Search

Sitka spruce (Picea sitchensis) needles contain a variety of bioactive compounds including phenolic compounds and flavonoids, many of which have been used in the cosmetic, pharmaceutical, and food industries. This study aimed to investigate the effects of novel extraction techniques, including ultrasound-assisted extraction (UAE), microwave-assisted extraction (MAE) and simultaneous ultrasound–microwave-assisted extraction (UMAE) on the recovery of phenolic, flavonoids and associated antioxidant and anti-cancer properties from Sitka spruce (Picea sitchensis) needles. The ferric reducing antioxidant power (FRAP) assay was used to evaluate the antioxidant capacity, and the Alamar Blue assay using the human brain glioblastoma cancer cell line (U-251 MG) was used to evaluate the cytotoxicity activity. Results showed that US-probe accomplished the highest recovery of phenolic and flavonoids at 38 W cm−2 for 10 min (106.3 ± 2.5 mg GAE g−1 DW and 63.2 ± 3.8 mg QE g−1 DW, respectively). Hence, the highest cytotoxicity activity of IC50 (0.0114% w/v) was achieved by US-probe at 19 W cm−2 for 10 min. However, the antioxidant capacity of (2591.3 ± 92.5 mM TE g−1 DW) was achieved under UMAE at ultrasound intensity of 38 W cm−2, microwave power of 302.4 W for 10 min. This study emphasised the potential application of UAE and MAE in the extraction of bioactive as an environmentally friendly method to be used in the valorisation of by-products in food and agro-industries. This supports the use of renewable natural resources in an efficient way to produce high-value compounds therefore it is in line with the new era of bioeconomy and its new biorefinery concepts yes

The production of pistachio in Tunisia generates a large amount of potentially valuable waste, such as leaves, that could be used as source of bioactive compounds. In this work, the extraction of phytochemicals from Pistacia vera L. leaves (male and female) by microwave-assisted extraction (MAE) has been investigated. A response surface methodology (RSM) was used for the optimization of bioactive compounds extraction, where the independent variables were temperature and extraction time, and the dependent variable was extraction yield. Total phenolic content (TPC), total flavonoid content (TFC), antioxidant activities (DPPH, ABTS, and FRAP) and antimicrobial activity of the extracts obtained at optimal conditions for both leaves were evaluated and compared not only between them, but also with the extracts obtained by maceration. The optimum extraction conditions were 70 ? and 61 ?, and 5.6 and 12 min for male and female leaves respectivily. The best results were achieved for female leaves by MAE with 36% of extraction yield, TPC of 196.35 mg gallic acid equivalents (GAE)/g dry weight (DW), TFC of 83.34 mg catechin equivalents (CE)/g dry weight (DW), and high antioxidant and antimicrobial activities. The evaluation of biological activity of the extracts showed that MAE provides extracts with better antioxidant and antimicrobial capacities then those obtained by maceration. More-over, UPLC-DAD-ESI-MS was performed to confirm the presence of some phenolic compounds in MAE extracts, such as quercetin, apigenin and myricetin derivatives. The results revealed that MAE is an efficient technique for the extraction of active components from Pistacia vera L. leaves. The authors greatly acknowledge the financial support of the Ministry of Higher Education and Scientific Research of Tunisia. L.S. would like to thank to the Spanish Ministry of Universities for the Margarita Salas fellowship for the requalification of the Spanish university system financed by the European Union -Next GenerationEU.

This work designed, modeled and performed economic analysis of the base case extraction and recovery of catechin mix (CM) from Camellia sinensis leaves (CSL) using deep eutectic solvent (DES) and microwave assisted extraction (MAE) with the assistance of SuperPro Designer software. Techno-economic analysis of three commercial scales of manufacture was also investigated and compared using profitability parameters. Sensitivity and uncertainty analyses were further carried out on the most viable commercial scale to determine input variable (s) of highest significance on the profitability of the process. The 3.30 kg CM/batch is the most economically desirable scale with return on investment of 324.65%, payback period of 0.31 year, internal rate of return of 163.83% and net present value of 1,059,595,224. Out of the input variables selected for the sensitivity and uncertainty analyses, CSL and DES costs have the least effect on the selected profitability parameters of the process.

Pomelo peels have been well known as a valuable source of phenolic compounds mainly flavonoids. In this study, the influences of extraction conditions of three extraction methods on the polyphenols yield, flavonoids yield, and antioxidant activity of resulting pomelo flavedo extract (PFE) were evaluated. As a result, the suitable process parameters for the ultrasound assisted extraction were selected at an applied power of 120 W, the temperature of 60 oC for 20 min. Meanwhile, the microwave assisted extraction was operated at an applied power of 150 W for 25 min and the Soxhlet extraction was carried out up to 4 reflux cycles (35 min per cycle) at 80 oC. Among three methods, the microwave assisted extraction was considered as the most efficient method to obtain the high yield of polyphenols (80.56%) and flavonoids (86.58%). Naringin and hesperidin determined by high-performance liquid chromatography showed the value of 64.42 ± 2.90 mg/g DW and 0.97 ± 0.02 mg/g DW, respectively. The PFE extracted by the microwave assisted extraction could be a potent nutraceutical in further application on food or pharmaceutical industries.

Salah satu jenis tanaman mint yang memiliki kandungan minyak atsiri adalah jenis spearmint dengan kandungan carvone sebanyak 60 – 70%. Kandungan tersebut menyebabkan minyak atsiri daun mint memiliki sifat antioksidan, antifungal, dan antibakteri. Proses pengambilan minyak atsiri dengan metode tradisional seperti distilasi uap membutuhkan waktu dan energi yang lebih besar dibandingkan dengan metode Microwave Assisted Extraction (MAE) . Penelitian ini bertujuan untuk mengetahui pengaruh daya microwave (100, 180, dan 300 Watt) dan waktu ekstraksi (5, 10, 15 dan 20 menit) menggunakan metode MAE terhadap yield minyak daun mint. Selain itu, dilakukan karakterisasi sifat fisik yang ditentukan dari warna, indeks bias, densitas, dan komponen penyusun minyak daun mint. Hasil penelitian menunjukkan bahwa daya dan waktu mempengaruhi yield yang dihasilkan. Variasi daya dan waktu terbaik dari hasil penelitian (daya 180 Watt dan waktu 15 menit) menghasilkan yield sebesar 5,17%. Minyak mint yang dihasilkan memiliki warna kuning muda, indeks bias 1,362, dan densitas sebesar 0,8758 gram/mL. Hasil analisis dengan Gas Chromatography – Mass Spectrometry (GC-MS) menunjukkan bahwa komponen terbesar penyusun produk minyak mint hasil penelitian ini adalah carvone sebanyak 71%. Spearmint is one type of mint that contains essential oil with carvone (60-70%) as its main component. That component causes mint’s essential oil has antioxidant, antifungal and antibacteria properties. The traditional method to produce essential oil like steam distillation has long and energy consuming processes. The aims of this research were to investigate the influence of microwave power level (100, 180 and 300 Watt) and the extraction time (5, 10, 15 and 20 minutes) used Microwave Assisted Extraction to mint oil’s yield. Furthermore, characterization determined by oil’s colour, refractive index and density. The analysis of chemical component of mint oil was done using Gas Chromatography – Mass Spectrometry (GC-MS). The power level of microwave and extraction time influence to mint oil’s yield is proven in this research. The highest yield (5.17%) is generated at best variation of power and extraction time from the research are at 180 Watt and 15 minutes extraction time. The colour of mint oil is light yellow, refractive index value is 1.362 and density is 0.8758 gram/mL. The result of GC-MS showed that the major component of mint oil is 71% carvone .

Basal stem rot (BSR) is a devastating disease to Malaysian oil palm. Current techniques employed for BSR disease detection on oil palm are laborious, time consuming, costly, and subjected to accuracy limitations. An ergosterol detection method was developed, whereby it correlated well with the degree of infection in oil palm. This current study was designed to study the relationship between Ganoderma biomass, ergosterol concentration, BSR disease progress and to validate the efficiency of microwave assisted extraction (MAE) method for extraction of ergosterol compound. In addition, testing on the sensitivity of thin layer chromatography (TLC) analysis for detection of ergosterol was also the aim of this study. The optimised procedure involved extracting a small amount of Ganoderma-infected oil palm root tissues suspended in low volumes of solvent followed by irradiation in a conventional microwave oven at 70°C and medium high power for 30 s, resulting in simultaneous extraction and saponification. Based on the results obtained, MAE method may be effective in extracting low to high yields of ergosterol from infected oil palm roots demonstrating disease scale 2, 3 and 4. Positive relationship was observed between ergosterol content and inoculation period starting day 3 in the inoculated oil palm seedlings and hour 6 in germinated seeds. TLC analysis demonstrated a good correlation with high performance liquid chromatography (HPLC) quantification. Therefore, a semi-quantitative TLC analysis may be applied for handling a large amount of samples during onset field survey.

The extraction of proanthocyanidins (PACs), despite being an important and limiting aspect of their industrial application, is still largely unexplored. Herein, the possibility of combining eutectic solvents (ESs) with microwave assisted extraction (MAE) in the extraction of PACs from grape pomace (GP) is explored, aiming to improve not only the extraction yield but also the mean degree of polymerization (mDP). The combination of choline chloride with lactic acid was shown to be the most effective combination for PACs extraction yield (135 mgPAC/gGP) and, despite the occurrence of some depolymerization, also enabled us to achieve the highest mDP (7.13). Additionally, the combination with MAE enabled the process to be completed in 3.56 min, resulting in a considerably reduced extraction time.

The present study aimed to assess the antimicrobial properties of encapsulated lyophilized powdered extracts of pomegranate peels (PP), avocado peels (AP) and avocado seeds (AS) in vitro and in vivo. Minimum Inhibitory Concentration (MIC) and Minimal Bactericidal Concentration (MBC) methods, optical density measurement, and well diffusion assay were used to determine antimicrobial activity against food borne bacteria (Gram− Escherichia coli, Salmonella typhimurium, Campylobacter jejuni, Pseudomonas putida), (Gram+ Staphylococcus aureus, Listeria monocytogenes, Clostridium perfringens, Lactobacillus plantarum), and fungi (Penicillium expansum and Aspergillus niger) based on a mixture design model. Additionally, the most effective powder was studied in vivo in yogurt, cream cheese, and minced meat burger. The samples that contained high polyphenol content also exhibited higher antioxidant, antimicrobial, and antifungal activity. From the results of the well diffusion, the MIC/MBC, and the cell optical density assays, the antimicrobial activity of the extracts was found to be correlated to the total phenolic content (TPC) of the samples and the type of the microorganism. The pomegranate peels extract presented the higher TPC and antioxidant activity and constitute the highest percentage in the most active antimicrobial mixture. The powders that were tested in vitro showed microbial type-dependent effects in each food model. The results presented here can be further studied in the large-scale industrial production of natural food preservatives.

