17 results
Search Results
2. An LC-MS/MS method for comparing the stability of ethanol's non-oxidative metabolites in dried blood spots during 90 days
- Author
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Hao Wang, Jing Chang, Jiaolun Li, Chengqiang Zhang, Zebin Lin, Yunfeng Zhang, Jingru Wang, Xinyu Zhang, Yulan Rao, Yi Zhang, and Zhibin Huang
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Paper ,Time Factors ,Health (social science) ,Alcohol Drinking ,Glucuronates ,Alcohol ,Glycerophospholipids ,Sulfuric Acid Esters ,Toxicology ,Biochemistry ,Ethyl sulfate ,03 medical and health sciences ,Behavioral Neuroscience ,chemistry.chemical_compound ,0302 clinical medicine ,Ethyl glucuronide ,Drug Stability ,Tandem Mass Spectrometry ,Liquid chromatography–mass spectrometry ,Humans ,Desiccation ,Whole blood ,Detection limit ,Chromatography ,Ethanol ,Filter paper ,Fatty Acids ,General Medicine ,030227 psychiatry ,Neurology ,chemistry ,Oxidation-Reduction ,Biomarkers ,030217 neurology & neurosurgery ,Chromatography, Liquid - Abstract
Problems of stability were found for biomarkers of alcohol consumption: ethyl glucuronide (EtG), ethyl sulfate (EtS), phosphatidylethanols (PEths), and fatty acid ethyl esters (FAEEs) in whole blood. The purpose of this study was to establish a method for the determination of these four kinds of ethanol's non-oxidative metabolites in dried blood spots (DBS) by liquid chromatography tandem mass spectrometry (LC-MS/MS), and to evaluate their stability. In this method, 50 μL of human blood was spotted onto a filter paper for DBS analysis. Samples were extracted by methanol, reconstituted by 2-propanol, and injected into the LC-MS/MS system. Limits of detection were among 0.5–50 ng/mL, and deviations in accuracy and precision were all lower than 15% at three quality control levels. The stability of the four kinds of ethanol non-oxidative metabolites in DBS was investigated during a 90-day range under three temperatures, −20 °C, 4 °C, and 25 °C. EtG and EtS showed a high level of stability in DBS in the 90-day range, regardless of the temperature. FAEEs were unstable after three days. PEths showed stability within 15 days in postmortem DBS and 60 days in antemortem DBS, respectively, at all temperatures.
- Published
- 2020
3. Detection of mephedrone and its metabolites in fingerprints from a controlled human administration study by liquid chromatography-tandem mass spectrometry and paper spray-mass spectrometry
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Vincenzo Abbate, Catia Costa, Min Jang, Andrew T. Kicman, Mark C. Parkin, Joanna Czerwinska, Melanie J. Bailey, Claire George, and Paul I. Dargan
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Male ,Paper ,Metabolite ,Mass spectrometry ,01 natural sciences ,Biochemistry ,Methamphetamine ,Analytical Chemistry ,03 medical and health sciences ,chemistry.chemical_compound ,Mephedrone ,Tandem Mass Spectrometry ,Fingerprint ,Liquid chromatography–mass spectrometry ,Administration, Inhalation ,Electrochemistry ,medicine ,Humans ,Environmental Chemistry ,Sample preparation ,Dermatoglyphics ,Chromatography, High Pressure Liquid ,Spectroscopy ,030304 developmental biology ,0303 health sciences ,Chromatography ,010401 analytical chemistry ,0104 chemical sciences ,Substance Abuse Detection ,Paper chromatography ,chemistry ,Central Nervous System Stimulants ,Quantitative analysis (chemistry) ,medicine.drug - Abstract
The use of synthetic stimulants, including designer cathinones, remains a significant concern worldwide. Thus, the detection and identification of synthetic cathinones in biological matrices is of paramount importance for clinical and forensic laboratories. In this study, distribution of mephedrone and its metabolites was investigated in fingerprints. Following a controlled human mephedrone administration (100 mg nasally insufflated), two mass spectrometry-based methods for fingerprint analysis have been evaluated. The samples deposited on triangular pieces of chromatography paper were directly analysed under ambient conditions by paper spray-mass spectrometry (PS-MS) while those deposited on glass cover slips were extracted and analysed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The LC-MS/MS method was 5-6 times more sensitive than PS-MS but required sample preparation and longer analysis time. Mephedrone was detected in 62% and in 38% of all post-administration samples analysed by LC-MS/MS and PS-MS, respectively. Nor-mephedrone was the only metabolite detected in 3.8% of all samples analysed by LC-MS/MS. A large inter- and intra-subject variation was observed for mephedrone which may be due to several factors, such as the applied finger pressure, angle and duration of contact with the deposition surface and inability to control the 'amount' of collected fingerprint deposits. Until these limitations are addressed, we suggest that the sole use of fingerprints can be a useful diagnostic tool in qualitative rather than quantitative analysis, and requires a confirmatory analysis in a different biological matrix.
