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1.
Water Sci Technol ; 82(5): 799-828, 2020 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-33031062

RESUMO

Since it is difficult to analyze the components of organic matter in complex effluent matrices individually, the use of more collective, but at the same time, specific wastewater characterization methods would be more appropriate to evaluate changes in effluent characteristics during wastewater treatment. For this purpose, size distribution and structural (resin) fractionation tools have recently been proposed to categorize wastewater. There are several case studies available in the scientific literature being devoted to the application of these fractionation methods. This paper aimed to review the most relevant studies dealing with the evaluation of changes in wastewater characteristics using size distribution and structural (resin) fractionation tools. According to these studies, sequential filtration-ultrafiltration procedures, as well as XAD resins, are frequently employed for size and structural fractionations, respectively. This review focuses on the most relevant publications including biological treatment processes, as well as chemical treatment methods such as coagulation-flocculation, electrocoagulation, the Fenton's reagent and ozonation. This study aims at providing an insight into the possible treatment mechanisms and details the understanding what structural features of wastewater components enabled or prevented efficient treatment (removal) or targeted pollutants.


Assuntos
Eliminação de Resíduos Líquidos , Águas Residuárias , Fracionamento Químico , Floculação , Ultrafiltração
2.
J Environ Qual ; 49(1): 220-227, 2020 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-33016352

RESUMO

The economic viability of corn biorefineries depends heavily on the sale of coproducts as animal feeds, but elevated phosphorus (P) contents can exacerbate manure management issues. Phosphorus removal from light steep water and thin stillage, two concentrated in-process aqueous streams at wet milling and dry-grind corn biorefineries, could simultaneously generate concentrated fertilizer and low-P animal feeds, but little is known regarding how differences in stream composition affect removal. To address this data gap, we show that the solubility of P in light steep filtrate (LSF) and thin stillage filtrate (TSF) exhibits distinct sensitivity to calcium (Ca) and base addition due to differences in P fractionation and protein abundance. In LSF, P was primarily organic, and near-complete removal of P (96%) was observed at pH 8 and a Ca/total P (TP) ratio of 2. In TSF, TP removal was lower (81%), and there was more equal distribution of organic and orthophosphate, indicating that the Ca requirements of inorganic P precipitation were a limiting factor. The C/H/N ratio, elemental characterization, and crude protein analysis of the precipitated solids indicated that coprecipitation of amorphous solids containing Ca, Mg, and K with soluble proteins facilitated removal of P, particularly in LSF. Although the removal mechanisms and solubility limits differed, these results highlighted the magnitude (40-70 mM) and efficacy (80-96%) of P recovery from two biorefinery streams.


Assuntos
Fósforo , Zea mays , Ração Animal , Animais , Fracionamento Químico , Água
3.
Mar Pollut Bull ; 159: 111484, 2020 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-32892919

RESUMO

In this study a novel sustainable method based on supercritical fluid extraction (SFE) method was developed for simultaneous extraction and fractionation of petroleum biomarkers. We herein proposed a two-step supercritical fluid extraction method for crude oil and tar ball to separate the petroleum biomarkers into aliphatic and aromatic fractions. In the first step, pure scCO2 was used, while scCO2 modified was used as a solvent in the subsequent step. CO2 SFE can serve as an environmental-friendly alternative to common column chromatography method for petroleum biomarker or compositional analysis by GC-MS. The extraction process was shown to be selective, according to the polarity of the solvent, providing fractionation of aliphatic and aromatic hydrocarbons. Yet the total extraction procedure in SFE was significantly faster than column chromatography methods (~80 min vs. 8 h). We will discuss the implications of this SFE method as a novel sustainable alternative to the existing extraction techniques.


