinetics

Author

Joël Albet, Kheira Hadjeba, Olivier Surel, Frédéric Violleau, and Roland Cazalis

Subjects
Environmental Engineering, Ozone, Corn, biology, Seedling, Kinetics, chemistry.chemical_element, Germination, biology.organism_classification, Oxygen, Horticulture, chemistry.chemical_compound, Root, chemistry, Agronomy, Oxidative treatment, Seeds, Environmental Chemistry, After treatment
Abstract

Corn seeds were treated with high purity oxygen ([O3] = 0 g/m3) and oxygen mixed with ozone ([O3] = 20 g/m3) during 6.8 or 20.5 minutes. Germination tests started immediately or 48 h after treatment. Effects of oxidative treatments on germination were determined by measuring seedlings and roots (>3 and >20 mm) rate at 3, 4 and 5 days of germination test. Results obtained for treated seed samples were higher than for untreated ones. A faster start of germination was observed for treated samples. This early germination start led to a larger number of germinated seeds with longer roots at 4 and 5 days. Nevertheless, too long an ozone treatment seemed to be unfavorable for seed growth, whereas a short one seemed to be most beneficial.

Published
2008

40. In vitro and in planta fungicide properties of ozonated water against the esca-associated fungus Phaeoacremonium aleophilum

Author

Christel Couderc, Frédéric Violleau, Marielle Pagès, Stéphane Compant, Romain J. G. Pierron, Alban Jacques, Centre National de la Recherche Scientifique - CNRS (FRANCE), Ecole d'Ingénieurs de Purpan - EIP (FRANCE), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Institut National de la Recherche Agronomique - INRA (FRANCE), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), Austrian Institute of Technology - AIT (AUSTRIA), Laboratoire de Génie Chimique - LGC (Toulouse, France), Ecole supérieure d'agriculture de Purpan (ESAP), Laboratoire de Génie Chimique (LGC), Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées, Austrian Institute of Technology [Vienna] (AIT), and Institut National Polytechnique de Toulouse - INPT (FRANCE)

Subjects
Fungicide, Esca, Fungus, Horticulture, Biology, Ozonated water, Conidium, [SDV.SA.STA]Life Sciences [q-bio]/Agricultural sciences/Sciences and technics of agriculture, Vitis vinifera L, Botany, Spore germination, Génie chimique, Génie des procédés, [SDV.MP.MYC]Life Sciences [q-bio]/Microbiology and Parasitology/Mycology, Inoculation, fungi, Phaeoacremonium aleophilum, biology.organism_classification, 6. Clean water, 3. Good health, Spore, [SDV.BV.PEP]Life Sciences [q-bio]/Vegetal Biology/Phytopathology and phytopharmacy, Germination, Sciences agricoles
Abstract

Ozone could be used as a sanitary agent in the food and agricultural industries. The present study investigates whether ozonated water could be used to control conidia dispersal of the esca-associated fungus Phaeoacremonium aleophilum. The fungicide properties of ozonated water was firstly assessed in vitro by exposing spores to several concentrations of ozonated water (2.2, 4.5, or 13.5g/m3 of ozone dissolved into water) and observing the germination rate on plate. Secondarily an in planta approach was conducted on grapevine cuttings of cv. Cabernet Sauvignon clone 15. P. aleophilum conidia were inoculated in pruning wounds, which then received ozonated (4.5g/m3) or sterile water. P. aleophilum DNA was quantified by a quantitative polymerase chain reaction (qPCR) 4 and 9 weeks post-inoculation. The effect of ozonated water on plant-defense gene expression was monitored by reverse-transcriptase qPCR (RT-qPCR) 48h post treatment. The results indicate that ozonated water totally suppresses spore germination in vitro. In addition, at 9 weeks post-inoculation, fungal development was significantly reduced by 50% in planta. RT-qPCR analysis shows that ozonated water did not induce plant-defense-related genes 48h post treatment. The fungicide properties of ozonated water and the absence of gene induction in planta make however ozonated water a promising candidate for limiting grapevine infection by P. aleophilum in nurseries.