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- 2020
4. In vitro hepatic biotransformation of the algal toxin pectenotoxin-2
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Alistair L. Wilkins, Christiane Kruse Fæste, Christopher O. Miles, and Morten Sandvik
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Paper ,endocrine system ,in vitro study ,metabolite ,animal cell ,Wistar rat ,Toxicology ,Algal bloom ,complex mixtures ,Hydrolysis ,male ,In vivo ,lcsh:RA1190-1270 ,controlled study ,rat ,toxin ,liver metabolism ,seco acid ,liquid chromatography-mass spectrometry ,lcsh:Toxicology. Poisons ,Hepatic biotransformation ,Oxidative metabolism ,nonhuman ,Chemistry ,In vitro metabolism ,atom ,liver cell ,aerobic metabolism ,In vitro ,cell suspension ,unclassified drug ,pectenotoxin 1 ,pectenotoxin 2 ,Oxygen atom ,Biochemistry ,hydrolysis ,priority journal ,retention time ,acid ,biotransformation ,oxygen ,pectenotoxin 13 ,pectenotoxin 11 - Abstract
We have investigated the in vitro metabolism of pectenotoxin-2 (PTX-2) using primary hepatocytes from Wistar rats in suspension. Purified PTX-2 was rapidly metabolized. Two major and several minor oxidized PTX-2 metabolites were formed, none of which had retention times corresponding to PTX-1, -11, or −13. Hydrolysis products, such as PTX-2 seco acid, were not observed. Preliminary multi-stage LC-MS analyses indicated that the major hepatic PTX-2 metabolites resulted from the insertion of an oxygen atom at the positions C-19 to C-24, or at C-44. The rapid oxidative metabolism may explain the low oral toxicity of PTXs observed in vivo studies., Highlights • PTX-2 is rapidly metabolized in rat hepatocytes. • Two major and several minor oxidized PTX-2 metabolites were formed. • The results may explain the low oral toxicity of PTXs observed in vivo studies.
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- 2020
5. Ionic liquid based vortex assisted liquid–liquid microextraction combined with liquid chromatography mass spectrometry for the determination of bisphenols in thermal papers with the aid of response surface methodology
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Nasreen Ghazi Ansari, Smita Panchal, Devendra Kumar Patel, G.N.V. Satyanarayana, Ravindra Singh Thakur, and Ankita Asati
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Paper ,Liquid Phase Microextraction ,Bisphenol ,Analytical chemistry ,Ionic Liquids ,010501 environmental sciences ,01 natural sciences ,Biochemistry ,Analytical Chemistry ,Matrix (chemical analysis) ,chemistry.chemical_compound ,Phenols ,Tandem Mass Spectrometry ,Liquid chromatography–mass spectrometry ,Sulfones ,Response surface methodology ,Benzhydryl Compounds ,Chromatography, High Pressure Liquid ,0105 earth and related environmental sciences ,Detection limit ,Chromatography ,Chemistry ,010401 analytical chemistry ,Organic Chemistry ,Extraction (chemistry) ,General Medicine ,Thermal paper ,0104 chemical sciences ,Ionic liquid - Abstract
A sensitive, rapid and efficient ionic liquid-based vortex assisted liquid-liquid microextraction (IL-VALLME) with Liquid Chromatography Mass spectrometry (LC-MS/MS) method is proposed for the determination of bisphenols in thermal paper. Extraction factors were systematically optimized by response surface methodology. Experimental factors showing significant effects on the analytical responses were evaluated using design of experiment. The limit of detection for Bisphenol-A (BPA) and Bisphenol-S (BPS) in thermal paper were 1.25 and 0.93μgkg-1 respectively. The dynamic linearity range for BPA was between 4 and 100μgkg-1 and the determination of coefficient (R2) was 0.996. The values of the same parameters were 3-100μgkg-1 and 0.998 for BPS. The extraction recoveries of BPA and BPS in thermal paper were 101% and 99%. Percent relative standard deviation (% RSD) for matrix effect and matrix match effects were not more than 10%, for both bisphenols. The proposed method uses a statistical approach for the analysis of bisphenols in environmental samples, and is easy, rapid, requires minimum organic solvents and efficient.
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- 2017
6. An improved method for glycosaminoglycan analysis by LC–MS/MS of urine samples collected on filter paper
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Auray-Blais, Christiane, Lavoie, Pamela, Zhang, Haoyue, Gagnon, René, Clarke, Joe T.R., Maranda, Bruno, Young, Sarah P., An, Yan, and Millington, David S.