Sargassum polycystum merupakan alga cokelat penghasil polisakarida sulfat yang memiliki aktivitas farmakologi yang menjanjikan. Selama ini metode ekstraksi polisakarida sulfat masih bersifat konvensional (seperti maserasi, sokletasi, dan refluks) yang memerlukan waktu ekstraksi relatif lama (4-6 jam). Penelitian ini bertujuan untuk mengekstraksi polisakarida sulfat menggunakan metode Microwave Assisted Extraction (MAE) serta melakukan uji toksisitasnya. Karakterisasi ekstrak polisakarida sulfat menggunakan spektrofotometer UV-Visible dan Fourier Transform Infrared (FT- IR). Uji toksisitas terhadap larva Artemia salina Leach dilakukan dengan metode Brine Shrimp Lethality Test (BSLT). Hasil ekstraksi polisakarida sulfat diperoleh rendemen sebesar 3,42±0,01% dimana tidak jauh berbeda dari metode konvensional. Hasil perhitungan bobot susut pengeringan polisakarida sulfat 7,60±0,085%. Karakterisasi polisakarida sulfat dengan spektrofotometer UV- Visible diperoleh panjang gelombang optimum pada 270 nm. Hasil spektrum FT-IR terdapat gugus fukosa yang dihubungkan oleh gugus sulfat dan O-Sulfat yang mengindikasikan adanya fukoidan. Selain itu masih ditemukan peregangan ester C=O yang menunjukan adanya asam uronat. Asam tersebut merupakan penyusun alginat dimana bukan merupakan polisakarida sulfat. Dari uji toksisitas diperoleh nilai LC50 polisakarida sulfat terhadap larva A. salina Leach sebesar 113,11 mg/mL yang tergolong kategori toksik. Ekstraksi polisakarida sulfat menggunakan MAE dapat mempercepat waktu ekstraksi dibandingkan dengan metode konvensional, tetapi perlu dilakukan tahap selanjutnya untuk menghilangkan senyawa pengotor lainnya seperti asam uronat. ABSTRACTSargassum polycystum, a brown algae, produces sulfate polysaccharides that have promising pharmacological activity. To date, the extraction of sulfate polysaccharide is still conventional (such as maceration, shoxletation and reflux) and requires a relatively long time (4-6 h). This study aims to extract the sulfate polysaccharides using the Microwave Assisted Extraction (MAE) and assess the toxycity. Sulfate polysaccharide extract was characterized by UV-Visible and Fourier Transform Infrared (FT-IR) spectrophotometer and tested for its toxicity against Artemia salina Leach larvae using the Brine Shrimp Lethality Test (BSLT) method. The yield of sulfate polysaccharide extraction was 3.42±0.01% which is not much different from conventional methods, but the advantage of the MAE method is in terms of time efficiency. The result of the calculation of the drying shrinkage weight of the sulfate polysaccharide is 7.60±0.085%. Characterization of sulfate polysaccharide using a UV-Visible spectrophotometer obtained an optimum wavelength at 270 nm. Based on spectra of FT-IR, it was identified that there are fucose groups which are connected by sulfate and O-Sulfate groups which indicates the presence of fucoidan. In addition, there was still a stretch of ester C=O which indicates the presence of uronic acid. The acid is a constituent of alginate which is not a sulfate polysaccharide. The LC50 value of sulfate polysaccharide against A. salina Leach larvae was 113.11 mg/mL which was classified as toxic. The extraction of sulfate polysaccharides using MAE can speed up the extraction time compared to conventional method, but a further step is needed to remove other impurities such as uronic acid

A study was conducted to develop a rapid, simple microwave assisted extraction (MAE) methods for the extraction of for the polysaccharide from Pithecellobium dulce pods utilizing fundamental principles of “green” chemistry. The plant is reported to be a folk remedy for ear and toothache. It also acts as an emollient, anodyne and larvicidal in folk medicine. As the fruit is liked by common people throughout the country especially by the local residents of Vellore, a scientific investigation on the edible part of the plant was initiated in our laboratory. Optimization of extraction procedures using modern technologies significantly reduces the quantity of solvent consumed and waste generated during an extraction process. Thus microwave assisted extraction combined with soxhlet extraction (MASE) is demonstrated in our lab. Analysis of variance showed that the contribution of the quadratic model was significant for the responses. Under the optimum conditions, the extraction yield of crude polysaccharides was 63.7%. Whereas the combined experimental model (MASE) with 20% alcohol as extracting solvent resulted in the percentage of yield as 72.8%. This chapter outlines a systematic approach for optimization of an extraction procedure for isolation of potential polysaccharide from plant sources. The extracts were tested to determine the total polysaccharide content, total phenolic content and total flavonoid content and the quantitative analysis was correlated with the methods established.

The traditional ways in the extraction of bioactive compounds using conventional methods are disadvantageous from both economic and environmental perspectives. In this, the potential of microwave-assisted hydrodistillation conditions for extraction of phytosterol from legume pods was investigated. Salkowski test performed on the legume pod has shown the reddish brown in all sample which confirmed the presence of phytosterol qualitatively. Liebermann-Burchard procedure and ultraviolet-visible spectroscopy (UV-Vis) apparatus were used to study the concentration of phytosterol at different extraction parameters which are temperature (25–80 °C), solvent concentration (50–100% v/v), irradiation time (1–10 min) and microwave power (400–800 W). The optimal conditions for highest yield of extract (0.219 mg/L) were obtained at a microwave power of 600 W, the irradiation time of 6 min, and ethanol concentration of 75% v/v. Results obtained in this study have shown the capability of microwave-assisted hydrodistillation in the extraction of phytosterol from legume pod. Further works are nevertheless required to provide a deeper understanding of the mechanisms involved to facilitate the development of an optimum system applicable to the industry.

International audience; Microwave is a very efficient energy carrier for the extraction of essential oils from aromatic plants in unit operations intended for distillation. The aim of this work was to compare six extraction processes: four Microwave Assisted Extraction (MAE) and two conventional processes for the extraction of orange essential oils. The comparison was based on different processing and qualitative criteria such as extraction yield, power efficiency, biochemical and sensorial attributes. Two multiple criteria methods were developed to select the most efficient process. The first method is based on the income over energy cost index. The results show that among the set of extraction processes studied only Microwave Hydrodiffusion and Gravity (MHG) would be operational cost efficient. The second method combines both processing and qualitative criteria. The results show that the extraction processes with combination of microwaves and steam are best ranked followed by those with just microwaves.

Phaseolus vulgaris L. has beneficial effects on several chronic non-communicable diseases (e.g., cardiovascular diseases) related to oxidative stress. This redox state may influence platelet activation and aggregation; which is crucial in thrombus formation. In this work, the antiplatelet and antioxidant potential of aqueous extracts obtained by green processes, microwave-assisted extraction and ultrasound-assisted extraction, from 25 landraces of common beans were investigated. Phenol content and antioxidant potential were determined using the Folin-Ciocalteu method, total monomeric anthocyanin and ORAC assay, respectively. The antiplatelet potential of the extracts was explored by turbidimetry. Microwave extraction showed higher phenol content and antioxidant activity in most extracts. Soja landrace extract obtained by microwave-assisted extraction showed higher phenol content and antioxidant activity (893.45 ± 87.30 mg GAE/g and 35,642.85 ± 2588.88 ORAC μmolTE/g, respectively). Although most of the extracts obtained by microwave-assisted extraction showed antiplatelet activity, the extract of Hallado Aleman landrace obtained by ultrasound-assisted extraction (IC50 = 0.152 ± 0.018 mg/mL) had the highest antiplatelet potential. The extraction method, MAE and UAE, influences the biological potential of the beans, specifically the antiplatelet activity and antioxidant activity. The functional value of this legume for direct consumption by the population was evidenced, as well as its inclusion in food formulations.

Currently, exploration of natural dyes is increasingly being activated and developed, especially to find natural sources of dyes from different plant species and also to develop natural dyestuff extraction process technology for textile applications. During this natural dye extraction process is done by conventional methods that require a long time and a large amount of solvent. Therefore, it is a necessary alternative to the use of "green techniques" are economical in its use. In this research, extraction of Jackfruit wood waste with the microwave by studying the extraction time required to produce the optimum yield and comparing with the conventional method (heat-reflux extraction). Both of these methods use water solvent. On the microwave-assisted extraction, the optimum extraction time at 30 minutes with the acquisition yield of 3.14% (microwave power 400 watt, the ratio of material to solvent 0.02 g/mL). Whereas extraction with heat-reflux method showed the optimum extraction time of 180 minutes with a yield of 3.50%. Identification of groups of pigments contained in the Jackfruit wood waste is known categories tannin, flavonoid, and quinone. Fourier Transform Infrared Spectroscopy was used to identify the major chemical groups in the extracted dye. Description of the effects of extraction with microwave and conventional, structural damage shown in a solid surface material using by Scanning Electron Microscopy. Further, the test for dyeing the fabric was obtained as a brown color are more dominant in a natural dye compared to textile dye.

Olea europaea L. leaves constitute a source of bioactive compounds with recognized benefits for both human health and technological purposes. In the present work, different extracts from olive leaves were obtained by the application of two extraction methods, Soxhlet and microwave-assisted extraction (MAE), and six solvents (distilled water, ethanolic and glycerol mixtures solvents). MAE was applied under 40, 60 and 80 °C for 3, 6.5 and 10 min. The effect of the extraction method, solvent and treatment factors (the latter in MAE) on the total phenol content (TPC), the antioxidant activity (AA) and the phenolic profile of the extracts were all evaluated. The extracts showed high values of TPC (up to 76.1 mg GAE/g DW) and AA (up to 78 mg TE/g DW), with oleuropein being the most predominant compound in all extracts. The Soxhlet extraction method exhibited better yields in TPC than in MAE, although both methods presented comparable AA values. The water MAE extract presented the strongest antimicrobial activity against five foodborne pathogens, with minimum inhibitory concentration (MIC) values ranging from 2.5 to 60 mg/mL. MAE water extract is proposed to be exploited in the food and nutraceutical industry in the frame of a sustainable economy.

Namen magistrskega dela je bil ovrednotiti vpliv metod ekstrakcije na biološko aktivnost izvlečkov iz listov koprive (Urtica dioica L.) ter iz semen koromača (Foeniculum vulgare). Izvlečke smo pripravili s pospešeno ekstrakcijo (ASE), ekstrakcijo z mikrovalovi (MAE) ter refluksno ekstrakcijo. Izvlečkom smo določili vsebnost skupnih fenolnih spojin (TPC), ki je bila 504 ± 26 – 3301 ± 171 mg GAE/100 g s.s. za liste koprive ter 237 ± 10 – 860 ± 26 mg GAE/100 g s.s. za semena koromača. Fenolni profil smo analizirali z UPLC-MS/MS. V izvlečkih listov koprive smo identificirali 27 različnih spojin, med katerimi sta močno prevladovala cimetna kislina ter kemferol, v izvlečkih semen koromača pa je bila med 21 identificiranimi spojinami prevladujoča spojina kemferol-3-O-glukuronid. Optimalna metoda ekstrakcije bioaktivnih spojin iz listov koprive je bila ASE, za semena koromača pa klasični refluks, pri obeh s 30 % acetonom kot topilom. Ob upoštevanju optimalnih pogojev ekstrakcije smo pripravili nova izvlečka in jima določili antioksidativni potencial (DPPH, FRAP) in protimikrobno aktivnost z metodo mikrodilucije. Izvlečki listov koprive so izkazali boljšo antioksidativno kot tudi protimikrobno aktivnost v primerjavi z izvlečki semen koromača, kar sovpada z vrednostmi TPC. Oba izvlečka sta zavirala rast seva P. fragi (MIK = 0,5 mg/mL za izvleček listov koprive, MIK = 2 mg/mL za izvleček semen koromača), medtem ko je le izvleček listov koprive deloval inhibitorno proti sevu S. aureus (MIK = 2 mg/mL). Ostale testirane bakterije in kvasovke na izvlečka niso bile občutljive. The aim of this work was to evaluate the impact of different extraction methods on bioactivity of the extracts from nettle (Urtica dioica L.) leaves and fennel (Foeniculum vulgare) seeds. Extracts were obtained by using accelerated solvent extraction (ASE), microwave assisted extraction (MAE) and heat reflux extraction. Total phenolic content (TPC) was determined and ranged from 504 ± 26 to 3301 ± 171 mg GAE/100 g dw in nettle leaves extracts and from 237 ± 10 to 860 ± 26 mg GAE/100 g dw in fennel seeds extracts. Phenolic profile analyses were carried out by UPLC-MS/MS. In total, 27 different compounds were identified in nettle leaves extracts, among those cinnamic acid and kaempferol were far the most abundant in all the extracts while kaempferol-3-O-glucuronide was identified as the most dominant among 21 compounds found in fennel seeds extracts. ASE proved to be optimal method for the extraction of bioactive compounds from nettle leaves, while classical heat reflux for fennel seeds, for both using 30 % acetone as a solvent. Based on the optimal extraction conditions, new extracts were prepared for which antioxidative potential (DPPH, FRAP) and antimicrobial activity using microdilution method were determined. Nettle leaves extract showed both, better antioxidative and antimicrobial activity, compared to fennel seeds extract, which correlated also with TPC values. Both extracts had antimicrobial effect on P. fragi (MIC = 0,5 mg/mL for nettle leaves extract and MIC = 2 mg/mL for fennel seeds extract) while only nettle leaves extract had an inhibitory effect against S. aureus (MIC = 2 mg/mL). Other bacteria and yeasts tested were not sensitive to the extracts.