Published
2015

41. Ozonation of sunflower oils: Impact of experimental conditions on the composition and the antibacterial activity of ozonized oils

Author

Frédéric Violleau, Djamila Ali Haimoud-Lekhal, Sophie Moureu, A. Calmon, Chimie Agro-Industrielle (CAI), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National de la Recherche Agronomique (INRA), Ecole d'Ingénieurs de Purpan (INPT - EI Purpan), and Midi-Pyrenees Region [12050572]

Subjects
Staphylococcus aureus, Linoleic acid, chemistry.chemical_element, Mastitis, Iodine, Biochemistry, Peroxide, Ozonized sunflower oil, Ozonation conditions, chemistry.chemical_compound, Ozone, [SDV.IDA]Life Sciences [q-bio]/Food engineering, Escherichia coli, Humans, Plant Oils, Sunflower Oil, Organic chemistry, [SPI.GPROC]Engineering Sciences [physics]/Chemical and Process Engineering, Food science, Molecular Biology, Organic Chemistry, Streptococcus, Cell Biology, Antimicrobial, Sunflower, Anti-Bacterial Agents, Oleic acid, chemistry, Composition (visual arts), Antibacterial activity, Fatty acid composition
Abstract

International audience; Ozone can react with vegetable oils to produce ozonized oils which have antimicrobial properties and can be used in dermatology. The aim of this study was to evaluate the influence of ozonation conditions and of the initial fatty acid composition on iodine index (II), peroxide index (IP), acidity value (AV) of ozonized sunflower oils. The antibacterial activity of these products against the three bacterial strains that are more often involved in mastitis (Staphylococcus aureus,Escherichia coli and Streptococcus uberis) was also evaluated. In that purpose, two different sunflower oils have been studied: a "classical" oil (55% linoleic acid, 35% oleic acid) and a "high oleic" oil (90% oleic acid). Both were ozonized with or without water during different times (from 1 to 7 h). Results show that the addition of water has a direct impact on the increase in IP (up to 2600 meq of active oxygen/kg of oil with water and 430 without) and AV but does not influence the kinetic of the decrease in II. Minimal inhibitory concentrations were ranging from 1.25 to 40 mg/mL and the antibacterial activity of oils ozonized with water was better than the one of oils ozonized alone. These results are an open door to new applications of ozonized oils.

Published
2015

42. The effect of vegetable protein modifications on the microencapsulation process

Author

Françoise Silvestre, Vanessa Durrieu, Frédéric Violleau, Alla Nesterenko, Isabelle Alric, Laboratoire de Chimie Agro-Industrielle (LCA), Institut National de la Recherche Agronomique (INRA)-Ecole Nationale Supérieure de Chimie de Toulouse, Ecole d'Ingénieurs de Purpan - EIP (FRANCE), Chimie Agro-Industrielle (CAI), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National de la Recherche Agronomique (INRA), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Institut National de la Recherche Agronomique - INRA (FRANCE), and Institut National Polytechnique de Toulouse - INPT (FRANCE)

Subjects
Agronomie, 030309 nutrition & dietetics, General Chemical Engineering, Spray-drying, [SDV.SA.AGRO]Life Sciences [q-bio]/Agricultural sciences/Agronomy, Vegetable Proteins, Modification, Acylation, 03 medical and health sciences, Hydrolysis, Protein acylation, 0404 agricultural biotechnology, Native state, Microencapsulation, Soy protein, Sunflower protein, 0303 health sciences, Chromatography, Chemistry, 04 agricultural and veterinary sciences, General Chemistry, 040401 food science, Spray drying, Emulsion, Food Science
Abstract

International audience; The use of soy proteins (SoyP) and sunflower proteins (SunP) in the microencapsulation by spray-drying technique of α-tocopherol (T) with a core/wall ratio of 2/1 was studied. SoyP and SunP were used as wall material in an unmodified and modified state. The enzymatic (hydrolysis and cross-linking) and chemical (acylation and cationization) modifications were carried out on vegetable proteins in order to improve their encapsulating properties. The results obtained demonstrated that in the native state, SunP showed higher retention efficiency for T microencapsulation (92.6%) compared to SoyP (79.7%), which could be connected to the different composition of protein extracts. Hydrolysis, acylation and cationization of protein resulted in reduced emulsion viscosity. The retention efficiency of T was improved up to 94.8–99.5% after protein acylation, which was attributed to improved affinity between core and wall material.