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GLYCOSAMINOGLYCANS , *LIQUID chromatography-mass spectrometry , *URINALYSIS , *PAPER , *ENZYME deficiency , *METHANOLYSIS , *HEPARAN sulfate , *LYSOSOMAL storage diseases , *BODY fluids - Abstract
Abstract: Background: Mucopolysaccharidoses are complex lysosomal storage disorders caused by any of eleven different enzyme deficiencies resulting in the accumulation of substrates, mainly glycosaminoglycans (GAGs), in various tissues and biological fluids. Method: We developed and validated a urine filter paper methodology for the analysis of GAGs using liquid chromatography–tandem mass spectrometry (LC–MS/MS) for mucopolysaccharidoses type I, type II and type VI patients. We focused on 2 objectives: first, its applicability to high-risk screening, and secondly, to facilitate the collection and shipping of samples to reference centers as part of diagnostic investigation, as well as from treated patients needing to be monitored for assessment of the efficacy of treatment. GAGs in urine dried onto filter paper were extracted and subjected to methanolysis to obtain the repeating disaccharides of the molecules. We devised a multiple reaction monitoring method in positive electrospray ionization mode. Results: The use of deuterated internal standards for dermatan sulfate (DS) and heparan sulfate (HS) reduced a troubling matrix effect. The resulting CVs were <14%. Linearity assessment showed Pearson correlation coefficients of 0.999 and 0.997, for DS and HS, respectively. The stability on filter paper was good for DS and HS for up to 6weeks at various temperatures. Conclusion: We devised a robust and efficient LC–MS/MS methodology for GAGS quantification in urine dried on filter paper and subjected to environmental conditions likely to be encountered during collection, storage and shipping of specimens from referring physicians to medical centers. [Copyright &y& Elsevier]
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- 2012
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7. Determination of Aromatic Amines Released from Azo Dyes in Paper Packaging by Liquid Chromatography-Tandem Mass Spectrometry
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Liu Shanshan, Huimin Deng, Yang Fei, Zhonghao Li, Gangling Tang, Fan Ziyan, Zhaoyang Bian, and Wang Ying
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Paper ,02 engineering and technology ,Tandem mass spectrometry ,01 natural sciences ,Analytical Chemistry ,Sodium dithionite ,chemistry.chemical_compound ,Tandem Mass Spectrometry ,Liquid chromatography–mass spectrometry ,Environmental Chemistry ,Amines ,Coloring Agents ,Pharmacology ,Chromatography ,010401 analytical chemistry ,Extraction (chemistry) ,Food Packaging ,021001 nanoscience & nanotechnology ,0104 chemical sciences ,Food packaging ,Chromatographic separation ,chemistry ,Mass spectrum ,0210 nano-technology ,Citric acid ,Azo Compounds ,Agronomy and Crop Science ,Chromatography, Liquid ,Food Science - Abstract
An LC-tandem MS (LC–MS/MS) method for the determination of 21 kinds of carcinogenic aromatic amines released from azo dyes in food wrappers was used in this research. Sodium dithionite was added to a citric acid buffer medium to reduce and decompose possible azo dyes. The extract was analyzed after liquid–liquid extraction (LLE) and dispersive SPE (d-SPE). The conditions for chromatographic separation, mass spectrum, LLE, and d-SPE were optimized. Under optimal conditions, the LOD was in the range of 0.13–0.35 mg/kg and LOQ in the range of 0.38–1.05 mg/kg, with the addition of standard recoveries of most aromatic amines being ≥80% and RSDs ≤10%. The recoveries for 2,4-diaminotoluene and 2,4-diaminoanisole were significantly lower, being ≤40%. The method was successfully used to analyze 30 practical samples, and the results showed that it is user-friendly, with high sensitivity, rapid control, and low matrix interference.