Bu çalışmada ekstraksiyon yöntemlerine özgü işlem değişkenlerinin (pH, sıcaklık, süre, hız/genlik/güç) pektin verimi üzerindeki etkisini incelemek amacıyla, iki materyal (karpuz ve nar kabuğu) ve üç yöntem ile (klasik çözgen ekstraksiyonu, ultrason destekli ekstraksiyon, mikrodalga destekli ekstraksiyon) pektin ekstraksiyonu gerçekleştirilmiştir. Box-Behnken deneme dizaynına göre her materyal için, beşi merkez noktada olmak üzere klasik çözgen ekstraksiyonu ve ultrason destekli ekstraksiyon için 29, mikrodalga destekli ekstraksiyon için 17 deneme yapılmıştır. Yanıt yüzey yöntemi kullanılarak Box-Behnken deneme dizaynına göre ekstraksiyon işlem koşulları, maksimum pektin verimi yanıt olarak seçilerek optimize edilmiştir. Elde edilen verilerin regresyon analizi sonucu yanıt için pH, sıcaklık, süre, hız/genlik/güç değişkenlerine bağlı olarak ikinci dereceden polinomiyal denklem oluşturulmuştur. Modele göre belirlenmiş optimum işlem koşullarında üç deneme yapılmış ve optimum nokta deneysel olarak da doğrulanmıştır. Optimum koşullarda elde edilen pektin verimleri klasik çözgen ekstraksiyonunda; karpuz kabuğu için %7.39 (pH 2.1, sıcaklık 94ºC, süre 131 dakika, hız 521 rpm), nar kabuğu için %17.39 (pH 2.5, sıcaklık 90ºC, süre 134 dakika, hız 485 rpm) olarak bulunmuştur. Ultrason destekli ekstraksiyonda en yüksek verim; karpuz kabuğu için %8.16 (pH 1.0, sıcaklık 90ºC, süre 22 dakika, %44 genlik), nar kabuğu için %11.56 (pH 1.5, sıcaklık 69ºC, süre 29 dakika, %32 genlik) olarak bulunmuştur. Mikrodalga destekli ekstraksiyonda en yüksek verim; karpuz kabuğu için %9.40 (pH 1.3, süre 6 dakika, güç 596 W), nar kabuğu için %9.86 (pH 1.2, süre 4 dakika, güç 614 W) olarak bulunmuştur. Optimum koşullarda üretilen 6 çeşit pektin; nem içeriği, kül miktarı, protein içeriği, metil esterifikasyon derecesi, galakturonik asit içeriği, ferulik asit içeriği, görünür viskozite ve akış özelliklerinin belirlenmesi, emülsiyon stabilitesi ve mikroskobik yapı, nötralize şeker içeriği, molekül ağırlığı ve FTIR spektroskopisi analizleri yapılarak karakterize edilmiştir. Karpuz kabuğu pektinlerinden, en yüksek protein içeriği (%15.12), metil esterifikasyon derecesi (%48.16), ferulik asit içeriği (%0.36), viskozite (0.0672 Pa.s) ve molekül ağırlığı (65.07 kDa) ile en düşük kremleşme indeksine (%23.04) sahip olan örnek, mikrodalga destekli ekstraksiyon yöntemi ile elde edilen olmuştur. Nar kabuğu pektinlerinden ise, en yüksek protein içeriği (%5.72), metil esterifikasyon derecesi (%70.92), ferulik asit içeriği (%1.49), viskozite (0.1401 Pa.s) ve molekül ağırlığı (232.27 kDa) ile en düşük kremleşme indeksine (%0.00) sahip olan örnek, ultrason destekli ekstraksiyon yöntemi ile elde edilen olmuştur. Bunlara ek olarak, örneklerin pektin verimi ve bu örneklerden hazırlanan emülsiyonların mikroskobik yapıları değerlendirildiğinde en iyi emülsifiye edici özelliğe sahip pektinler, karpuz kabuğu için mikrodalga destekli ekstraksiyon yöntemi ile elde edilen, nar kabuğu için ise ultrason destekli ekstraksiyon yöntemi ile elde edilen olmuştur. Seçilen iki adet pektinin dondurma üretiminde emülsifiye edici madde yerine kullanımını değerlendirmek üzere dondurma üretimi gerçekleştirilmiştir. Pektin ilavesinin ilk damlama süresini uzattığı, dondurma hacmini kısmen, viskozite ve sertliği ise önemli düzeyde artırdığı bulgulanmıştır., In this study, in order to examine the effect of process variables (pH, temperature, time, speed/amplitude/power) of different extraction methods on the pectin yield, pectin extraction was performed with two waste materials (watermelon and pomegranate peel) and three different extraction methods (classical solvent extraction, ultrasonic assisted extraction, microwave assisted extraction). According to the Box-Behnken trial design, 29 trials for classical solvent extraction and ultrasonic assisted extraction and 17 trials for microwave assisted extraction were performed for each material, five at the center point. Using the response surface method, the extraction process conditions were optimized according to the Box-Behnken experiment design by selecting the maximum pectin yield as the response. The regression analysis of the obtained data showed that, a quadratic polynomial equation was formed for the response depending on the variables of pH, temperature, time, speed/amplitude/power. At three trials were carried out at the optimum conditions determined from the model, and the optimum point was verified experimentally. Pectin yields obtained under optimum conditions in classical solvent extraction; 7.39% (pH 2.1, temperature 94ºC, time 131 min, speed 521 rpm) for watermelon peel and 17.39% (pH 2.5, temperature 90ºC, time 134 minutes, speed 485 rpm) for pomegranate peel. Highest efficiency in ultrasonic assisted extraction was found as 8.16% (pH 1.0, temperature 90ºC, time 22 minutes, 44% amplitude) for watermelon peel and 11.56% (pH 1.5, temperature 69ºC, time 29 minutes, 32% amplitude) for pomegranate peel. Highest yield in microwave assisted extraction was 9.40% (pH 1.3, time 6 minutes, power 596 W) for watermelon skin and 9.86% (pH 1.2, time 4 minutes, power 614 W) for pomegranate peel. 6 pectin samples produced under optimum conditions were characterized as moisture content, ash content, protein content, methyl esterification degree, galacturonic acid content, ferulic acid content, determination of apparent viscosity and flow properties, emulsion stability and microscopic structure, neutralized sugar content, molecular weight and FTIR spectroscopy. Among the watermelon peel pectins, the highest protein content (15.12%), methyl esterification degree (48.16%), ferulic acid content (0.36%), viscosity (0.0672 Pa.s) and molecular weight (65.07 kDa) with lowest degree of creaming (23.04%) was obtained by microwave assisted extraction method. Among the pomegranate peel pectins, the highest protein content (5.72%), methyl esterification degree (70.92%), ferulic acid content (1.49%), viscosity (0.1401 Pa.s) and molecular weight (232.27 kDa) with lowest degree of creaming (0.00%) was obtained by ultrasound assisted extraction method. In addition, when the pectin yield of the samples and the microscopic structures of the emulsions prepared from these samples were evaluated, the pectins with the best emulsifying properties were obtained by microwave assisted extraction method for watermelon peel and ultrasound assisted extraction method for pomegranate peel. Ice cream production was carried out to evaluate the use of two selected pectins instead of emulsifiers in ice cream production. It was found that the addition of pectin prolongs the first dripping time, partially increases the volume of ice cream, and significantly increases the viscosity and hardness.

International audience; Microwave assisted extraction (MAE) was investigated for the extraction of total saponins compounds from the starfish Echinaster sepositus. In order to achieve optimization of microwave extraction and to determine the influence of each operational variable (the solvent concentration (X1), irradiation time (X2), microwave power (X3), and liquid-solid ratio (X4)) on the extraction of saponins, response surface methodology (RSM) coupled with a Box–Behnken design (BBD) was applied. The optimized experimental conditions were 58.7 % aqueous methanol as solvent, 177 W as microwave power for 3 min irradiation time at 43.6 mL g−1 of liquid-solid ratio. The extraction yield under these conditions was 60.3 ± 0.6 mg g−1. The optimized MAE was compared with other methods, ultrasound assisted extraction (UAE) and with conventional solvent extraction (CSE). It was demonstrated that microwave produced saponins extraction 7.8 times as more as that produced by CSE and 3.3 as more as UAE has produced. From the in vitro hemolytic tests and electro-generated O2[rad]− quenching tests, we have noted that the microwave saponins extract was the most active one comparing with both UAE and CSE extracts.

Bu tez çalışmasında, karpuz kabuğundan geleneksel ve mikrodalga destekli ekstraksiyon ile pektin eldesi üzerine çalışılmıştır. Geleneksel yöntemle pektin ekstraksiyonunda etkili parametreler olan sıcaklık (45-95 °C), katı/sıvı oranı (1:10–1:50 g/mL), süre (40-240 dk), pH değeri (1-4) yanıt yüzey metodu ile optimize edilmiştir. Optimum koşulda sıcaklık 82,43 °C, katı/sıvı oranı 1:20g/mL, süre 189,6 dk ve pH değeri 1,75 olarak belirlenerek kuru maddede pektin verimi %15 bulunmuştur. Geleneksel ekstraksiyondaki pektin verimini arttırmak için mikrodalga destekli ekstraksiyon uygulamasında sanayi tipi mikrodalga gücü 16000 W olan sistemde 2 dk’lık uygulama sonucu örnek sıcaklığı 85±2 °C’ye ulaşmış, pektin verimi kuru maddede %17,19 olarak bulunmuştur. Elde edilen pektinlere, aronya ekstraktı, CaCl2 ve gliserol eklenerek yenilebilir film üretilmiştir. Çilek ve küp kesilmiş elmaların raf ömrünü arttırmak için bu filmlerle kaplama işlemi uygulanmıştır. Çilekler +5°C’de 16 gün, küp elmalar +5°C’de 7 gün depolanarak kalite analizleri gerçekleştirilmiştir. Mikrodalga pektinle kaplanmış çilek ve küp elmaların toplam fenolik madde miktarı depolama sonunda kontrol örneğe göre sırasıyla %44,27 ve %46,07 daha yüksek bulunmuştur. Mikrodalga destekli pektin ekstraksiyonun kısa sürede yüksek verimde pektin eldesine ve daha iyi film oluşturarak meyvelerin raf ömrüne olumlu etkisi olduğu belirlenmiştir.

Polybrominated diphenyl ethers (PBDEs) are a class of persistent organic pollutants (POPs) widely used as flame retardants in a variety of everyday household products.[1] They easily migrate and can enter the human organism through contaminated food and inhalation/ ingestion of house dust, which are the main routes of human exposure.[2] PBDEs are lipophilic, hence, they accumulate in human milk, the most commonly used biological matrix for monitoring POP concentrations in humans.[3] Microwave-assisted extraction (MAE) has a number of advantages, such as lower solvent consumption and processing time, reduced analyte loss as well as higher sample throughput, but it is applied almost exclusively for solid samples. This is the first application of MAE to human milk samples - the influence of sample preparation and pretreatment were investigated, and extraction conditions (type and volume of solvent, temperature) were optimized. PBDEs were extracted from freeze-dried milk dissolved in ultrapure water with n-hexane:acetone (1:1, v/v) and formic acid and 2-propanol as denaturing agents were added at 80 °C for 20 min. Analytical recoveries ranged from 60 to 72 %, with good repeatability (RSD 4-9 %). Undoubtedly, MAE has the potential for future use in PBDE extraction from human milk and could, under appropriate conditions, be applied in the trace analysis of other POPs from liquid samples.