Published
2014

43. Changes in the glutathione thiol-disulfide status in wheat grain by foliar sulphur fertilization: consequences for the rheological properties of dough

Author

D. Kleiber, Illa Tea, T. Genter, and Frédéric Violleau

Subjects
chemistry.chemical_classification, Chromatography, biology, Protein polymerization, food and beverages, Glutathione, Biochemistry, Gluten, chemistry.chemical_compound, Glutenin, chemistry, Plant protein, biology.protein, Urea, Storage protein, Glutathione disulfide, Food science, Food Science
Abstract

Storage proteins and glutathione in wheat play an important role in gluten network formation and can be modified by supplementation of nitrogen (N) and sulphur (S) in wheat plants. The glutathione thiol-disulfide status and its relationship to the molecular weight distribution wheat polymeric protein and dough rheological properties have been examined after different foliar S fertilizations (S derived from micronized elemental S and NS, a mixture of N urea and elemental S) applied at the post-anthesis stage. Changes in levels of reduced glutathione (GSH), glutathione disulfide (GSSG), polymeric protein-glutathione mixed disulfide (PPSSG) were analysed by reversed phase high performance liquid chromatography, during grain development using the wheat cultivars, Soissons and Tremie. During the grain desiccation phase, S supplementation (i) increased the GSSG/GSH ratio by 23–25% (ii) induced PPSSG accumulation, and (iii) decreased the formation of SDS-unextractable polymeric protein (UPP) and its molecular mass distribution. However, simultaneous N and S supplementation results in: (i) a decrease in PPSSG formation by 20–30% and (ii) an increase of UPP by 7–18% by enhancing both the branching of the aggregated proteins and their molecular weight. The mixograph parameters show that all forms of endogenous glutathione are linked to dough weakening and are negatively correlated with dough mixing tolerance, dough strength and consistency, while UPP is positively correlated with dough strength and consistency. These findings indicate that S nutrition influences dynamics of the glutathione forms in the grain and results in modification the degree of polymerization of storage protein. Thus both the changes in the form of glutathione and protein polymerization influence the rheological properties of dough.

Published
2005

44. Impact of Cultivar and Environment on Size Characteristics of Wheat Proteins Using Asymmetrical Flow Field-Flow Fractionation and Multi-Angle Laser Light Scattering

Author

T. Aussenac, E. Lemelin, L. Salvo, V. Lein, and Frédéric Violleau

Subjects
Field flow fractionation, Chromatography, Chemistry, Sodium, Sonication, Organic Chemistry, Analytical chemistry, Wheat flour, food and beverages, chemistry.chemical_element, Fractionation, Plant protein, Molar mass distribution, Multi-Angle Laser Light Scattering, Food Science
Abstract

The use of multi-angle laser light scattering (MALLS) in conjunction with asymmetrical flow field-flow fractionation (A-FFFF) was investigated for the determination of the molecular weight distribution (MWD) of wheat proteins. The wheat flour proteins were dissolved by sonication in 0.1M sodium phosphate (pH 6.9) containing 2% SDS. The results presented make it evident that efficient separation and size characterization of monomeric (M < 105 g/mol) and polymeric protein (105 ≤ M < 108 g/mol) wheat proteins can be achieved with A-FFFF/MALLS/UV in a single run. Therefore, this method appears to be able to detect significant modifications of MWD of wheat protein, whatever the factor inducing these alterations (i.e., genetic or environmental) and whatever the nature of these alterations (i.e., monomeric-to-polymeric ratio or MWD of polymeric protein). In the present study, we have indeed demonstrated that the MWD of wheat proteins can be altered from one cultivar to another in three main ways: by cha...