Assuntos
Cromatografia com Fluido Supercrítico , Petróleo/análise , Biomarcadores , Fracionamento Químico , Cromatografia Gasosa-Espectrometria de Massas
4.
Chemosphere ; 258: 127357, 2020 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-32947670

RESUMO

Diffusive isotope fractionation of non- and perdeuterated benzenes and toluenes in aqueous solution was investigated. The experimental method was based on a Stokes diaphragm cell. The isotope composition of diffusate and retentate was found to be identical within a range of uncertainty of ±5‰ for benzene and ±10‰ for toluene. These data are consistent with a previous fractionation study using phase-transition kinetics as the potentially fractionating step. The present study contributes to strengthening the data base for diffusive isotope fractionation of organic compounds in aqueous solution. According to the presented data, diffusion of naturally occurring, monodeuterated organic compounds does not significantly affect their hydrogen isotope pattern.


Assuntos
Hidrocarbonetos/química , Poluentes Químicos da Água/química , Benzeno , Isótopos de Carbono , Fracionamento Químico/métodos , Difusão , Hidrogênio , Isótopos , Cinética , Tolueno , Água
5.
Biosens Bioelectron ; 169: 112592, 2020 Dec 01.
Artigo em Inglês | MEDLINE | ID: mdl-32942143

RESUMO

Global health and food security constantly face the challenge of emerging human and plant diseases caused by bacteria, viruses, fungi, and other pathogens. Disease outbreaks such as SARS, MERS, Swine Flu, Ebola, and COVID-19 (on-going) have caused suffering, death, and economic losses worldwide. To prevent the spread of disease and protect human populations, rapid point-of-care (POC) molecular diagnosis of human and plant diseases play an increasingly crucial role. Nucleic acid-based molecular diagnosis reveals valuable information at the genomic level about the identity of the disease-causing pathogens and their pathogenesis, which help researchers, healthcare professionals, and patients to detect the presence of pathogens, track the spread of disease, and guide treatment more efficiently. A typical nucleic acid-based diagnostic test consists of three major steps: nucleic acid extraction, amplification, and amplicon detection. Among these steps, nucleic acid extraction is the first step of sample preparation, which remains one of the main challenges when converting laboratory molecular assays into POC tests. Sample preparation from human and plant specimens is a time-consuming and multi-step process, which requires well-equipped laboratories and skilled lab personnel. To perform rapid molecular diagnosis in resource-limited settings, simpler and instrument-free nucleic acid extraction techniques are required to improve the speed of field detection with minimal human intervention. This review summarizes the recent advances in POC nucleic acid extraction technologies. In particular, this review focuses on novel devices or methods that have demonstrated applicability and robustness for the isolation of high-quality nucleic acid from complex raw samples, such as human blood, saliva, sputum, nasal swabs, urine, and plant tissues. The integration of these rapid nucleic acid preparation methods with miniaturized assay and sensor technologies would pave the road for the "sample-in-result-out" diagnosis of human and plant diseases, especially in remote or resource-limited settings.


Assuntos
Doenças Transmissíveis/diagnóstico , Dispositivos Lab-On-A-Chip , Ácidos Nucleicos/isolamento & purificação , Doenças das Plantas , Sistemas Automatizados de Assistência Junto ao Leito , Betacoronavirus/isolamento & purificação , Fracionamento Químico/instrumentação , Fracionamento Químico/métodos , Doenças Transmissíveis/microbiologia , Doenças Transmissíveis/parasitologia , Doenças Transmissíveis/virologia , Infecções por Coronavirus/diagnóstico , Infecções por Coronavirus/virologia , Desenho de Equipamento , Humanos , Técnicas de Amplificação de Ácido Nucleico/instrumentação , Técnicas de Amplificação de Ácido Nucleico/métodos , Ácidos Nucleicos/sangue , Ácidos Nucleicos/urina , Pandemias , Doenças das Plantas/microbiologia , Doenças das Plantas/parasitologia , Doenças das Plantas/virologia , Pneumonia Viral/diagnóstico , Pneumonia Viral/virologia
6.
PLoS One ; 15(8): e0235723, 2020.
Artigo em Inglês | MEDLINE | ID: mdl-32797045