19 Páginas.-- 6 Figuras.-- 2 Tablas, Olea europaea L. leaves constitute a source of bioactive compounds with recognized benefits for both human health and technological purposes. In the present work, different extracts from olive leaves were obtained by the application of two extraction methods, Soxhlet and microwave-assisted extraction (MAE), and six solvents (distilled water, ethanolic and glycerol mixtures solvents). MAE was applied under 40, 60 and 80 °C for 3, 6.5 and 10 min. The effect of the extraction method, solvent and treatment factors (the latter in MAE) on the total phenol content (TPC), the antioxidant activity (AA) and the phenolic profile of the extracts were all evaluated. The extracts showed high values of TPC (up to 76.1 mg GAE/g DW) and AA (up to 78 mg TE/g DW), with oleuropein being the most predominant compound in all extracts. The Soxhlet extraction method exhibited better yields in TPC than in MAE, although both methods presented comparable AA values. The water MAE extract presented the strongest antimicrobial activity against five foodborne pathogens, with minimum inhibitory concentration (MIC) values ranging from 2.5 to 60 mg/mL. MAE water extract is proposed to be exploited in the food and nutraceutical industry in the frame of a sustainable economy., The authors are grateful to the Ministry of Economy and Competitiveness of Spain for funding this research through the project CTQ2016-78729-R, to the Andalusian research project PY18-616 (Plan for Research, Development and Innovation 2020), and to the Andalusian knowledge transfer project AT17-5927 co-funded by the European Regional Development Fund instrument (ERDF Andalusian Operative Programme 2014–2020).

A sequential extraction process has been designed for valorizing globe artichoke plant residues and waste (heads, leaves, stalks, and roots left in the field) by means of green extraction techniques according to a biorefinery approach. We investigated two cascading extractions based on microwave-assisted extractions (MAE) and green solvents (water and ethanol) that have been optimized for varying temperature, solvent and extraction time. In the first step, phenols were extracted with yields that ranged between 6.94 mg g&minus, 1 dw (in leaves) and 3.28 mg g&minus, 1 dw (in roots), and a phenols productivity of 175.74 Kg Ha&minus, 1. In the second step, inulin was extracted with impressive yields (42% dw), higher than other conventional inulin sources, corresponding to an inulin productivity of 4883.58 Kg Ha&minus, 1. The remaining residues were found to be valuable feedstocks both for bioenergy production and green manure (back to the field), closing the loop according to the Circular Economy paradigm.

U okviru ove disertacije ispitane su mogućnosti primene savremenih metoda za dobijanje tečnih ekstrakata (ultrazvučna ekstrakcija, mikrotalasna ekstrakcija i ekstrakcija subkritičnom vodom) i lipofilnih ekstrakata (ekstrakcija superkritičnim ugljendioksidom) bogatih polifenolima iz nadzemnog dela očajnice (Marrubium vulgare L.). Tečni ekstrakti su optimizovani primenom eksperimentalnog dizajna i metode odzivne površine, i podvrgnuti su spray drying tehnici sušenja. Tečni i suvi ekstrakti su detaljno ispitani po pitanju hemijskog sastava i biološke aktivnosti, antimikrobne i in vitro antihiperglikemijske aktivnosti.Za svaku od navedenih ekstrakcionih tehnika ispitan je uticaj glavnih parametara: ultrazvučna ekstrakcija (temperatura, vreme ekstrakcije i snaga ultrazvuka), mikrotalasna ekstrakcija (koncentracija etanola, vreme ekstrakcije i snaga mikrotalasa) i ekstrakcija subkritičnom vodom (temperatura, vreme ekstrakcije i koncentracija HCl u ekstragensu). Kod tečnih ekstrakata dobijenih ultrazvučnom i mikrotalasnom ekstrakcijom na optimizovanim uslovima utvrđeno je prisustvo hlorogenske kiseline i kvercetina koji nisu detektovani u maceratima. Ispitana je antimikrobna aktivnost oba ekstrakta i utvrđeno da je B. cereus najosetljiviji bakterijski soj, dok je u slučaju kvasaca S. cerevisiae posebno osetljiv na oba ekstrakta. Pored ove aktivnosti ispitana je i in vitro antihiperglikemijska aktivnost oba ekstrakta prema α-amilazi i α-glukozidazi, pri čemu ultrazvučni ekstrakt pokazuje veću antihiperglikemijsku aktivnost (50,63% inhibira α-amilazu i 48,67% inhibira α-glukozidazu) što se potencijalno može objasniti prisustvom hlorogenske kiseline (33,11 μg/mL) i kvercetina (34,88 μg/mL). U subkritičnom ekstraktu, dobijenom na optimalnim uslovima, detektovano je jedino prisustvo hidroksi metilfurfurala usled čega ovaj ekstrakt nije podvrgnut ispitivanju antimikrobne i antihiperglikemijske aktivnosti.U cilju ekstrakcije lipofilnih komponenata M. vulgare primenjene su destilacija etarskog ulja (0,05%), Soxhlet ekstrakcija (3,23%) i ekstrakcija superkritičnim ugljendioksidom na pritiscima 100, 200 i 300 bar i temperaturama 40, 50 i 60 °C. Najdominantnija komponenta u svim dobijenim superkritičnim ekstraktima je hemotaksonomski marker marubiin koji nije identifikovan u Soxhlet ekstraktu.Tečni ekstrakti dobijeni ultrazvučnom i mikrotalasnom ekstrakcijom na optimizovanim uslovima i macerat su osušeni spray drying tehnikom (uz dodatak 10 i 50% maltodekstrina) u cilju dobijanja stabilnije forme suvog ekstrakta. Suvim ekstraktima su određene najznačajnije fizičke osobine i hemijski sastav kao i antimikrobna i antihiperglikemijska aktivnost kako bi se procenila mogućnost njihove inkorporacije u funkcionalnu hranu, dijetetske suplemente ili u formulaciji različitih gotovih proizvoda koji se primenjuju preventivno ili radi poboljšanja zdravlja ljudi., Within the scope of this dissertation, the possibilities of applying modern methods for obtaining liquid (ultrasonic extraction, microwave extraction and subcritical water extraction) and lipophilic extracts (extraction with supercritical carbon dioxide) rich in polyphenols from the aboveground part of white horehound (Marrubium vulgare L.) were examined. Liquid extracts were optimized using an experimental design and response surface method, and subjected to spray drying. Liquid and dry extracts have been extensively examined for their chemical composition and biological activity, antimicrobial and in vitro antihyperglycaemic activities.For each of these extraction techniques, the influence of the main parameters was examined: ultrasonic extraction (temperature, extraction time and ultrasound power), microwave extraction (ethanol concentration, extraction time and microwave power) and subcritical water extraction (temperature, extraction time and HCl concentration in the extractant). Liquid extracts obtained by ultrasonic and microwave extraction under optimized conditions revealed the presence of chlorogenic acid and quercetin, which were not detected in macerates. The antimicrobial activity of both extracts was examined and B. cereus was found to be the most sensitive bacterial strain, whereas in the case of yeast S. cerevisiae was particularly sensitive to both extracts. In addition to this activity, the in vitro antihyperglycaemic activities of both extracts against α-amylase and α-glucosidase were investigated, with ultrasound extract showing higher antihyperglycemic activity (50.63% inhibited α-amylase and 48.67% inhibited α-glucosidase) which could potentially be explained by the presence of chlorogenic acid (33.11 μg/mL) and quercetin (34.88 μg/mL). In the subcritical extract, obtained under optimal conditions, only the presence of hydroxy methylfurfural was detected, and this extract was not subjected to antimicrobial and antihyperglycemic activity.For the extraction of lipophilic components of M. vulgare, distillation of essential oil (0.05%), Soxhlet extraction (3.23%) and extraction with supercritical carbon dioxide at pressures of 100, 200 and 300 bar and at temperatures of 40, 50 and 60 ° C were applied. The most dominant component in all the supercritical extracts obtained is the chemotaxonomic marker marubiin, which was not identified in the Soxhlet extract.The liquid extracts obtained by the ultrasound and microwave extraction under optimized conditions and the macerate were spray dried (with the addition of 10 and 50% maltodextrin) to obtain a more stable form of the dry extract. Dry extracts underwent determination of the most important physical properties and chemical composition as well as antimicrobial and antihyperglycemic activities to evaluate their incorporation into functional foods, dietary supplements or in the formulation of various finished dosage forms that are administered preventively or to improve human health.

U ovom radu istraživan je utjecaj konvencionalne ekstrakcije (CE) te ekstrakcije potpomognute mikrovalovima (MAE) na sastav i udio fenolnih spojeva (ukupni fenoli, flavonoidi, flavonoli i hidorksicimetne kiseline) lista tršlje sa lokacija Barbariga, Lun, Hvar i Vela Luka ubranog tijekom tri fenološke faze (cvatnja; rani plod i zreli plod) u ovisnosti o vrsti i polarnosti otapala (voda, 100% i 80% metanol i etanol) i vremenu ekstrakcije (30 - 210 minuta) kod CE, te temperature (50-70 °C), snage mikrovalova (200-500 W) i vremena (4-12 min) kod MAE. Optimalni uvjeti ekstrakcije definirani su na temelju masenih udjela fenolnih spojeva. Najbolji ekstrakcijski kapacitet kod CE i MAE postignut je upotrebom 80 %-tne vodene otopine metanola kao otapala i to kod CE tijekom 90 min, a kod MAE u vremenu od 12 min, temperaturi od 69 °C i snazi mikrovalova od 500 W. U ekstraktima lista tršlje dobivenim pri optimalnim uvjetima pomoću HPLC-DAD i LC-MS/MS provedena je kvalitativna i kvantitativna analiza pojedinčanih fenolnih spojeva te se pokazalo da je najzastupljenija fenolna kiselina je 5-O-galoilkina kiselina, dok je miricetin ramnozid određen kao dominantni flavonol glikozid. Istraživan je i utjecaj tlaka na prinos eteričnih ulja dobivenih iz uzoraka lista tršlje, te njihov antimikrobni učinak prema gram-negativnim bakterijama Escherichia coli soj AB1157 i Erwinia amylovora soj EaED pomoću disk difuzijske metode. GC-MS analizom identificirano i kvantificirano 56 sastavnica od kojih su α-pinen, β-pinen i limonen određene kao dominantne. Sva eterična ulja su pokazala umjereni antimikrobni učinak prema navedenim gram-negativnim bakterijama u usporedbi sa antimikrobnim učinkom antibiotika kloramfenikol. Antimikrobno djelovanje eteričnih ulja tršlje pripisuje se sinergističkom djelovanju svih sastavnica. This study researched the influence of conventional (CE) and microwave assisted extraction (MAE) on the composition and mass fractions of phenolic compounds (total phenols, flavonoids, flavonols and hydroxycinnamic acids) in mastic tree leaves harvested at locations Barbariga, Lun, Hvar and Vela Luka during three phenological stages (flowering, early and late fruiting) depending on the solvent type and polarity (100% water, 100% and 80% methanol or ethanol), extraction time (30-210 minutes) concerning CE as well as temperature (50-70°C), microwave power (200-500W) and time (4-12 min) regarding MAE. Optimal extraction conditions for CE and MAE were obtained by using 80% methanol as a solvent during 90 minutes regarding CE and 12 minutes concerning MAE at temperature of 69 °C and microwave power of 500 W. In mastic tree leaves extracts obtained by optimal extraction conditions, phenolic profile was determined using HPLC-DAD and UPLC-MS/MS methods by which the dominant fenolic acid determined was 5-O-galloylquinic acid, while myricetin rhamnoside was deterimined as a dominant flavonol gylcoside. Furthermore, the influence of pressure on the mastic leaf essential oil yield was researched as well as their antimicrobial activity against gram-negative bacteria Escherichia coli strain AB1157 and Erwinia amylovora strain EaED by disc-diffusion method. Using GC-MS analysis, 56 components of the obtained essential oil were identified and quanitified among which α-pinene, β-pinene and limonene were determined as dominant. All essential oil samples exhibited moderate antimicrobial activity against mentioned gram-negative bacteria, in comparison to antibiotic chloramphenicol, due to the synergictic activity of all essential oil compounds.