- Published
- 2016
8. Rotating-disc micro-solid phase extraction of F2-isoprostanes from maternal and cord plasma by using oxidized buckypaper as sorbent membrane
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Roberta Curini, Salvatore Fanali, Velia Purcaro, Giovanni Vento, Patrizia Papacci, Tecla Gasperi, Maria Bianchi, Pierpaolo Tomai, Andrea Martinelli, Alessandra Gentili, Maria Sofia Cori, Luciana Teofili, Tomai, Pierpaolo, Martinelli, Andrea, Gasperi, Tecla, Bianchi, Maria, Purcaro, Velia, Teofili, Luciana, Papacci, Patrizia, Cori, Maria Sofia, Vento, Giovanni, Curini, Roberta, Fanali, Salvatore, and Gentili, Alessandra
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Paper ,Analyte ,Buckypaper ,Calibration curve ,Biological samples ,Carbon nanotubes ,LC–MS ,Sample preparation ,Solid phase extraction ,Adsorption ,F2-Isoprostanes ,Female ,Fetal Blood ,Humans ,Infant, Newborn ,Limit of Detection ,Nanotubes, Carbon ,Pregnancy ,Solid Phase Extraction ,Solvents ,Tandem Mass Spectrometry ,010402 general chemistry ,01 natural sciences ,Biochemistry ,Carbon nanotube ,Analytical Chemistry ,Liquid chromatography–mass spectrometry ,Biological sample ,Nanotubes ,Chromatography ,Chemistry ,Elution ,010401 analytical chemistry ,Organic Chemistry ,Extraction (chemistry) ,Infant ,General Medicine ,Newborn ,biological samples ,buckypaper ,carbon nanotubes ,sample preparation ,solid phase extraction ,analytical chemistry ,biochemistry ,organic chemistry ,Carbon ,0104 chemical sciences ,Settore MED/38 - PEDIATRIA GENERALE E SPECIALISTICA ,Quantitative analysis (chemistry) - Abstract
This paper describes the development of an original micro-solid phase extraction device and its evaluation for the isolation of F2-isoprostanes (F2-IsoPs) from cord and maternal plasma samples. The unit is very simple and consists in a rotating disc (1.8 cm diameter) of oxidized buckypaper (BP), enwrapped in a polypropylene mesh pouch. Even if the selected F2-IsoPs have logP and pKa values that make them suitable candidates for their sorption on BP, several parameters were optimized to maximize recoveries: time of adsorption and desorption; stirring speed; volume, pH and ionic strength of the sample; type, volume, and fractions of the elution solvent; oxidation grade of BP. Among all, the last one was crucial in affecting extraction yields because of the analyte interactions with polar functionalities, introduced by a preliminary oxidative acid treatment. The investigation established the optimal oxidation time and highlighted the pros and cons of the acid activation step. All extracts were analyzed by means of liquid chromatography-tandem mass spectrometry (LC–MS/MS). Validation was performed according to the main FDA guidelines for bioanalytical methods. Depending on the spike level and analyte, recoveries ranged between 30 and 120% with precision and accuracy values lower than 20%. Quantitative analysis was accomplished by matrix-matched calibration curves whose determination coefficients were higher than 0.95. Lower limit of quantitation (LLOQ) spanned the range 2.45–6.77 μg L−1. The validated method was applied to the analysis of eight pairs of mother/child plasma samples, revealing the presence of 8-iso-15-keto-PGF2α and 8-iso-PGE2 at a concentration of about 10 μg L−1 in most cord plasma samples of preterm newborns.
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- 2018
9. A microfluidic paper-based analytical device (μPAD) with smartphone readout for chlorpyrifos-oxon screening in human serum
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Davide Migliorelli, Leos Uttl, Daniel Filippini, Aristeidis S. Tsagkaris, Jana Pulkrabova, and Jana Hajslova
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Paper ,Microfluidics ,02 engineering and technology ,01 natural sciences ,Analytical Chemistry ,law.invention ,Liquid chromatography–mass spectrometry ,law ,Lab-On-A-Chip Devices ,Analytisk kemi ,Humans ,Chromatography ,Microfluidic paper-based analytical device ,Chlorpyrifos ,Chlorpyrifos-oxon ,Lab-on-a-chip ,Wax-printing ,Smartphone readout ,Chemistry ,010401 analytical chemistry ,Acute intoxication ,Paper based ,Microfluidic Analytical Techniques ,021001 nanoscience & nanotechnology ,0104 chemical sciences ,3. Good health ,Smartphone ,Occupational exposure ,0210 nano-technology ,Chlorpyrifos oxon - Abstract
Acute intoxication incidents due to neurotoxic organophosphate (OP) insecticides are occasionally reported, related either to suicidal attempts or occupational exposure due to the misuse of protective equipment. Among them, chlorpyrifos is a compound related to great controversy, which is still authorized and easily accessible in many countries around the world. However, to screen for its exposure markers, instrumental methods are commonly applied, which cannot enable rapid monitoring at an early stage of an intoxication. Therefore, in this study, a microfluidic paper-based analytical device (mu PAD) able to rapidly screen for chlorpyrifos-oxon, the toxic chlorpyrifos metabolite, in human serum was developed and fully validated. The mu PAD combines wax-printed butyrylcholinesterase (BChE) paper sensors, a lab-on-a-chip (LOC) prototype injector and a smartphone as the analytical detector. In principle, the wax-printed strips with adsorbed BChE are embedded into LOC injectors able to deliver samples and reagents on-demand. A smartphone reader was used to monitor the color development on the strips providing binary qualitative results. mu PAD method performance characteristics were thoroughly evaluated in terms of specificity, detection capability (CC beta) and ruggedness. The developed analytical platform is rapid (results within 10 min), cost-efficient (0.70 (sic)), potentially applicable at the point-of-need and attained a low CC beta (10 mu g L-1 in human serum). Finally, mu PAD characteristics were critically compared to wellestablished methods, namely an in-house BChE microplate assay and liquid chromatography tandem mass spectrometry. Funding Agencies|European Unions Horizon 2020 research and innovation program under the Marie Sklodowska-Curie grantEuropean Union (EU) [720325]; METROFOOD-CZ research infrastructure project (MEYS Grant) [LM2018100]; [A2_FPBT_2020_013]