RESUMO

Mixtures of drugs often have greater therapeutic value than any of their constituent drugs alone, and such combination therapies are widely used to treat diseases such as cancer, malaria, and viral infections. However, developing useful drug mixtures is challenging due to complex interactions between drugs. Natural substances can be fruitful sources of useful drug mixtures because secondary metabolites produced by living organisms do not often act in isolation in vivo. In order to facilitate the study of interactions within natural substances, a new analytical method to quantify interactions using data generated in the process of bioassay-guided fractionation is presented here: the extract fractional inhibitory concentration index (EFICI). The EFICI method uses the framework of Loewe additivity to calculate fractional inhibitory concentration values by which interactions can be determined for any combination of fractions that make up a parent extract. The EFICI method was applied to data on the bioassay-guided fractionation of Lechea mucronata and Schinus terebinthifolia for growth inhibition of the pathogenic bacterium Acinetobacter baumannii. The L. mucronata extract contained synergistic interactions (EFICI = 0.4181) and the S. terebinthifolia extract was non-interactive overall (EFICI = 0.9129). Quantifying interactions in the bioassay-guided fractionation of natural substances does not require additional experiments and can be useful to guide the experimental process and to support the development of standardized extracts as botanical drugs.


Assuntos
Antibacterianos/farmacologia , Produtos Biológicos/farmacologia , Extratos Vegetais/farmacologia , Infecções por Acinetobacter/tratamento farmacológico , Acinetobacter baumannii/efeitos dos fármacos , Anacardiaceae/química , Antibacterianos/isolamento & purificação , Produtos Biológicos/isolamento & purificação , Fracionamento Químico , Descoberta de Drogas , Avaliação Pré-Clínica de Medicamentos/métodos , Sinergismo Farmacológico , Humanos , Extratos Vegetais/isolamento & purificação
7.
J Oleo Sci ; 69(9): 1087-1093, 2020 Sep 02.
Artigo em Inglês | MEDLINE | ID: mdl-32788522

RESUMO

Previously, we reported that the polar lipid fraction from the golden oyster mushroom, Pleurotus citrinopileatus, suppresses colon injuries which result from apoptosis induced by inflammatory stresses in vivo and in vitro (Yamashita et al., J. Oleo Sci., 69, 751-757 (2020)). Here, we investigated the use of lipid classes in mushroom polar lipid fraction in alleviating colon injury using differentiated Caco-2 cells as an intestinal tract model. The mushroom polar lipid fraction was separated into four fractions using silica thin layer chromatography. Each mushroom polar lipid fraction suppressed lipopolysaccharide (LPS)-induced decreases in the viability of intestinal cells, and the effects of sphingolipid fractions were significantly stronger than those of fraction that did not contain sphingolipids. Addition of sphingolipid fractions suppressed the expression of apoptosis-related proteins (e.g., death receptors and caspases) in the LPS-treated cells. Mushroom polar lipids, especially sphingolipids suppress intestinal apoptosis induced by inflammatory stress, and highly polar sphingolipids may exert stronger suppressive effects.


Assuntos
Apoptose/efeitos dos fármacos , Doenças do Colo/tratamento farmacológico , Doenças do Colo/patologia , Fitoterapia , Pleurotus/química , Esfingolipídeos/isolamento & purificação , Esfingolipídeos/farmacologia , Apoptose/genética , Células CACO-2 , Caspases/genética , Caspases/metabolismo , Fracionamento Químico , Doenças do Colo/induzido quimicamente , Expressão Gênica , Humanos , Técnicas In Vitro , Inflamação , Lipopolissacarídeos , Esfingolipídeos/uso terapêutico
8.
J Chromatogr A ; 1628: 461434, 2020 Sep 27.
Artigo em Inglês | MEDLINE | ID: mdl-32822974