Published
2005

45. Optical methyl 2-chloropropionate synthesis by decomposition of methyl 2-(chlorocarbonyloxy)propionate with hexaalkylguanidinium chloride hydrochloride

Author

Frédéric Violleau, Pierre Le Gars, Sophie Thiebaud-Roux, and Elisabeth Borredon

Subjects
inorganic chemicals, chemistry.chemical_classification, Hydrochloride, Organic Chemistry, Inorganic chemistry, Biochemistry, Medicinal chemistry, Chloride, Decomposition, Catalysis, chemistry.chemical_compound, chemistry, Drug Discovery, medicine, Propionate, Nucleophilic substitution, SN2 reaction, Racemization, medicine.drug
Abstract

The decomposition of methyl S-(−)-2-(chlorocarbonyloxy)propionate in the presence of hexaalkylguanidinium chloride hydrochloride was confirmed to correspond to a nucleophilic substitution of the second order. However, racemization occured by the contact between the catalyst and methyl R-(+)-2-chloropropionate ( I ). This phenomenon is caused by the exchange between the chloride ion from catalyst and the chlorine atom of ( I ) according to a SN2 mechanism as well.

Published
2002

46. Polymeric Micelles Encapsulating Photosensitizer: Structure/Photodynamic Therapy Efficiency Relation

Author

Mireille Gaucher, Marie-Pierre Rols, Véronique Pimienta, Ugo Till, Anne-Françoise Mingotaud, Frédéric Violleau, Christophe Chassenieux, Laure Gibot, Pascale Saint-Aguet, Arnaud Lemelle, Béatrice Moukarzel, Patricia Vicendo, Institut de pharmacologie et de biologie structurale (IPBS), Centre National de la Recherche Scientifique (CNRS)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées, Interactions moléculaires et réactivité chimique et photochimique (IMRCP), Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut de Chimie de Toulouse (ICT-FR 2599), Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Institut de Recherche pour le Développement (IRD)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées, Institut de Chimie de Toulouse (ICT-FR 2599), Département Sciences Agronomiques et Agroalimentaires - EI Purpan, Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole d'Ingénieurs de Purpan (INPT - EI Purpan), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), Ecole d'Ingénieurs de Purpan (INPT - EI Purpan), Institut des Molécules et Matériaux du Mans (IMMM), Le Mans Université (UM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université de Toulouse (UT)-Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS), Institut de Chimie de Toulouse (ICT), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Institut Ecologie et Environnement (INEE), Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS)-Fédération de Recherche Fluides, Energie, Réacteurs, Matériaux et Transferts (FERMAT), Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS), Université de Toulouse (UT), Ecole d'Ingénieurs de Purpan (INP - PURPAN), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National Polytechnique (Toulouse) (Toulouse INP), and Université de Toulouse (UT)-Université de Toulouse (UT)

Subjects
Chlorophyll, Light, Polymers and Plastics, Polymers, Polyesters, Chemical structure, Cell Culture Techniques, Bioengineering, Micelle, Polyethylene Glycols, Biomaterials, Lactones, Structure-Activity Relationship, chemistry.chemical_compound, Drug Stability, Dynamic light scattering, Amphiphile, Polymer chemistry, Fluorescence Resonance Energy Transfer, Materials Chemistry, Copolymer, Humans, Scattering, Radiation, [CHIM]Chemical Sciences, Photosensitizer, Micelles, ComputingMilieux_MISCELLANEOUS, Drug Carriers, Photosensitizing Agents, HCT116 Cells, Photochemotherapy, chemistry, Pheophorbide A, Biophysics, Nanomedicine
Abstract

Various polymeric micelles were formed from amphiphilic block copolymers, namely, poly(ethyleneoxide-b-ε-caprolactone), poly(ethyleneoxide-b-d,l-lactide), and poly(ethyleneoxide-b-styrene). The micelles were characterized by static and dynamic light scattering, electron microscopy, and asymmetrical flow field-flow fractionation. They all displayed a similar size close to 20 nm. The influence of the chemical structure of the block copolymers on the stability upon dilution of the polymeric micelles was investigated to assess their relevance as carriers for nanomedicine. In the same manner, the stability upon aging was assessed by FRET experiments under various experimental conditions (alone or in the presence of blood proteins). In all cases, a good stability over 48 h for all systems was encountered, with PDLLA copolymer-based systems being the first to release their load slowly. The cytotoxicity and photocytotoxicity of the carriers were examined with or without their load. Lastly, the photodynamic activity was assessed in the presence of pheophorbide a as photosensitizer on 2D and 3D tumor cell culture models, which revealed activity differences between the 2D and 3D systems.