- Published
- 2021
10. A New, Validated Wipe-Sampling Procedure Coupled to LC-MS Analysis for the Simultaneous Determination of 5-Fluorouracil, Doxorubicin and Cyclophosphamide in Surface Contamination
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Christelle Audeval, Christelle Percheron, Christine Bobin-Dubigeon, Pierre Leynia, Marie Amiand, Sophie Rochard, and Jean-Marie Bard
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Paper ,Quality Control ,Antimetabolites, Antineoplastic ,Health, Toxicology and Mutagenesis ,Toxicology ,Mass Spectrometry ,Analytical Chemistry ,Limit of Detection ,Liquid chromatography–mass spectrometry ,Occupational Exposure ,medicine ,Environmental Chemistry ,Doxorubicin ,Antineoplastic Agents, Alkylating ,Cyclophosphamide ,Chromatography, High Pressure Liquid ,Detection limit ,Antibiotics, Antineoplastic ,Chemical Health and Safety ,Chromatography ,Filter paper ,Chemistry ,Extraction (chemistry) ,technology, industry, and agriculture ,Reproducibility of Results ,Reference Standards ,Contamination ,Solutions ,Fluorouracil ,Calibration ,Equipment Contamination ,Indicators and Reagents ,Wipe sampling ,medicine.drug - Abstract
A wipe-sampling procedure followed by a simple liquid chromatography-mass spectrometry method was developed and validated for the simultaneous quantification of three cytotoxic drugs [5-fluorouracil (5FU), doxorubicin and cyclophosphamide (CP)] for the determination of surface contamination. After a solid-phase extraction procedure with wiping filter paper, the separation was performed within 30 min using a gradient mobile phase. The method was validated according to the recommendations of the US Food and Drug Administration. Wiping was performed using Whatman(®) filter paper on different surfaces such as stainless steel, polypropylene and glass. The method was linear, between 10 and 500 ng per wiping sample (i.e., 0.1-5 ng/cm(2)) for 5FU and doxorubicin, and between 1-100 ng per wiping sample (i.e., 0.01-1 ng/cm(2)) for CP. The lower limits of detection and quantification were 5 and 10 ng per wiping sample for 5FU and doxorubicin, and 0.5 and 1 ng per wiping sample for CP. This new sensitive methodology for surface contamination studies was successfully applied on commercial vials and different places in a cancer research hospital. This approach is particularly suitable to assess the risk of occupational exposure to cytotoxic drugs and to optimize the cleaning process, especially for the most toxic molecule studied, CP.
- Published
- 2013
11. Determination of primary aromatic amines in cold water extract of coloured paper napkin samples by liquid chromatography-tandem mass spectrometry
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Eddo Hoekstra, Sandro Valzacchi, Catherine Simoneau, Oguzhan Yavuz, and OMÜ
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Paper ,Toluidines ,Health, Toxicology and Mutagenesis ,Coloring agents ,Food Contamination ,010501 environmental sciences ,Toxicology ,01 natural sciences ,Uhplc ms ms ,Article ,Liquid chromatography–mass spectrometry ,Tandem Mass Spectrometry ,paper napkins ,media_common.cataloged_instance ,Humans ,Primary aromatic amines (PAAs) ,European union ,Amines ,Coloring Agents ,0105 earth and related environmental sciences ,media_common ,Chromatography ,Aniline Compounds ,Food contact ,Chemistry ,010401 analytical chemistry ,Public Health, Environmental and Occupational Health ,Chromatography liquid ,Water ,General Chemistry ,General Medicine ,Original Articles ,Cooking and Eating Utensils ,cold water extract ,0104 chemical sciences ,Europe ,Environmental chemistry ,UHPLC-MS/MS ,Carcinogens ,Maximum Allowable Concentration ,Food Science ,Food contaminant ,International agency ,Chromatography, Liquid - Abstract
WOS: 000380137500017 PubMed: 27146949 The aim of this study was the optimisation of a multi-analyte method for the analysis of primary aromatic amines ( PAAs) from napkins in order to support official controls and food safety. We developed a UHPLC- MS/ MS method for the simultaneous determination of 36 toxicologically relevant PAAs for paper and board. Good regression coefficients of the calibration curves in a range of 0.992- 0.999 and reproducibilities in a range of 2.3- 15% were obtained. Limits of detections ( LODs) were in the range of 0.03-1.4 mu g l(-1) and recoveries were in a range of 21-110% for all the amines. A total of 93 coloured paper napkin samples from different European countries were bought and extracted with water to determine the PAAs. The results showed that 42 of 93 samples contained at least one PAA. More than half of the detected PAAs are considered as toxic, carcinogenic or probably carcinogenic to humans by the International Agency for Research on Cancer ( IARC), or are classified as such in the European Union legislation on chemicals. Summed concentrations of PAAs in seven samples were higher than 10 mu g l(-1), the limit of summed PAA in the European Union plastic food contact material regulation. Also, eight PAAs, classified as Category 1A and 1B carcinogen in the European Union legislation of chemicals, were detected at concentrations higher than 2 mu g l(-1), exceeding the limit proposed by the Federal Institute for Risk Assessment in Germany. Aniline ( n = 14) was most frequently present in higher concentrations followed by o-toluidine, o-anisidine, 2,4-dimethylaniline and 4-aminoazobenzene. Red, orange, yellow and multicoloured paper napkins contained the highest concentrations of total PAAs (> 10 mu g l(-1)). Although the European Union has not harmonised the legislation of paper and board materials and, thus, there is no specific migration limit for PAAs from paper napkins, the present study showed that coloured paper napkins can contain toxic and carcinogenic PAAs at concentrations that are relevant for monitoring.