RESUMO

Differing sensitivity is the main obstacle for a direct combination of HPTLC with NMR spectroscopy. A sufficient amount of the isolated compound zone must be provided by HPTLC for subsequent offline NMR detection (HPTLC//NMR). To fill the gap, a straightforward procedure was developed using the same analytical HPTLC system for both bioprofiling and isolation of bioactive zones from multicomponent mixtures. The HPTLC-effect-directed analysis (EDA) revealed several bioactive compounds in five botanical extracts, i.e. Salvia officinalis, Thymus vulgaris and Origanum vulgare, all Lamiaceae, and peels of red and green apples (Jonagored and Granny Smith, respectively), both Rosaceae. A tricky case study was designed to show how to deal with potentially coeluting bioactive structural isomers, e.g., ursolic (UA), oleanolic (OA) and betulinic acids (all C30H48O3), which are most difficult to identify and assign. A multipotent bioactive HPTLC zone showed the same hRF value and mass signal in HPTLCHRMS, though containing the coeluting structural isomers UA and OA. After zone isolation from the HPTLC plate, first the 1H NMR spectrum allowed to distinguish distinct allylic H-18 protons, i.e. 2.20 ppm for UA and 2.85 ppm for OA, and at the same time, to quantify the two isomers by using the PUlse Length-based CONcentration methodology (HPTLC//1H qNMR-PULCON). In case of a partial overlap of the diagnostic signal with that of the matrix, results were corroborated with those obtained by using the 1H deconvoluted or 2D 1H-13C Heteronuclear Single Quantum Coherence spectra. The comparison of the quantitative results showed a good correlation (R2 = 0.9718) between the two orthogonal methods HPTLC-Vis and HPTLC//1H qNMR-PULCON. A sufficient zone isolation from the HPTLC plate (mean isolation rate of 82%) for both UA and OA (0.27 - 4.67 mM) was achieved for HPTLC//qNMR, comparing the isolated bioactive compound zone with the respective zone in the botanical extract via HPTLC-Vis densitometry. The HPTLC-EDA-Vis//1H qNMR-PULCON procedure for bioprofiling and quantification/identification/confirmation of bioactive compounds in botanical extracts is considered as straightforward, eco-friendly (only 16 mL solvent required), simple (NMR calibration used over weeks) and reliable new alternative to the status quo of bioactivity-guided fractionation.


Assuntos
Bioensaio/métodos , Espectroscopia de Ressonância Magnética , Compostos Fitoquímicos/análise , Fracionamento Químico , Cromatografia em Camada Delgada , Lamiaceae/química , Ácido Oleanólico/análise , Ácido Oleanólico/química , Extratos Vegetais/química , Padrões de Referência , Triterpenos/análise , Triterpenos/química
9.
Bioresour Technol ; 314: 123757, 2020 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-32645572

RESUMO

The new concept of integrated biorefineries has significantly changed pulp and paper industries. Lignin, which until then was only burned to generate energy, is now an important raw material for new products production. Kraft lignin (KL) fractions obtained by sequential fractionation with five organic solvents. This sequence allows to extract fractions from lower molar mass to higher molar one, resulting in more homogeneous samples. Lignin's fractions were characterized by FTIR, GPC, TGA and Higher Heating Value (HHV). HHV for KL was 24966, the lowest being 17,891 (F5) and the highest being 27051 J/g (F1), inversely proportional to the molar masses of fractions. This is a very important result indicating that the lower HHV fractions can be used for certain applications, such as antioxidants, additives, polymers, among others, adding value to kraft lignin. Fractions with higher HHV could be used for energy generation in the cellulose paper industry.