Published
2014

47. Asymmetrical flow field-flow fractionation with multi-angle light scattering and quasi-elastic light scattering for characterization of polymersomes: comparison with classical techniques

Author

Ugo Till, Anne-Françoise Mingotaud, Bruno Payré, Glenn Hamon, Christophe Chassenieux, Frédéric Violleau, Pascale Saint-Aguet, Jean-Daniel Marty, Mireille Gaucher-Delmas, Dominique Goudounèche, Interactions moléculaires et réactivité chimique et photochimique (IMRCP), Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut de Chimie de Toulouse (ICT-FR 2599), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD), Département Sciences Agronomiques et Agroalimentaires - EI Purpan, Ecole d'Ingénieurs de Purpan (INPT - EI Purpan), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées, Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC), Institut des Molécules et Matériaux du Mans (IMMM), Le Mans Université (UM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Centre de Microscopie Électronique Appliquée à la Biologie (CMEAB), Hôpital de Rangueil, CHU Toulouse [Toulouse]-CHU Toulouse [Toulouse]-Toulouse Réseau Imagerie-Genotoul ( TRI-Genotoul), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées, Institut de Chimie de Toulouse (ICT), Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Institut Ecologie et Environnement (INEE), Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS)-Fédération de Recherche Fluides, Energie, Réacteurs, Matériaux et Transferts (FERMAT), Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS), Ecole d'Ingénieurs de Purpan (INP - PURPAN), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Université de Toulouse (UT), Université de Toulouse (UT), Toulouse Réseau Imagerie-Genotoul ( TRI-Genotoul), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Université Toulouse III - Paul Sabatier (UT3), and Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)

Subjects
education.field_of_study, Materials science, Light, Polyesters, Population, Analytical chemistry, Multiangle light scattering, Equipment Design, Methylmethacrylate, Biochemistry, Molecular physics, Light scattering, Fractionation, Field Flow, Analytical Chemistry, Characterization (materials science), Surface-Active Agents, Polymersome, Analytical light scattering, [CHIM]Chemical Sciences, Scattering, Radiation, Static light scattering, Particle Size, education, Refractive index, ComputingMilieux_MISCELLANEOUS
Abstract

Polymersomes formed from amphiphilic block copolymers, such as poly(ethyleneoxide-b-e-caprolactone) (PEO-b-PCL) or poly(ethyleneoxide-b-methylmethacrylate), were characterized by asymmetrical flow field-flow fractionation coupled with quasi-elastic light scattering (QELS), multi-angle light scattering (MALS), and refractive index detection, leading to the determination of their size, shape, and molecular weight. The method was cross-examined with more classical ones, like batch dynamic and static light scattering, electron microscopy, and atomic force microscopy. The results show good complementarities between all the techniques; asymmetrical flow field-flow fractionation being the most pertinent one when the sample exhibits several different types of population.

Published
2014

48. pH-induced demineralization of casein micelles modifies their physico-chemical and foaming properties

Author

Naaman Francisco Nogueira Silva, Frédéric Gaucheron, Frédéric Violleau, Anne-Laure Fameau, Michel Piot, Antônio Fernandes de Carvalho, Science et Technologie du Lait et de l'Oeuf (STLO), Institut National de la Recherche Agronomique (INRA)-AGROCAMPUS OUEST, Departemento de Technologia de Alimentos, Laboratorio de Leite e Derivados, Universidade Federal de Vicosa (UFV), Département Sciences Agronomiques et Agroalimentaires - EI Purpan, Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole d'Ingénieurs de Purpan (INPT - EI Purpan), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées, Unité de recherche sur les Biopolymères, Interactions Assemblages (BIA), Institut National de la Recherche Agronomique (INRA), Région Bretagne ARED 6188, Institut national d'enseignement supérieur pour l'agriculture, l'alimentation et l'environnement (Institut Agro)-Institut national d'enseignement supérieur pour l'agriculture, l'alimentation et l'environnement (Institut Agro), Ecole d'Ingénieurs de Purpan (INPT - EI Purpan), and Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3)