- Published
- 2016
12. Confirmation of congenital adrenal hyperplasia by adrenal steroid profiling of filter paper dried blood samples using ultra-performance liquid chromatography-tandem mass spectrometry
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Michael Morris, Heather A. Brown, A. Michael Wallace, Claudia Rossi, Scott Gillingwater, Lisa Calton, Paolo Sacchetta, Andrea Urbani, Francesca Petrucci, and Domenico Ciavardelli
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Paper ,Quality Control ,Coefficient of determination ,Clinical Biochemistry ,Tandem mass spectrometry ,Mass spectrometry ,Tandem Mass Spectrometry ,Liquid chromatography–mass spectrometry ,Adrenal Glands ,medicine ,Humans ,Congenital adrenal hyperplasia ,Chromatography, High Pressure Liquid ,Blood Specimen Collection ,Chromatography ,Adrenal Hyperplasia, Congenital ,Filter paper ,medicine.diagnostic_test ,Chemistry ,Settore BIO/12 ,Biochemistry (medical) ,General Medicine ,medicine.disease ,Dried blood spot ,Immunoassay ,Steroids ,Blood Chemical Analysis ,Filtration - Abstract
Background: The specificity of screening for congenital adrenal hyperplasia by direct measurement of 17-hydroxyprogesterone in filter paper dried blood spot samples by immunoassay is low and has a high false-positive rate. In order to reduce the false-positive rate of this test, we developed a rapid, robust, specific confirmatory procedure in which cortisol, 4-androstene-3,17-dione and 17-hydroxyprogesterone were measured simultaneously by ultra-performance liquid chromatography-tandem mass spectrometry. Methods: After extraction, samples were analysed by ultra-performance liquid chromatography-tandem mass spectrometry and 17-hydroxyprogesterone was quantified accurately. Other steroids were determined using stable deuterated internal standards. In total, 25 patient blood spot samples and 92 control samples were analysed. Results: The assay was linear for 17-hydroxyprogesterone, with a coefficient of determination >0.997 and imprecision ≤6.5%. An upper limit of normal for 17-hydroxyprogester-one of 4.45 nmol/L was established by analysing a cohort of samples from unaffected newborns. In addition, a cut-off of 3.5 for the peak areas ratio (17-hydroxyprogesterone+4-androstene-3,17-dione)/cortisol, allows confirmation of the affected steroidogenic enzyme. Conclusions: A high throughput method for the detection of steroids related to congenital adrenal hyperplasia has been developed, allowing the false-positive rate associated with screening for 17-hydroxyprogesterone by immunoassay to be determined.