Assuntos
Calefação , Lignina , Fracionamento Químico , Solventes
10.
Bioresour Technol ; 315: 123857, 2020 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-32707508

RESUMO

In the context of emerging biorefinery for microalgae, polyethyleneimine (PEI), has been tested in order to achieve separation of fat-soluble and water-soluble compounds from Haematococcus pluvialis. Several parameters were taken into account (ratio between sample and PEI, pH, and ionic strength) and 2 conditions (0.075% PEI pH 7.4, and 0.100% PEI pH8.5) were studied for up-scalability, with a recovery of flocculated compounds (lipids and pigments), and a complete characterization of both phases. Using 0.075% PEI, pH7.4, 100% sugars and 89.8% proteins were retained in the supernatant, but some trace of beta-carotene were also detected. For 0.100% PEI, pH 8.5, a loss in proteins content was highlighted (61.2% proteins retained), but no residual lipids or pigments were detected. PEI could therefore be considered as an efficient method to fractionate fat-soluble and water-soluble compounds from microalgae.


Assuntos
Microalgas , Fracionamento Químico , Clorofíceas , Floculação , Polietilenoimina
11.
Nat Protoc ; 15(8): 2568-2588, 2020 08.
Artigo em Inglês | MEDLINE | ID: mdl-32651564

RESUMO

RNA-protein interactions play a pivotal role in cell homeostasis and disease, but current approaches to study them require a considerable amount of starting material, favor the recovery of only a subset of RNA species or are complex and time-consuming. We recently developed orthogonal organic phase separation (OOPS): a quick, efficient and reproducible method to purify cross-linked RNA-protein adducts in an unbiased way. OOPS avoids molecular tagging or the capture of polyadenylated RNA. Instead, it is based on sampling the interface of a standard TRIzol extraction to enrich RNA-binding proteins (RBPs) and their cognate bound RNA. OOPS specificity is achieved by digesting the enriched interfaces with RNases or proteases to release the RBPs or protein-bound RNA, respectively. Here we present a step-by-step protocol to purify protein-RNA adducts, free protein and free RNA from the same sample. We further describe how OOPS can be applied in human cell lines, Arabidopsis thaliana, Schizosaccharomyces pombe and Escherichia coli and how it can be used to study RBP dynamics.


Assuntos
Fracionamento Químico/métodos , Proteoma/isolamento & purificação , Proteínas de Ligação a RNA/isolamento & purificação , RNA/isolamento & purificação , Transcriptoma , Linhagem Celular , Humanos , Proteoma/metabolismo , RNA/metabolismo , Proteínas de Ligação a RNA/metabolismo , Fluxo de Trabalho
12.
Nat Commun ; 11(1): 3389, 2020 07 07.
Artigo em Inglês | MEDLINE | ID: mdl-32636418

RESUMO

Monomethylmercury (MMHg) is a potent toxin that bioaccumulates and magnifies in marine food webs. Recent studies show abundant methylated Hg in deep oceans (>1000 m), yet its origin remains uncertain. Here we measured Hg isotope compositions in fauna and surface sediments from the Mariana Trench. The trench fauna at 7000-11000 m depth all have substantially positive mass-independent fractionation of odd Hg isotopes (odd-MIF), which can be generated only in the photic zone via MMHg photo-degradation. Given the identical odd-MIF in trench fauna and North Pacific upper ocean (<1000 m) biota MMHg, we suggest that the accumulated Hg in trench fauna originates exclusively from MMHg produced in upper oceans, which penetrates to depth by sorption to sinking particles. Our findings reveal little in-situ MMHg production in deep oceans and imply that anthropogenic Hg released at the Earth's surface is much more pervasive across deep oceans than was previously thought.


Assuntos
Cadeia Alimentar , Isótopos de Mercúrio/análise , Mercúrio/análise , Compostos de Metilmercúrio/análise , Biota , Fracionamento Químico , Monitoramento Ambiental , Sedimentos Geológicos , Oceano Pacífico , Poluentes Químicos da Água/análise
13.
Chemosphere ; 260: 127515, 2020 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-32682130