Proizvodnju maslinovog ulja iz plodova masline karakterizira nastanak velikih količina ekotoksičnog otpada - komine masline i otpadnih voda, čije odlaganje predstavlja izazov u ekološkom i ekonomskom smislu. S druge strane, ekstrakt komine masline sadrži značajne količine bioaktivnih antioksidansa te se u tom smislu može smatrati vrijednom sekundarnom sirovinom. Ovim radom istražena je učinkovitost mikrovalne ekstrakcije spregnute inkapsulacijom ciklodekstrinima u dobivanju ekstrakata komine masline. Primjenom postupka optimirane mikrovalne ekstrakcije dobiveni su značajno kvalitetniji ekstrakti u kraćem vremenu i uz manji utrošak otapala, u usporedbi s klasičnom ekstrakcijom otapalom. Ispitan je utjecaj različitih ciklodekstrina na mjereni antioksidacijski potencijal. Rezultati provedenih istraživanja pokazuju da inkapsulacija ciklodestrinima rezultira dodatnim porastom prinosa antioksidansa, ovisno o vrsti primijenjenog ciklodekstrina , pri čemu se β- ciklodekstrin pokazao kao najbolji ekscipijens. Olive oil production is characterized by the production of a large amount of ecotoxic waste - olive pomace and wastewater, the disposal of which is a challenge in ecological and economic terms. On the other hand, olive pomace extract contains significant amounts of bioactive antioxidants and in this sense can be considered a valuable secondary raw material. This paper investigates the efficiency of microwave extraction coupled by encapsulation with cyclodextrins in obtaining olive pomace extracts. Using the optimized microwave extraction process, significantly better quality extracts were obtained in a shorter time and with lower solvent consumption, compared to conventional solvent extraction. The influence of different cyclodextrins on the measured antioxidant potential was investigated. The results of the conducted research show that encapsulation with cyclodextrins results in an additional increase in antioxidant yield, depending on the type of cyclodextrin used, with β-cyclodextrin proving to be the best excipient.

S porastom problema zbrinjavanja otpada i razgradnje plastične ambalaže raste i interes današnjih istraživanja k upotrebi biorazgradivih materijala. Među njima jestivi biofilmovi s visokovrijednim funkcionalnim sastojcima izoliranim iz različitih nusproizvoda prehrambene industrije svakako zauzimaju značajno mjesto. Sukladno današnjim trendovima u razvoju biorazdradivih materijala, i ovo istraživanje je pokazalo razvoj novih funkcionalnih pektinskih biofilmova s dodatkom ekstrakata kore mandarine. Njihova ugradnja u pektinske biofilmove praćena je promjenama u kemijskim i fizikalnim svojstvima. Rezultati su pokazali da biofilmovi s fenolnim ekstraktima kore mandarine pokazuju porast intenziteta boje, vlačne čvrstoće, te smanjenja modula elastičnosti u odnosu na biofilmove bez ekstrakata. Time je pokazano da se ekstrakti kore mandarine mogu uspješno primijeniti za izradu ekoloških prihvatljivih funkcionalnih pektinskih biofilmova. With the increases of waste disposal problems and decomposition of plastic packaging, the interest of nowadays investigations for the use of biodegradable materials is growing. Among them, edible biofilms with high-value functional ingredients isolated from various by-products of the food industry certainly occupy a significant place. In line with today’s trends in the development of biodegradable materials, this research has also shown the development of new functional pectin biofilms with the addition of tangerine peel extracts. Their incorporation into pectin biofilms is accompanied by changes in chemical and physical properties. The results showed that pectin biofilms with added phenolic extracts of tangerine peel have increased color intensity, tensile strength, but decreased the moduls of elasticity in comparison with biofilms without extracts. In this regard is showed that tangerine peel extracts could be successfully implemented for production of environment friendly functional pectin biofilms.

Background Gloriosa superba L. (Colchicaceae) is a high-value medicinal plant indigenous to Africa and Southeast Asia. Its therapeutic benefits are well-established in traditional medicines including Ayurveda. It is well known for its natural bioactive compound colchicine which exhibits a wide range of pharmacological activities i.e. rheumatism, gout and was also introduced into clinical practices. The increasing demand as well as its illegal harvesting has brought this valuable plant under threatened category. Methods The present investigation describes a microwave assisted extraction (MAE) strategy coupled with a densitometric-high performance thin layer chromatographic (HPTLC) methodology for the analysis of colchicine from 32 different populations of G. superba. A Box-Behnken statistical design (3 level factor) has been employed to optimize MAE, in which power of microwave, time of irradiation, aqueous ethanol and pH were used as independent variables whereas colchicine was used as the dependent variables. Chromatography was carried out on Silica gel 60 F254 TLC plates with toluene: methanol, 85:15 (v/v) being used as solvent system. Densitometric measurement was performed at λ=254 nm following post-derivatization (10% methanolic sulphuric acid). Results Optimal conditions for extraction to obtain the maximum colchicine yield was found to be 7.51 mg g− 1 which was very close to be predicted response 7.48 mg g− 1 by maintaining microwave power (460 W), irradiation time (6.4 min), aqueous ethanol-30, pH -3. Colchicine content ranged between 2.12–7.58 mg g− 1 among 32 G. superba populations in which only three chemotypes viz. GS- 1, GS- 3, and GS- 2 collected from West Bengal and Sikkim, respectively exhibited maximum yield of colchicine. Conclusion Therefore, this newly developed optimized MAE coupled with HPTLC densitometry methodology not only quantifies colchicine in order to identify elite chemotypes of G. superba, but it also encourages in selecting high yielding populations of the plants for industrial use and economic boost for the farmers. This validated, simple and reproducible HPTLC protocol is being used for the first time to estimate colchicine from natural populations of G. superba obtained from 32 different geographical regions of India. Graphical abstract

Objectives The aim of this study was to develop artificial neural network (ANNs) models for prediction of physical (total dissolved solids, extraction yield) and chemical (total polyphenolic content, antioxidant activity) properties of industrial hemp extracts, prepared by two different extraction methods (solid-liquid extraction and microwave-assisted extraction) based on combined UV-VIS-NIR spectra. Spectral data were gathered for 46 samples per extraction method. Results The PCA analysis ensured efficient separation of the samples based on the amount of ethanol in extraction solvent using NIR spectra for both conventional and microwave-assisted extraction. Conclusions Results showed that reliable ANN models (R2 >0.7000) for describing physical, chemical, and simultaneously physical and chemical characteristics can be developed based on combined UV-VIS-NIR spectra of industrial hemp extracts without spectra pre-processing.

The author B.M.-G. is grateful to the National Youth Guarantee System for the grant for young research personnel. Also, the authors are grateful to the University of Granada for a “Contrato Puente” postdoctoral contract (S.P.-M.)., Olive leaves contain bioactive compounds that have been shown to activate AMP-activated protein kinase (AMPK), which decreases intracellular lipid accumulation. Microwave-assisted extraction (MAE) is a green extraction technique that is frequently used in the recovery of phenolic compounds from plants. Thus, in this study, a Box-Behnken design was used to optimize MAE conditions such as temperature, percentage of ethanol and extraction time to obtain the maximum content of total compounds and compounds that activate AMPK. To this end, all extracts were characterized by High-Performance Liquid Chromatography Coupled to Electrospray Ionization Time-of-Flight Mass Spectrometry (HPLC-ESI-TOF-MS). The optimum conditions to obtain the highest content of total compounds were 123 ◦C, 100% of ethanol/water (v/v) and 23 min, whereas the optimum conditions for the highest amount of compounds that activate AMPK were 111 ◦C, 42% of ethanol/water (v/v) and 23 min. Thus, a multi-analysis by desirability was carried out to establish MAE optimal conditions for both responses. The optimum conditions were 111 ◦C, 100% EtOH and 23 min with a desirability of 0.97, which means that the responses are close to their individual optimal values. As a result, the olive leaf extract obtained at these optimal MAE conditions has great potential to be effective in the treatment of obesity., Spanish Ministry of Economy and Competitiveness (MINECO) AGL2015-67995-C3-2, Ministry of Science, Innovation and Universities RTI2018-096724-B-C22, Ministry of Economy, Knowledge, Business and University of the Junta de Andalucia B-AGR-466-UGR18

In this new century, sustainable development challenges chemical sciences to develop new and clean technological processes. The agri-food industry produces significant quantities of waste, raising significant economic and environmental concerns. Food waste valorization using environmentally friendly procedures is of increasing importance. This study describes the use of several Natural Deep Eutectic Solvents (NADESs) for the microwave-assisted extraction (MAE) of valuable bioactive phenolic compounds from olive oil processing wastes. The extracted samples were characterized by liquid chromatography electrospray ionization quadrupole time-of-flight mass spectrometry (LC-ESI-QTOF/MS) analysis and the quantification of the phenolic compounds was performed by HPLC analysis. The obtained data were compared with those obtained using water as the solvent in the same extraction conditions. The extraction process is nontoxic, simple and selective and meets most of the criteria to be considered as a sustainable process, with the solvents arising directly from nature.

Phenolic compounds are broadly represented in plant kingdom, and their occurrence in easily accessible low-cost sources like wastes from agri-food processing have led in the last decade to an increase of interest in their recovery and further exploitation. Indeed, most of these compounds are endowed with beneficial properties to human health (e.g., in the prevention of cancer and cardiovascular diseases), that may be largely ascribed to their potent antioxidant and scavenging activity against reactive oxygen species generated in settings of oxidative stress and responsible for the onset of several inflammatory and degenerative diseases. Apart from their use as food supplements or as additives in functional foods, natural phenolic compounds have become increasingly attractive also from a technological point of view, due to their possible exploitation in materials science. Several extraction methodologies have been reported for the recovery of phenolic compounds from agri-food wastes mostly based on the use of organic solvents such as methanol, ethanol, or acetone. However, there is an increasing need for green and sustainable approaches leading to phenolic-rich extracts with low environmental impact. This review addresses the most promising and innovative methodologies for the recovery of functional phenolic compounds from waste materials that have appeared in the recent literature. In particular, extraction procedures based on the use of green technologies (supercritical fluid, microwaves, ultrasounds) as well as of green solvents such as deep eutectic solvents (DES) are surveyed.

International audience; A robust method is provided to analyze 18 hydrophilic and hydrophobic biocides in both dissolved and particulate fractions of five types of urban and surface waters using high-performance liquid chromatography coupled to tandem mass spectrometry. The linearity, accuracy, and intermediate precision were validated. The target biocides were enriched by solid-phase extraction using Chromabond HR-X 200-mg cartridges and eluted with methanol, ethyl acetate, and dichloro-methane. Suspended matter was extracted by microwave-assisted extraction in methanol and dichlo-romethane. Recoveries and variability (respectively > 75% and < 30% for most of the target biocides and matrices) made it possible to quantify biocides at a trace level in all matrices. Limits of quantification were in the range of nanograms per liter in the dissolved fraction and in the range of nanograms per gram of dry weight in the particulate fraction for most of the biocides and matrices, and were generally lower than those reported in previous studies. The method was successfully applied to surface waters, treated and untreated wastewa-ter, combined sewer overflows, and stormwater, providing unique data in these matrices for some substances , in particular with respect to particle contamination. In urban waters, concentrations of most of the biocides ranged from 10 to 200 ng/L. Diuron, isothiazolinone, and benzalkonium concentrations could reach 0.9, 0.9, and 20 μg/L respectively. In rivers, most of the biocides were measured at less than 10 ng/L, but higher concentrations were observed for benzalkoniums (up to 200 ng/L) or after rain events, which indicates biocide transfer from urban surfaces into the aquatic environment during wet weather.