- Published
- 2011
13. Analysis of isothiazolinone biocides in paper for food packaging by ultra-high-performance liquid chromatography–tandem mass spectrometry
- Author
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H. Song, Bo Li, Qin-Bao Lin, and T.-J. Wang
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Paper ,Spectrometry, Mass, Electrospray Ionization ,Calibration curve ,Health, Toxicology and Mutagenesis ,Analytical chemistry ,Standard solution ,Toxicology ,High-performance liquid chromatography ,Matrix (chemical analysis) ,Isothiazolinone ,chemistry.chemical_compound ,Limit of Detection ,Tandem Mass Spectrometry ,Liquid chromatography–mass spectrometry ,Recycling ,Ultrasonics ,Chromatography, High Pressure Liquid ,Detection limit ,Chromatography ,Chemistry ,Extraction (chemistry) ,Food Packaging ,Public Health, Environmental and Occupational Health ,Reproducibility of Results ,General Chemistry ,General Medicine ,Thiazoles ,Calibration ,Solvents ,Disinfectants ,Food Science - Abstract
A novel and simple method to detect isothiazolinone-type biocides (2-methyl-3-isothiazolinone (MI), 5-chloro-2-methyl-3-isothiazolinone (CMI), 1,2-benzisothiazolinone (BIT) and 2-octyl-3-isothiazolinone (OIT)) in paper used for food packaging by ultrasonic extraction coupled with UPLC-MS/MS was developed. Parameters affecting process efficiency such as extraction solvents, UPLC mobile phase, gradient elution procedure and MS/MS conditions were studied to optimise the operating conditions. Using the optimised gradient elution procedure, the retention time was less than 6 min. The limits of detection (LODs) were found to be between 0.001 and 0.010 mg kg⁻¹, which was validated using actual concentrations. After diluting the standard solution with a blank matrix, the linear calibration curve ranges were 0.002-1.000 mg kg⁻¹ for BIT and OIT, 0.005-1.000 mg kg⁻¹ for MI, and 0.020-1.000 mg kg⁻¹ for CMI, with correlation coefficients higher than 0.9985 (n = 6). A good level of precision with a mean recovery greater than 81.3% and a relative standard deviation (RSD) less than 6.2% were also obtained. A methodology has been proposed for the analysis of isothiazolinones in paper.
- Published
- 2010
14. Detection of methamphetamine and its main metabolite in fingermarks by liquid chromatography-mass spectrometry
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Ruiqin Yang, Xueguo Chen, Ying-jian Xu, and Ting Zhang
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Adult ,Male ,Paper ,Spectrometry, Mass, Electrospray Ionization ,Surface Properties ,Metabolite ,Mass spectrometry ,Pathology and Forensic Medicine ,law.invention ,Methamphetamine ,chemistry.chemical_compound ,law ,Liquid chromatography–mass spectrometry ,Limit of Detection ,medicine ,Humans ,Dermatoglyphics ,Sweat ,Detection limit ,Chromatography ,Reproducibility of Results ,Middle Aged ,Wood ,Amphetamine ,Linear relationship ,chemistry ,Metals ,Extraction methods ,Cotton swab ,Central Nervous System Stimulants ,Female ,Glass ,Law ,Plastics ,medicine.drug ,Chromatography, Liquid - Abstract
A sensitive and efficient method applying liquid chromatography-mass spectrometry for the analysis of methamphetamine and its main metabolite in fingermark deposits was described. Using this method, good linear relationship of methamphetamine was obtained in the range of 0.005μg to 0.5μg per cotton swab, the limit of detection was 1.5ng per cotton swab, the limit of quantitation was 5.0ng per cotton swab and the average values of recovery ratios were above 70.1%. Moreover, the influence factors for the detection of methamphetamine in fingermarks, such as kinds of substrates, development methods and extraction methods, were all discussed in details. The results showed that good recovery ratios could be obtained on painted wood and smooth substrates surfaces. Development methods in commercial powder could not influence the quality of examination of exogenous drug in latent fingermark. Furthermore, the results indicated that the method mentioned here could be applied in the analysis of forensic trace evidences and samples obtained in clinically addicted cases.
- Published
- 2014
15. Detection of ethyl glucuronide in blood spotted on different surfaces
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Wolfgang Weinmann, Annette Thierauf, Eckhard Kaufmann, M. Winkler, Gisela Skopp, D. Thoma, and Andreas Alt
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Male ,Paper ,Time Factors ,Alcohol Drinking ,Surface Properties ,Polyesters ,Alcohol ,Glucuronates ,Mass Spectrometry ,Pathology and Forensic Medicine ,Specimen Handling ,chemistry.chemical_compound ,Forensic Toxicology ,Ethyl glucuronide ,Liquid chromatography–mass spectrometry ,Floors and Floorcoverings ,Humans ,Dried blood ,Whole blood ,Ethanol ,Chromatography ,Elution ,Textiles ,Forensic toxicology ,Temperature ,Hydrocarbons ,chemistry ,Feasibility Studies ,Female ,Glass ,Law ,Chromatography, Liquid - Abstract
This study aims to show that sensitive detection of ethyl glucuronide in dried blood spotted onto various surfaces after a period of 24h is feasible. At present, there is insufficient information how tightly ethyl glucuronide (EtG) binds to various materials and how easily it can be eluted. 4ml aliquots of blood samples obtained from seven volunteers after consumption of alcoholic beverages were applied to six different surfaces. After drying and a 24h-storage at 20±2°C the samples were re-dissolved in water, and EtG was subsequently analyzed by a LC-MS Paul-type ion trap. A comparison was made between dried and corresponding fluid samples. EtG was detectable in all subjects' samples following consumption of alcohol. EtG was also detectable after a storage time of four weeks at 4°C in whole blood that had been preserved with EDTA. EtG was detectable in all samples dried on different surfaces and its concentration remained relatively constant irrespective of the particular condition of the material. Detection of EtG in blood spots from the scene may indicate recent alcohol consumption in cases where collection of blood remained undone or could not be performed.