Subjects
education.field_of_study, Chromatography, Chemistry, General Chemical Engineering, Population, 0402 animal and dairy science, Ionic bonding, 04 agricultural and veterinary sciences, General Chemistry, 040401 food science, 040201 dairy & animal science, Micelle, caséine micelle suspension acidification agrégation mousse, Suspension (chemistry), Demineralization, Colloid, 0404 agricultural biotechnology, Chemical engineering, Ionic strength, Casein, [SDV.IDA]Life Sciences [q-bio]/Food engineering, education, ultracentrifugation lait, [SDV.AEN]Life Sciences [q-bio]/Food and Nutrition, Food Science
Abstract

The organization and functional properties of caseins are influenced by several factors like temperature, pH, ionic environment, ionic strength, casein type and organization. The objective of this work was to prepare suspensions of casein micelles with different mineralization states to study their new physico-chemical and foaming properties. The different suspensions were obtained after milk acidification at various pH values (6.7 as control and 6.4, 6.1, 5.8 and 5.5) and then dialyzed against milk ultrafiltrate to have similar pH values and ionic environment. Each suspension was characterized in terms of i. composition and distribution of minerals and casein molecules between continuous and colloidal phases, ii. physico-chemical characteristics (percentage of sedimentable material, turbidity, particle size distribution, state of aggregation of casein molecules, shape, charge and hydration) and iii. foaming properties (foaming capacity and foam stability). The obtained suspensions were progressively demineralized and partial dissociations of casein micelles were observed. The dissociated part corresponded to non-sedimentable particles by ultracentrifugation. These particles have average diameter of about 20–35 nm and molecular weight between 106 and 107 g mol−1. The proportion of this population smaller in size increased when the pH used to obtain the different casein suspensions was acid (6.7

Published
2013

49. Study of the degradation of pesticides on loaded seeds by ozonation

Author

Joël Albet, Frédéric Violleau, Marc Bourgin, Chimie Agro-Industrielle (CAI), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National de la Recherche Agronomique (INRA), Université Toulouse III - Paul Sabatier (UT3), and Université Fédérale Toulouse Midi-Pyrénées

Subjects
0106 biological sciences, Ozone, 010501 environmental sciences, seeds, 01 natural sciences, 7. Clean energy, 12. Responsible consumption, chemistry.chemical_compound, Imidacloprid, Chemical Engineering (miscellaneous), [SPI.GPROC]Engineering Sciences [physics]/Chemical and Process Engineering, Waste Management and Disposal, pesticide, 0105 earth and related environmental sciences, loaded, Waste management, Process Chemistry and Technology, food and beverages, Human decontamination, Pesticide, decontamination, Pollution, 6. Clean water, Incineration, ozone, chemistry, Degradation (geology), Sewage treatment, 010606 plant biology & botany, Renewable resource
Abstract

International audience; Every year in France, seed producers must downgrade more than 12,000 tons of seeds. These seeds are currently incinerated in cement factories at seed producers’ expenses and non-available for the processes of valorization of renewable resources, due to their significant pesticide content. Consequently, the quantity of pesticides present in the seed loading must be reduced before a subsequent valorization of the downgraded seeds. The purpose of this work is thus to develop a process for the decomposition of a large amount of the pesticides present in the seed loading. Ozonation was proved to be efficient in wastewater treatment for the removal of pesticides of interest, usually present in the seed loading. Consequently, ozone was applied to soft wheat seeds loaded with Gaucho Ble´ loading solution, in a fixed bed reactor. The humidification of seeds before ozonation, the concentration of ozone in the inlet gas and the ozonation time were revealed to be the predominant factors to accelerate the kinetics of degradation of pesticides in the seed loadings. Using optimal conditions (determined by a Box–Behnken experimental design), pesticides were successfully decomposed (respectively 99 and 90% for the degradation of imidacloprid and bitertanol), within 96 min of treatment. The kinetic laws for the ozonation reactions of both pesticides were also determined and the partial orders of the reaction were 1 for both ozone and the pesticide. The subsequent application of this process for the treatment of other loaded seeds showed good degradation yields for all the studied pesticides and demonstrated the interest of such a process for the removal of pesticides on loaded seeds.