Antibacterial tests were carried out using ethanol extract of kelubi meat (Eleidoxa conferta), extraction using the Microwave-Assisted Extraction method with a ratio of 2: 20 for 30 minutes at 60 °C. Antibacterial tests using diffusion methods with concentrations of 20%, 40%, 60%, 80%, and 100%; positive control of 0.005% amoxillin and DMSO negative control. Antibacterial test results showed that the inhibition zone of ethanol extract in E. coli bacteria with a concentration of 20% was in the moderate category, for a concentration of 40% including the strong category while the concentration of 60%, 80% and 100% was very strong. The inhibition zone of ethanol extract for the S. aureus bacterium with a concentration of 20% is included in the strong category while the concentration of 40%, 60%, 80%, and 100% is categorized as very strong. From these results it can be concluded that the inhibitory zone in Stapylococcus aureus bacteria is greater than that of E. coli bacteria.

Lippia citriodora has been demonstrated to have a wide variety of phytochemicals which provide benefits to human health acting as antioxidants or anti-obesogenics. In this study, these phytochemicals were recovered using a microwave-assisted technology and applying optimal conditions and microencapsulated using spray drying. In this study, two di erent carbohydrates, maltodextrin (MD) and inulin (IN), were compared as carriers in the encapsulation procedure. The spray drying process was optimized by using a response surface methodology (RSM) based on a central composite design 22, where air inlet temperature and the sample:encapsulating agent ratio (S:EA) were selected as independent variables. Both designs were analyzed equally to evaluate di erences between each carrying agent on polar compounds’ encapsulation (process yield (Y%), encapsulation e ciency (EE%) and recovery of compounds (R%)) during the spray drying. The EE% and R% of each polar compound was monitored by High Performance Liquid Chromatography coupled to Time-of-Flight mass spectrometer by electrospray interface (HPLC-ESI-TOF-MS). The results showed that the use of IN as a carrier increased the powder recovered and the recovery of polar compounds after the spray dry process, whereas MD achieved a higher encapsulation efficiency., Spanish Government RTI2018-096724-B-C22

Herbal industry of developing countries is facing several technical issues related to the extraction conditions in order to attain the maximum yield of a plant extract with maximum therapeutic attributes. Therefore the present study was aimed to investigate the best technique for respective herbal products. The effect of three different extraction techniques: ultrasonic assisted extraction, microwave assisted and orbital shaker assisted extraction, by using three solvents (80% methanol, ethanol, and ethyl acetate) on the antioxidant potential of Caralluma tuberculata stem (non-conventional vegetable) extracts were investigated. Folin-Ciocalteu method was applied on tested samples in order to find the concentration of total phenols. Therefore, the optimized extract of high yield and maximum total phenolic content was selected for further analysis like total flavonoid contents, FRAP, DPPH and ABTS scavenging potential. Quantification of phenolic acids in the extracts was also carried out by HPLC. Significant variation was observed in the yield of total phenols within the extracts, but better results were obtained in aqueous methanolic extract of ultrasonic assisted extraction, followed by microwave assisted and orbital shaker assisted extraction. Present findings supported the view that ultrasonic assisted extraction can be used for phytochemicals profiling, activity guided assays and the development of herbal products. Correlation coefficients of active principles indicated a significant relationship to antioxidant capacity P < 0.05.

Algae have been considered as a source of high value bioactive compounds including pigments, lipids, fatty acids, polysaccharides, antioxidants and minerals. These compounds serve as a source of nutrition for both humans and animals and as additives in food production. Conventional solvent and/or green extraction techniques are mostly applied to extract these compounds from algae biomass. In this review, paper the most frequently used green extraction techniques such as supercritical fluid extraction, microwave assisted extraction, ultrasound-assisted extraction, pressurized liquid extraction, subcritical water extraction and pulsed electric field extraction were investigated in terms of their process conditions, applications, advantages and disadvantages.

Microwave assisted extraction (MAE) tech-nique was employed for the extraction of pectin from black mulberry (Morus nigra L.) pomace in this research. The effects of process variables namely microwave power (300-900 watt), irradiation time (10-30 min) and liquid to solid ratio (15-30 mL/g) on the yield, degree of esterification (DE) and galacturonic acid content (GalA) of pectin were investigated and optimized by using response surface methodology (RSM) with a face canter central composite design. Depending on the extraction conditions, the yield, DE and GalA of pectins varied in the range of 8.87-14.47% (dry weight basis), 44.44-57.06%, and 29.17-43.13%, respectively. The results showed that both the microwave power and irradiation time had highly significant effects on the pectin yield, while the effect of liquid to solid ratio was found to be not significant, in this regard. The optimal extraction conditions for maximum yield, DE and GalA of pectin were power of 900 watt, irradiation time of 18.17 min and liquid to solid ratio of 15 mL/g. Under these conditions, 13.16% of pectin with DE of 55.07% and GalA of 36.94% was extracted. The intrinsic viscosity and viscosity average molecular weight of a representative pectin sample was also determined and it was found to be 1.22 dL/g and 32.78 kDa, respectively. The black mulberry pomace pectin showed a viscoelastic behavior in the frequency sweep test and the crossover between G' and G" occurred at low frequency region (~ 0.07 rad/s).

Kenikir (Cosmos caudatus) adalah tanaman yang sering dimanfaatkan daunnya untuk bahan pangan maupun juga sebagai obat-obatan karena memiliki kandungan senyawa fenolik yang cukup tinggi. Ekstraksi senyawa fenol menggunakan metode konvensional masih memerlukan waktu yang cukup lama dan jumlah pelarut yang banyak. Sehingga perlu dicari alternatif metode ekstraksi yang memiliki waktu ekstraksi dan kebutuhan pelarut yang relatif rendah seperti menggunakan Microwave Assisted Extraction (MAE). Tujuan dari penelitian ini adalah melakukan ekstraksi senyawa fenolik dari daun kenikir dengan metode MAE terhadap total fenol dan aktivitas antioksidan. Penelitian ini menggunakan 2 faktor perlakuan yaitu rasio pelarut terhadap kenikir segar yaitu 1:4, 1:6, dan 1:8 (b/v) dan waktu ekstraksi 2, 3 dan 4 menit. Penelitian ini menjelaskan bahwa nilai total fenol tertinggi (17,162 ± 0,11 mg GAE/g berat segar) diperoleh pada perlakuan rasio pelarut 1:8 (b/v), sedangkan aktivitas antioksidan tertinggi (4,203 ± 0,26 mg/ml) pada perlakuan rasio pelarut 1:4 (b/v). Waktu perlakuan 3 menit menunjukkan hasil yang optimal untuk nilai total fenol dan aktivitas antioksidan. Hasil tersebut juga menunjukkan nilai yang lebih baik jika dibandingkan dengan metode konvensional baik dengan maserasi biasa dan maserasi dengan waterbath. Extraction of Phenolic Compounds from Cosmos caudatus using Microwave Assisted Extraction (MAE) Abstract. Cosmos caudatus, a plant commonly used its leaves for food and also as a medicine since it contains high phenolic compounds. The extraction of phenolic compounds using conventional methods still require more extraction time and need much more of solvent. Therefore, it was necessary to find an alternative extraction method that has a rapid extraction time and a few solvent need such as using Microwave Assisted Extraction (MAE). The aim of this study is to extract of phenolic compounds from Cosmos caudatus with MAE method of total phenol and antioxidant activity. This study using 2 treatment factors, the sampel-solvent ratio of 1:4, 1:6, and 1:8 (w/v) and the extraction time of 2, 3 and 4 minutes. This study explained that the highest total phenolic compounds (17.162 ± 0.11 mg GAE/g fw) and antioxidant activity (4.203 ± 0.26 mg/ml) were obtained at 1:8 and 1:4 (w/v) of sampel-solvent ratio, respectively. The extraction time of 3 minutes was the optimal condition for total phenolic compounds and antioxidant activity. These results also showed the highest parameter value when compared with both conventional methods: maceration and maceration with waterbath.

Ekstraksiyon,endüstriyel uygulamalar ve analitik amaçlar için oldukça önemlidir. Bu alandakiçalışmalar çoğunlukla gıdaların fonksiyonel özelliklerinin zenginleştirilmesindekullanılan antosiyanin, fenolik bileşikler gibi gıda bileşiklerinin eldesindeyoğunlaşmaktadır. Bu noktada, çalışılan ekstraksiyon tekniğinin çevre dostuolması yanında, ekstraksiyonu hedeflenen bileşik üzerinde meydana gelebilecekolumsuz etkilerin de azaltılması önem taşımaktadır. Bu amaçla birçok yeniteknik geliştirilmekte ve çeşitli gıdalarda çalışmalar yürütülmektedir. Sonyıllarda, geleneksel ekstraksiyon yöntemlerine alternatif olarak geliştirilenyeşil ekstraksiyon yöntemleri ile solvent kullanımının ve ekstraksiyonsüresinin azaltılması yanında verimin arttırılması da hedeflenmektedir. Buderleme, son yıllarda sıklıkla kullanılan yeşil ekstraksiyon tekniklerinin(mikrodalga, ultrases, yüksek basınç, vurgulu elektrik alan, ohmik ve süperkritikakışkan ekstraksiyon) prensiplerine, avantajlarına ve kullanım alanlarınaodaklanmaktadır., Extraction is animportant method for analytical and industrial applications. The studiesrelated to this subject mostly focus on the extraction of compounds such asanthocyanins, phenolic compounds which can be used for the production offunctional foods. It is important to protect not only the extracted compoundsfrom the adverse effects of extraction but also the environment by employinggreen extraction techniques. Hence, new technologies are being developed andstudies are being conducted with different foods. Recently, it is aimed toreduce the solvent consumption and extraction time by employing new green extractionmethods which are developed as alternatives to conventional methods. Thisarticle reviews the most commonly employed green extraction methods (microwave,ultrasound, high pressure, pulsed electric field, ohmic and supercritical fluidextraction) by focusing on the principals, advantages and applications of thenew methods.

The synthesis and characterization of Ag nanoparticles from Citrus limonum (lemon leaves) collected the Eastern Black Sea region was investigated in this study. A household microwave system device was used for microwave extraction of lemon leaves samples. The extract was prepared by taking 10g of dried lemon leaves. 10 g of sample was shaken in 100 mL of water for 90 min and extracted in a household microwave device at 4 minutes, 600 W. Ag nanoparticles were synthesized that the obtained aqueous solution was taken in different volumes by mixing 1 mM and 5mM AgNO3 solution. The colloid solution was subjected to microwave in an oven 1, 3, 5, 10, 15, 20 and 30 minutes at 90, 180, 360 W. Then production of AgNPs, the mixture was watched by UV-Vis spectroscopy (Shimadzu UVP-1240 spectrophotometer) measurements at different wavelengths (300 – 800 nm) for SPR of silver nanoparticles. The transition from yellow to a dark brown, shows the synthesis of silver nanoparticles.