RESUMO

In this work we present an assessment of mercury (Hg) and methyl mercury (MeHg) bioaccumulation in different species of marine sponges collected off the Northwestern Mediterranean and Northeastern Atlantic coasts. Overall the results showed significant accumulation of Hg in sponges, with the Mediterranean sponge Chondrilla nucula exhibiting the highest total Hg content (up to 0.5 mg kg-1) and bio-concentration factor (BCF) up to 23. A significant inter-species variability of Hg bioaccumulation was observed among species collected at the same site. The sponges, collected in marine environment contaminated with Hg show consistently higher Hg accumulation, meaning that the bioaccumulation is proportional to the Hg availability in the surrounding environment. Different extraction protocols were tested for MeHg analysis and, generally, a low MeHg ratio in Hg species (4% and 17% average for Mediterranean and Irish sponges respectively) was detected suggesting a possible demethylation process and therefore a promising role of sponges for Hg bioremediation Additionally, the Hg isotopic composition in these organisms was determined and it showed that MDF (mass dependent fractionation) is the main process in sponges, with the absence of significant MIF. This result suggests a dominant role of associated microbial population in the methylation and/or demethylation processes.


Assuntos
Bioacumulação , Monitoramento Ambiental/métodos , Mercúrio/análise , Compostos de Metilmercúrio/análise , Poríferos/metabolismo , Poluentes Químicos da Água/análise , Animais , Oceano Atlântico , Biotransformação , Fracionamento Químico , Mar Mediterrâneo , Mercúrio/metabolismo , Compostos de Metilmercúrio/metabolismo , Especificidade da Espécie , Poluentes Químicos da Água/metabolismo
14.
Food Chem ; 333: 127491, 2020 Dec 15.
Artigo em Inglês | MEDLINE | ID: mdl-32659672

RESUMO

A cascade process for the sequential recovery of proteins and feruloylated arabinoxylan from wheat bran is proposed, involving a protein isolation step, enzymatic destarching and subcritical water extraction. The protein isolation step combining lactic acid fermentation and cold alkaline extraction reduced the recalcitrance of wheat bran, thus improving the total yields of the subsequent subcritical water extraction. The time evolution of subcritical water extraction of feruloylated arabinoxylan was compared at two temperatures (160 °C and 180 °C). Longer residence times enhanced the purity of target feruloylated arabinoxylans, whereas higher temperatures resulted in faster extraction at the expense of significant molar mass reduction. The radical scavenging activity of the extracted feruloylated arabinoxylans was preserved after the initial protein isolation step. This study opens new possibilities for the cascade valorization of wheat bran into enriched protein and non-starch polysaccharide fractions, which show potential to be used as functional food ingredients.


Assuntos
Fracionamento Químico/métodos , Ácidos Cumáricos/química , Fibras na Dieta/análise , Proteínas de Plantas/isolamento & purificação , Xilanos/química , Xilanos/isolamento & purificação , Temperatura Alta , Peso Molecular
15.
Food Chem ; 333: 127488, 2020 Dec 15.
Artigo em Inglês | MEDLINE | ID: mdl-32682229

RESUMO

A mild mixed-solvent of n-hexane/isopropanol is proposed for extracting total mineral oil hydrocarbons (MOH) from commercial milk powder products. Unlike acid-hydrolysis, the mixed-solvent extraction was performed at ambient temperature and the low-boiling-point hydrocarbons were retained to the greatest extent. After extraction, total MOH was determined by on-line liquid chromatography-gas chromatography with a flame ionization detector (LC-GC-FID). The validation of the proposed extraction method revealed a recovery efficacy of 83.0-107.5% and a limit of quantification of 0.5 mg/kg. Then, the total MOH in ten commercial milk powders was determined and mineral oil saturated hydrocarbons (MOSH)/polyolefin oligomeric saturated hydrocarbons (POSH) were found to be within the range of 0.61-5.46 mg/kg. The comparison of the total and surface MOSH/POSH indicated that a major part of the contamination was derived from sources before packaging. The present study provides a robust method for the extraction and determination of total MOH in milk powders.