Published
2013

50. Kinetic aspects and identification of by-products during the zonation of bitertanol in agricultural wastewaters

Author

Laurent Debrauwer, Joël Albet, Marc Bourgin, Frédéric Violleau, UMR 1010, Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées, Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées, Analyse de Xénobiotiques, Identification, Métabolisme (E20 Metatoul-AXIOM), ToxAlim (ToxAlim), Institut National de la Recherche Agronomique (INRA)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole Nationale Vétérinaire de Toulouse (ENVT), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Ecole d'Ingénieurs de Purpan (INPT - EI Purpan), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National de la Recherche Agronomique (INRA)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-MetaToul-MetaboHUB, Génopole Toulouse Midi-Pyrénées [Auzeville] (GENOTOUL), Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Ecole Nationale Vétérinaire de Toulouse (ENVT), Université Fédérale Toulouse Midi-Pyrénées-Institut National de la Santé et de la Recherche Médicale (INSERM)-Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Université Fédérale Toulouse Midi-Pyrénées-Institut National de la Santé et de la Recherche Médicale (INSERM)-Génopole Toulouse Midi-Pyrénées [Auzeville] (GENOTOUL), Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Institut National de la Santé et de la Recherche Médicale (INSERM), Chimie Agro-Industrielle (CAI), Institut National de la Recherche Agronomique (INRA)-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National Polytechnique (Toulouse) (Toulouse INP), French Ministry (ANRT), Region Midi-Pyrenees [RECH 09005248, RECH 10009504], Université Fédérale Toulouse Midi-Pyrénées-Institut National de la Santé et de la Recherche Médicale (INSERM)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut National de la Santé et de la Recherche Médicale (INSERM)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Génopole Toulouse Midi-Pyrénées [Auzeville] (GENOTOUL), Université Fédérale Toulouse Midi-Pyrénées-Institut National de la Santé et de la Recherche Médicale (INSERM)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), and Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National de la Recherche Agronomique (INRA)

Subjects
Reaction mechanism, Environmental Engineering, Ozone, Health, Toxicology and Mutagenesis, 0207 environmental engineering, 02 engineering and technology, ADVANCED OXIDATION PROCESSES, OZONOLYSIS, 010501 environmental sciences, Standard solution, Wastewater, 01 natural sciences, Waste Disposal, Fluid, Water Purification, AQUEOUS PESTICIDE DEGRADATION, Reaction rate, chemistry.chemical_compound, Reaction rate constant, RATE CONSTANTS, [SDV.IDA]Life Sciences [q-bio]/Food engineering, Environmental Chemistry, WATER, [SPI.GPROC]Engineering Sciences [physics]/Chemical and Process Engineering, 020701 environmental engineering, Dissolution, 0105 earth and related environmental sciences, Bitertanol, Ozonolysis, Chromatography, OZONE, Biphenyl Compounds, Public Health, Environmental and Occupational Health, Agriculture, General Medicine, General Chemistry, Triazoles, Pollution, 6. Clean water, Dilution, Kinetics, chemistry, Seed loading solution, HYDROCARBONS, Oxidation products, Water Pollutants, Chemical, RESISTANCE, OZONATION
Abstract

International audience; The degradation of bitertanol by ozone treatment is investigated. Solutions of bitertanol (8.4 mu g mL(-1)) were prepared either by dissolution of the standard or by dilution of Gaucho Ble seed loading solution and then ozonated under different conditions. Evolution of the concentrations of bitertanol and its ozonation by-products in both solutions was monitored by HPLC-UV as a function of the treatment time for a concentration of 100 g m(-3) of ozone in the inlet gas. Bitertanol degradation was found to follow a pseudo-first order reaction in both cases. However, the rate of the reaction in diluted seed loading solution was much lower (0.19 vs. 0.27 min(-1) in standard solution) and was close to the reaction rate observed in the presence of a radical scavenger, tert-butanol (0.11 min(-1)). Thus, it may be suggested that additives present in the seed loading solution may play the role of radical scavengers. Study of ozone concentration in the inlet gas (from 25 to 100 g m(-3)) showed that ozone degradation is also a first-order reaction with respect to ozone. Four ozonation by-products were highlighted, collected and identified by HPLC coupled with an ion trap mass spectrometer using positive electrospray ionization mode. A degradation pathway of bitertanol was finally proposed. (C) 2012 Published by Elsevier Ltd.

Published
2013

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