Pertimbangan dalam pemilihan metode ekstraksi untuk mendapatkan senyawa bioaktif dari bahan tanaman diantaranya adalah efisiensi waktu dan jumlah pelarut yang digunakan. Studi terdahulu menunjukan ekstraksi bahan aktif dengan gelombang mikro mempercepat waktu ekstraksindan menghemat penggunaan pelarut dibandingkan metode konvensional, tetapi waktu ekstraksibyang terlalu singkat dan penggunaan pelarut yang terlalu minim membuat hasil ekstraksi tidaknoptimal. Penelitian ini untuk mengetahui pengaruh rasio bahan:pelarut dan lama ekstraksi dengan gelombang mikro terhadap kandungan fitokimia dan aktivitas antioksidan dari ekstrak cabai rawit. Penelitian dilakukan menggunakan Rancangan Acak Kelompok 2 faktor yaitu rasio bahan:pelarut dengan variasi 1:5; 1:10; dan 1:15, serta lama ekstraksi (5, 10, dan 15 menit). Berdasarkan hasil pengujian, rasio bahan:pelarut 1:10 memberikan hasil terbaik untuk kadar total capsaicinoid, total fenol, total flavonoid, dan aktivitas antioksidan dengan nilai rata-rata sebesar 138.06 ± 6.35 mg CE/g BK ekstrak, 33.75 ± 1.75 mg GAE/g BK ekstrak, 205.41 ± 26.13 mg QE/g BK ekstrak, dan 447.96 ±25.63 μg/ml. Lama ekstraksi untuk menghasilkan nilai total capsaicinoid dan total fenol paling tinggi adalah 5 menit, sedangkan untuk total flavonoid pada waktu 10 dan 15 menit. Nilai IC50 memiliki korelasi yang linear dengan total capsaicinoid, total fenol, dan total flavonoid. Pemilihan perlakuan terbaik dengan metode multiple atribut menunjukan rasio bahan:pelarut 1:10 dan lama ekstraksi 10 menit merupakan kombinasi perlakuan paling optimal untuk ekstraksi senyawa fenol menggunakan Microwave Assisted Extraction ABSTRACT The consideration of extraction methods to obtain bioactive compounds of plant origin were the time efficiency and the amount of extraction solvent. Previous studies showed that microwave assisted extraction of active ingredients decrease the extraction time and minimize the solvent compared to conventional methods, but short extraction time and less solvents make extraction less optimal. The aim of this study to determine the effect of materials:solvent and extraction time of microwave assisted extraction to phytochemical content and antioxidant activity of the cayenne pepper extract. The study was conducted using a Randomized Block Design 2 factors of the ratio of material:solvent (1:5; 1:10; and 1:15) and extraction time (5, 10, and 15 min). The results showed that material:solvent ratio of 1:10 gave the best value for total capsaicinoid content, total phenol, total flavonoid and IC50 with average value of 138.06 ± 6.35 mg CE/g DW, 33.75 ± 1.75 mg GAE/g DW extract, 205.41 ± 26.13 mg QE/g DW extract, and 447.96 ± 25.63 μg/ml respectively. The optimal extraction time to generate total capsaicinoid and total phenol content was 5 minutes, while the optimal extraction time for total flavonoid was 10 and 15 minutes. IC50 in this study had a linear correlation with total capsaicinoid, total phenol, and total flavonoid. The best treatment with multiple attribute method showed the materials:solvent ratio of 1:10 and extraction time of 10 minutes was the most optimal treatment combination for extraction of phenol compound by microwave assisted extraction

🏆 Highly Cited Paper Natural deep eutectic solvents (NADES) have recently come to the fore as new green solvents for foods, cosmetics and pharmaceuticals due to their unique solvation power and low toxicity. Turmeric extracts were prepared using the microwave assisted extraction method (MAE) using five NADES containing binary combinations of choline chloride, lactic acid, fructose, and sucrose. The MAE method was optimized and modeled by using response surface methodology to obtain maximum total antioxidant capacity (TAC) and curcumin contents (CC) in extracts for each NADES. All NADES extracts, except NADES-1 containing fructose and cholin chloride, exhibited higher TAC and CC than those in 80% methanol:water which was the preferred solvent in literature. NADES solvents did not interfere with subsequent antioxidant capacity measurements using the CUPRAC method. The proposed MAE is a potentially efficient and sustainable procedure in pharmaceutical and food industries for the extraction of antioxidants and curcumin from turmeric. Turkiye Bilimsel ve Teknolojik Arastirma Kurumu (TUBITAK)

Sulfated polysaccharide fucoidan isolated from brown algae shows a wide range of biological activities that are significantly dependent on its chemical composition, which is closely related to the applied technique and extraction parameters. Therefore, the objective of this study was to evaluate the influence of microwave assisted extraction (MAE) and pressurized liquid extraction (PLE) parameters (solvent, temperature, time, and number of cycles) on the Fucus virsoides and Cystoseira barbata polysaccharide yield (%PS) and chemical composition (total sugar, fucose, and sulfate group). The optimal MAE parameters that resulted in the highest polysaccharide extraction from F. virsoides and C. barbata were 0.1 M H2SO4 for 10 min at 80 °C, while the optimal PLE parameters were 0.1 M H2SO4, for two cycles of 15 min at 140 °C. Furthermore, the %PS, chemical structure, molecular properties, and antioxidant activity of the F. virsoides and C. barbata polysaccharide extracts obtained with MAE, PLE, and conventional extraction (CE) performed under previously determinate optimal conditions were compared. PLE resulted in a significantly higher %PS from F. virsoides, while for C. barbata, a similar yield was achieved with CE and PLE, as well as CE and MAE, for both algae. Furthermore, the polysaccharides obtained using PLE had the highest polydispersity index, fucose, and sulfate group content, and the lowest uronic acid content, however their antioxidant activity was lower.

From the recent market trend, there is a huge demand for the bioactive compounds from various food matrices that could be capable enough to combat the emerging health effects in day-to-day life. Fenugreek is a well-known spice from ancient times for its medicinal and health benefits. In the present study, two methods of green extraction microwave (MAE) and ultrasound (UAE) assisted were studied in regard of extraction of fenugreek diosgenin. In this study, solvent type (acetone, ethanol, hexane and petroleum ether), solvent concentration (40, 60, 80 and 100%) and treatment time (1.5, 3.0, 4.5 and 6.0 min and 30, 40, 50 and 60 min for MAE and UAE method respectively) was varied to observe the effect of these parameters over extract yield and diosgenin content. The results of this study revealed that treatment time, type of solvent and its concentration and method adopted for extraction of diosgenin has significant effect. In relation with better yield extract and diosgenin content, the yield of fenugreek seed extract was 7.83% with MAE and 21.48% with UAE of fenugreek seed powder at 80% ethanol concentration at 6 and 60 min respectively. The content of diosgenin was observed in fenugreek seed powder extract was 35.50 mg/100 g in MAE and 40.37 mg/100 g in UAE with 80% ethanol concentration at 6 and 60 min respectively. The overall range of yield of fenugreek extract was varied from 1.04% to 32.48% and diosgenin content was 15.82 mg/100 g to 40.37 mg/100 g of fenugreek seed powder including both extraction methods. This study revealed that UAE would impose better ways for preparing fenugreek extract and observing diosgenin content from fenugreek seeds.

This study was designedto develop a cost effective green extraction method to separate valuable chemicalsfrom black tea waste (BTW) and tea dust called “caffeine dust” (CD). These materialsare totally unwanted residue and treated as rubbish. Two extraction methods wereused for extraction of waste materials obtained in three collection periods. Inconventional extraction method, material was subjected to hot water extraction at 80 oCfor 40 minutes. In microwave assisted extraction (MAE) method, different eco-friendlyaqueous solvents (water, citric acid-water or ethanol-water) were used undera controlled 600 W microwave power at 80 oC for only 4 minutes treatmentin a close microwavesystem.MAE and conventional method gave similar extract yields for both waste materialsbut MAE was more successful and economical completing the extraction in shortertime. Using citric acid-water solvent in MAE significantly increased theextraction of individual catechins such as epicatechin (EC) andepigallocatechin gallate (EGCG). This study showed that tea waste could beutilized for production of valuable chemicals using nontoxic solvents atextremely short extraction periods., This study was designed to develop a cost effective green extraction method to separate valuable chemicals from black tea waste (BTW) and tea dust called “caffeine dust” (CD). These materials are totally unwanted residue and treated as rubbish. Two extraction methods were used for extraction of waste materials obtained in three collection periods. In conventional extraction method, material was subjected to hot water extraction at 80 oC for 40 minutes. In microwave assisted extraction (MAE) method, different eco-friendly aqueous solvents (water, citric acid-water or ethanol-water) were used under a controlled 600 W microwave power at 80 oC for only 4 minutes treatment in a close microwave system. MAE and conventional method gave similar extract yields for both waste materials but MAE was more successful and economical completing the extraction in shorter time. Using citric acid-water solvent in MAE significantly increased the extraction of individual catechins such as epicatechin (EC) and epigallocatechin gallate (EGCG). This study showed that tea waste could be utilized for production of valuable chemicals using nontoxic solvents at extremely short extraction periods.

The recovery of antioxidant polyphenols from light, dark and mix brewer&rsquo, s spent grain (BSG) using conventional maceration, microwave and ultrasound assisted extraction was investigated. Total polyphenols were measured in the crude (60% acetone), liquor extracts (saponified with 0.75% NaOH) and in their acidified ethyl acetate (EtOAc) partitioned fractions both by spectrophotometry involving Folin&ndash, Ciocalteu reagent and liquid-chromatography-tandem mass spectrometry (LC-MS/MS) methods. Irrespective of the extraction methods used, saponification of BSG yielded higher polyphenols than in the crude extracts. The EtOAc fractionations yielded the highest total phenolic content (TPC) ranging from 3.01 &plusmn, 0.19 to 4.71 &plusmn, 0.28 mg gallic acid equivalent per g of BSG dry weight. The corresponding total polyphenols quantified by LC-MS/MS ranged from 549.9 &plusmn, 41.5 to 2741.1 &plusmn, 5.2 &micro, g/g of BSG dry weight. Microwave and ultrasound with the parameters and equipment used did not improve the total polyphenol yield when compared to the conventional maceration method. Furthermore, the spectrophotometric quantification of the liquors overestimated the TPC, while the LC-MS/MS quantification gave a closer representation of the total polyphenols in all the extracts. The total polyphenols were in the following order in the EtOAc fractions: BSG light &gt, BSG Mix &gt, BSG dark, and thus suggested BSG light as a sustainable, low cost source of natural antioxidants that may be tapped for applications in food and phytopharmaceutical industries.

The present study aimed, on the one hand, to improve the yield of microwave assisted extraction (MAE) of polyphenols from beech bark by using a design of experiments (DoE) approach. On the other hand, beech bark extracts (BBE) were characterized in terms of their phytochemical profile and evaluated for biological potential (antioxidant, antibacterial, antifungal, antimutagen, anti-&alpha, glucosidase, and anti-tyrosinase). The extraction time varies with the amount of extracted total phenolic content (TPC). The microwave power favors TPC extraction but in different proportions. The optimum conditions which gave the highest TPC (76.57 mg GAE/g dry plant material) were reached when the microwave power was 300 W, extraction time was 4 min, and the solvent was an ethanol&ndash, water (50:50) mixture. The practical value of TPC after a controlled experiment was 76.49 mg GAE/g plant material. The identified compounds were vanillic acid, gallic acid, epicatechin, catechin, protocatechuic acid, chlorogenic acid, ferulic acid, and isoquercitrin. The antioxidant potential of BBEs was demonstrated by in vitro experiments. The BBEs were active against Staphylococcus aureus, Pseudomonas aeruginosa, Salmonella typhimurium, Escherichia coli, and Candida species. All extracts were antimutagenic and expressed an inhibition on &alpha, glucosidase and tyrosinase activity. Regarding antimutagen activity, the assayed extracts may be considered to have low or no antimutagen effects.