- Published
- 2010
16. A method for lactate and pyruvate determination in filter-paper dried blood spots
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Tuen-Jen Wang, Chih-Kuang Chuang, Hsuan Liang Liu, Shuan-Pei Lin, Hsiang-Yu Lin, Chun-Yan Yeung, Dar-Shong Lin, Hsin-Tsung Ho, and Wen-Shyang Hsieh
- Subjects
Paper ,Sodium ,chemistry.chemical_element ,Biochemistry ,Analytical Chemistry ,Liquid chromatography–mass spectrometry ,Reference Values ,Tandem Mass Spectrometry ,Pyruvic Acid ,Humans ,Lactic Acid ,Dried blood ,Enzyme Assays ,Chromatography ,biology ,Spots ,Filter paper ,Chemistry ,Organic Chemistry ,Selected reaction monitoring ,Infant, Newborn ,General Medicine ,Reference Standards ,Enzyme assay ,Dried blood spot ,Calibration ,biology.protein ,Regression Analysis ,Filtration ,Chromatography, Liquid - Abstract
Lactic acidemia is commonly associated with severe diseases in pediatric patients. Quantitation of blood lactate and pyruvate is important for the diagnosis and clinical management. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method using dried blood spots (DBS) was developed and could be used for simultaneous quantification of blood lactate and pyruvate. The applicability of the developed method was tested and confirmed by the regression analysis between LC-MS/MS method and enzymatic assay. Lactate and pyruvate were extracted from DBS obtained from 580 full-term, 120 pre-term infants (gestations ranging from 24 to 36 weeks), and 65 patients with suspected lactic acidemia, with methanolic internal standard (IS) solutions of sodium L-lactate-(13)C(3) and pyruvate-(13)C(3). An API-2000 LC-MS/MS system with multiple reaction monitoring (MRM) mode was applied. The within-run and between-run precisions (CV%) were determined and the results were 1.9% and 3.9% for lactate (n=20) and 5.7% and 7.3% for pyruvate (n=20). The linearity of lactate (r=0.9986) and pyruvate (r=0.9973) based on the IS was excellent. The parameter r squared (r(2)) of linear regression between LC-MS/MS method and enzymatic assay was 0.9405 for lactate and 0.9447 for pyruvate, respectively, and the agreement between these methods was consistent and acceptable. The stability of lactate and pyruvate on DBS was also confirmed. The LC-MS/MS method we developed is a specific, sensitive, and reproducible method for measuring blood lactate and pyruvate concentrations. The use of DBS in this method makes it particularly attractive for pediatric patients.
- Published
- 2009
17. Determination of toxic compounds in paper-recycling process waters by gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry
- Author
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Damià Barceló, Anna Rigol, Silvia Lacorte, and A. Latorre
- Subjects
Paper ,Bisphenol A ,Biocide ,Conservation of Natural Resources ,Chromatography ,Chemistry ,Organic Chemistry ,Extraction (chemistry) ,Industrial Waste ,General Medicine ,Mass spectrometry ,Biochemistry ,Gas Chromatography-Mass Spectrometry ,Analytical Chemistry ,Nonylphenol ,chemistry.chemical_compound ,Liquid chromatography–mass spectrometry ,Textile Industry ,Water treatment ,Gas chromatography–mass spectrometry ,Water Pollutants, Chemical ,Chromatography, Liquid - Abstract
Three analytical methods were developed for the determination of toxic compounds in recirculating waters of a paper-recycling industry. Three main groups of compounds were considered: (i) wood extractives originated from the raw material; (ii) biocides added during the production process and (iii) surfactants and other adjuvants present in the formulates of these biocides. Wood extractives considered in this study included fatty and resin acids. They were analysed by liquid–liquid extraction using methyl tert.-butyl ether, followed by gas chromatography–mass spectrometry for previous formation of the respective trimethylsilyl esters. Water samples were also extracted with Oasis HLB (copolymer [poly(divinylbenzene-co-N-vinylpyrrolidone]) solid-phase extraction cartridges of 60 mg and analysed by liquid chromatography–electrospray mass spectrometry for the determination of additives and biocides. Using these two approaches levels up to 15 mg/l for total resin and fatty acids, 5 mg/l for alkylbenzene sulfonates and 2-(thiocyanomethylthio)benzotiazol, 100 μg/l for bisphenol A and 2,2-dibromo-3-nitrilepropionamide, and 300 μg/l for nonylphenol ethoxycarboxylate were detected in process waters at different production treatment stages. These levels are of relevance since poor water quality affects the paper-recycling process, the primary water treatment process and eventually, the environmental water quality.
- Published
- 2002
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