The data presented here are related to the research paper entitled “Structural features of spent coffee grounds water-soluble polysaccharides: towards tailor-made microwave assisted extractions” [1]. Microwave assisted extraction conditions were applied to spent coffee grounds for recovery of polysaccharides, namely arabinogalactans and galactomannans. Following an experimental design testing temperature, time, and alkali conditions as influence factors during microwave assisted extraction, this article reports the response data for the total extracted mass, sugars yield (including arabinogalactans and galactomannans total content, and mass ratio), and structural features (including degree of polymerization and degree of branching) for each set of operating conditions. In addition, it provides gas chromatography–mass spectrometry (GC–MS) chromatograms (and respective GC–MS spectra) of arabinogalactan and galactomannan mixtures with different structural features corresponding to representative microwave treatment conditions. Keywords: Coffee residue, Arabinogalactans, Galactomannans, Polysaccharides, Methylation analysis, Microwave assisted extraction

Background: Punica granatum extracts have been prescribed in traditional medicine for management of a variety of disease conditions including microbial infections. Generation of scientific evidence for validation of P. granatum peel extract’s anti-pathogenic efficacy is required. Methods: Hydroalcoholic extract of P. granatum peel (PGPE), prepared by microwave assisted extraction method was evaluated for its quorum-modulatory potential against two different human-pathogenic bacteria viz. Chromobacterium violaceum and Pseudomonas aeruginosa. Results: This extract was able to modulate in vitro production of quorum sensing-regulated pigments in both these test bacteria at ≥5 μg/ml. Virulence traits of P. aeruginosa like haemolytic activity, and biofilm formation were negatively affected by the test extract, and it also made P. aeruginosa more susceptible to lysis by human serum. Antibiotic susceptibility of both test bacteria was modulated owing to pre-treatment with PGPE. Exposure of these test pathogens to PGPE (≥0.5 μg/ml) effectively reduced their virulence towards the nematode Caenorhabditis elegans. Repeated subculturing of P. aeruginosa on PGPE-supplemented growth medium did not induce resistance to PGPE in this notorious pathogen, and this extract was also found to exert a post-extract effect on P. aeruginosa. Individual constituent phytocompounds of PGPE were found to be less efficacious than the whole extract. PGPE seemed to interfere with the signal-response machinery of P. aeruginosa and C. violaceum. PGPE also exhibited notable prebiotic potential by promoting growth of probiotic strains- Bifidobacterium bifidum and Lactobacillus plantarum at ≤50 μg/ml. Conclusions: This study indicates PGPE to be an effective antipathogenic and prebiotic preparation, and validates its therapeutic use mentioned in traditional medicine. This study also emphasizes the need for testing any bioactive extract at broadest possible concentration range, particularly in vivo, so that an accurate picture of dose-response relationship can emerge.

Conífera nativa da região sul e sudeste do Brasil a Arauraria angustifolia, sofreu através dos anos com a exploração indiscriminada de sua madeira, mas converteu-se numa espécie símbolo do sul do Brasil, devido ao consumo, pela população, das suas sementes comestíveis, os pinhões. Atualmente, as cascas dos pinhões e brácteas (sementes estéreis) da araucária são descartadas no ambiente sem reaproveitamento, porém estes subprodutos são fontes de compostos fenólicos, que podem ser usados para agregar valor. Para a extração de compostos bioativos tem sido empregado técnicas não convencionais que diminuem o uso de solventes orgânicos e o gasto energético. Por outro lado, o encapsulamento destes compostos busca garantir sua estabilidade e minimizar as limitações na aplicação industrial. À vista disso, o presente estudo objetivou avaliar a extração de compostos bioativos das brácteas da Araucaria angustifolia, através das extrações assistida de micro-ondas (EAM) e ultrassom (EAU) e o posterior encapsulamento do extrato através dos métodos de atomização e liofilização, utilizando pectina (PEC), colágeno hidrolisado (CH), polidextrose (PD) e goma guar parcialmente hidrolisada (GGPH) como materiais de parede. Para a EAU utilizou-se as potências de 250, 350 e 450 W, e tempos de 10, 15 e 20 min; e na EAM foram usadas potências de 700, 800 e 1000 W com tempos de 10, 15 e 20 min. A extração assistida por micro-ondas com o tempo de 20 min e potência de 1000 W resultou na melhor condição de extração, com teores de 47,61 mg g-1 (b.s) EAT, 27,09 mg g-1 (b.s) EAT, 779,95 mg g-1 (b.s) ECAT, 427,28 μmol g-1 (b.s) ET , 467,79 μmol g-1 (b.s) ET para compostos fenólicos totais, taninos totais, taninos condensados, e atividade antioxidante por ABTS e DPPH, respectivamente Essa condição quando comparada com a extração exaustiva realizada, não apresentou diferenças significativas quanto aos compostos fenólicos totais, taninos totais e taninos condensados, enquanto que a atividade antioxidante por DPPH apresentou valores maiores. Este mesmo extrato (1000 W; 20 min) foi encapsulado por atomização e liofilização, utilizando misturas de PEC-CH e PDGGPH, adicionadas ao extrato nas proporções de (0,25:0,75:9; m/m/m ) e (0,5:0,5:9; m/m/m), respectivamente. Os testes reológicos realizados nessas dispersões indicaram que ambas apresentaram comportamento de fluidos não-Newtonianos. Os pós obtidos com PD-GGPH resultaram nos maiores teores de compostos fenólicos totais (42,50 e 47,44 mg g-1 (b.s) EAT), taninos totais (36,88 e 40,91 mg g-1 (b.s) EAT), taninos condensados (498,46 e 669,58 mg g-1 (b.s) ECAT) e atividade antioxidante por ABTS (264,97 e 267,24 μmol g-1 (b.s) ET) e DPPH (139,78 e 157,83 μmol g-1 (b.s) ET) atomizados e liofilizados, respectivamente. Com relação às características físico-químicas, todos os pós apresentaram baixa atividade de água entre 0,19 e 0,35 e umidades de 1,52 a 3,48 %. A higroscopicidade foi elevada em todas as amostras com valores que variaram entre 30,68 a 45,27 %, enquanto que a solubilidade em água apresentou os melhores valores para os pós encapsulados com PD-GGPH, atomizado e liofilizado, com valores de 98,00 e 97,69 %, respectivamente. A microscopia eletrônica de varredura dos pós atomizados com PD-GGPH mostraram partículas com formato esférico regular, enquanto os pós de PEC-CH, exibiram formato irregular com a presença de rugosidade. Os pós liofilizados das duas dispersões apresentaram tamanhos e formas irregulares, devido principalmente a moagem realizada após liofilização. Os resultados do FTIR indicaram que o encapsulamento foi proporcionado por interações físicas entre os encapsulantes e os compostos fenólicos. A análise termogravimétrica indicou que a partir dos 220 °C iniciam-se as reações que desestruturam os materiais de parede, deixando os compostos encapsulados expostos, suscetíveis à degradação. A avaliação do armazenamento em condições aceleradas (temperaturas de 35 e 55 °C com 75 e 90 % de umidade relativa durante 35 dias) indicou que nos pós obtidos não ocorreram reduções significativas nos teores de compostos fenólicos e taninos totais durante o período de estocagem avaliado, havendo em algumas condições, o aumento destes teores no final da armazenagem, sendo que os pós resultantes da encapsulação com PEC-CH apresentaram os maiores aumentos com 70,7 e 101,9 % para compostos fenólicos totais e 81,0 e 116,0 % para taninos totais, atomizados e liofilizados, respectivamente. Estes aumentos se devem às reações de hidrólises e/ou reações de polimerizações que possam ter ocorrido durante a estocagem. Com os resultados obtidos tem-se que as brácteas de Araucaria angustifolia são fontes de compostos bioativos, sendo possível sua obtenção através da extração assistida por micro-ondas, e que seu encapsulamento permite a aplicação em formulações alimentícias Arauraria angustifolia, a native southern and southeastern Brazilian plant, has suffered through the years with the indiscriminate exploitation of its wood, but it has become a symbolic species in Brazil, due to the population's consumption of its edible seeds, named pinhão. At present, the bark of pine nuts and bracts (sterile seeds) of Araucaria are discarded in the environment without any reuse, but these by-products are considerable sources of phenolic compounds, which can be used to add value. For the extraction of the bioactive compounds, several unconventional techniques have been applied to minimize the use of organic solvents and energy expenditure. On the other hand, the encapsulation of these compounds seeks to guarantee the stability and to minimize the limitations in the industrial application. Therefore, the present study aimed to evaluate the extraction of bioactive compounds from Araucaria angustifolia bracts through assisted microwave extractions (MAE) and ultrasound (UAE) and subsequent encapsulation of the extract through spray drying and freeze drying methods, using pectin (PEC), hydrolyzed collagen (HC), polydextrose (PD) and partially hydrolyzed guar gum (PHGG) as wall materials. For UAE, potencies of 450, 350 and 250 W and times of 10, 15 and 20 min were used; for MAE it was used potencies of 1000, 800 and 700 W with times of 10, 15 and 20 min. The MAE with the time of 20 min and power of 1000 W resulted in the best extraction condition, with contents of 47.61 mg g-1 (d.b) EAT, 27.09 mg g-1 (d.b) EAT, 779.95 mg g-1 (d.b) ECAT, 427.28 μmol g-1 (d.b) ET, 467.79 μmol g-1 (d.b) ET for total phenolic compounds, total tannins, condensed tannins, and antioxidant activity by ABTS and DPPH assays, respectively This condition, when compared to the exhaustive extraction, did not show significant differences in total phenolic compounds, total tannins and condensed tannins, while the antioxidant activity by DPPH presented higher values. The same extract (1000 W, 20 min) was encapsulated by spray drying and freeze drying using mixtures of PEC-HC and PD-PHGG added to the extract in the proportions of (0.25:0.75:9) and (0.5:0.5:9) (w/w/w), respectively. The rheological tests performed on these dispersions indicated that both presented non- Newtonian fluid behavior. The PD-PHGG powders produced by spray drying and freeze drying, presented respectively: the highest total phenolic compounds (42.50 and 47.44 mg g-1 (d.b) EAT), total tannins (36.88 and 40.91 mg g-1 (d.b) EAT), condensed tannins (498.46 and 669.58 mg g-1 (d.b) ECAT) and antioxidant activity by ABTS (264.97 and 267.24 μmol g-1 (d.b) ET) and DPPH (139.78 and 157.83 μmol g-1 (d.b) ET). Regarding the physical-chemical characteristics, all the powders had low water activity between 0.19 and 0.35 and humidities of 1.52 to 3.48 %. The hygroscopicity was high in all samples with values ranging from 30.68 to 45.27 %, while the solubility presented the best values for the powders encapsulated with PD and PHGG, spray dried and freeze dried, with values of 98.00 and 97.69 %, respectively. Scanning electron microscopy of PD-PHGG spray dried powders showed regular spherical-shaped particles, whereas PEC-HC powders exhibited irregular shape with the presence of roughness. The freeze dried powders of the two dispersions presented irregular sizes and shapes, mainly due to the grinding performed after freeze drying. The FTIR results indicated that the encapsulation was provided by physical interactions between the encapsulants and phenolic compounds. The thermogravimetric analysis indicated that the reactions that destructure the wall materials begin at 220 °C, exposing the encapsulated compounds leading to susceptible degradation. The evaluation of the storage under accelerated conditions (temperatures of 35 and 55 °C with 75 and 90 % relative humidity for 35 days) indicated that there were no significant reductions in the contents of phenolic compounds and total tannins in the obtained powders during the evaluated storage period. However, in some conditions, there was an increase of these contents at the end of the storage, and the powders resulting from the encapsulation with PEC-HC showed the highest increases with 70.7 and 101.9 % for total phenolic compounds and 81.0 and 116.0 % for total, spray dried and freeze dried tannins, respectively. These increases might be due to hydrolysis reactions and / or polymerization reactions that may have occurred during storage.