Assuntos
Fracionamento Químico/métodos , Contaminação de Alimentos/análise , Hidrocarbonetos/análise , Hidrocarbonetos/isolamento & purificação , Leite/química , Óleo Mineral/química , Solventes/química , Animais , Hidrocarbonetos/química , Pós
16.
Food Chem ; 333: 127447, 2020 Dec 15.
Artigo em Inglês | MEDLINE | ID: mdl-32688304

RESUMO

Quantification of the specific folate vitamers to estimate total folate in foods is not standardized. A collaborative study, including eight European laboratories, was conducted in order to determine the repeatability and reproducibility of the method for folate quantification in foods using the plant-origin γ-glutamyl hydrolase as part of the extraction procedure. The seven food samples analyzed represent the food groups; fruits, vegetables, dairy products, legumes, offal, fish, and fortified infant formula. The homogenization step was included, and six folate vitamers were analyzed using LC-MS/MS. Total folate content, expressed as folic acid equivalent, was 17-490 µg/100 g in all samples. Horwitz ratio values were within the acceptable range (0.60-1.94), except for fish. The results for fortified infant formula, a certified reference material (NIST 1869), confirmed the trueness of the method. The collaborative study is part of a standardization project within the Nordic Committee on Food Analysis (NMKL).


Assuntos
Fracionamento Químico/métodos , Ácido Fólico/análise , Análise de Alimentos/métodos , Espectrometria de Massas em Tandem/métodos , Animais , Cromatografia Líquida/métodos , Cromatografia Líquida/normas , Laticínios/análise , Grão Comestível/química , Produtos Pesqueiros/análise , Análise de Alimentos/normas , Alimentos Fortificados/análise , Frutas/química , Humanos , Lactente , Fórmulas Infantis/análise , Reprodutibilidade dos Testes , Espectrometria de Massas em Tandem/normas , Verduras/química
17.
Food Chem ; 333: 127534, 2020 Dec 15.
Artigo em Inglês | MEDLINE | ID: mdl-32673948

RESUMO

A new kind of multi-component membrane was prepared by combining gelatin solution, porogen and an inclusion complex of ionic liquid (IL) and beta-cyclodextrin (ß-CD) in a simple physical manner for selective separation of tea polyphenols (TPs) from green tea crude extracts. After screening, it was found that the resulting membrane containing the IL of dicationic N-vinylimidazole proline salt ([VIm]2C3[l-pro]2) had the excellent performance for the enrichment of the target molecules. Then the newly-developed film was comprehensively characterized by scanning electron microscopy, conductivity, thermogravimetry and spectral analysis. Under pressure driving, the adsorption from an aqueous solution of a mixture of TPs and theophylline on IL@ß-CD-Gel membrane showed that the adsorption capacity for TPs was 303.45 mg/g with removal percentages of 94.38%. The experimental data fit well with pseudo-second-order model and Freundlich model. By using this composite material, a new technology of membrane separation for selective adsorption of TPs was finally established.


Assuntos
Fracionamento Químico/métodos , Gelatina/química , Líquidos Iônicos/química , Membranas Artificiais , Polifenóis/isolamento & purificação , Chá/química , beta-Ciclodextrinas/química , Polifenóis/análise
18.
J Chromatogr A ; 1623: 461175, 2020 Jul 19.
Artigo em Inglês | MEDLINE | ID: mdl-32505279

RESUMO

An ionic liquid hybrid zwitterionic polymer capillary microextraction (CME) column was prepared for the biomimetic enrichment of glycopeptides by one-step copolymerization of 2-methacryloyloxyethyl phosphorylcholine (MPC) and 1-butyl-3-vinylimidazolium bromide, in the presence of crosslinker trimethylolpropane trimethacrylate (TMA). The resultant monolith was characterized by scanning electron microscopy (SEM), fourier transform infrared (FT-IR) spectroscopy and pore size distribution measurement. Due to the incorporation of zwitterionic MPC owning a unique biomimic structure (i.e. hydrophilic cation/anion and hydrophobic long-alkyl chain), the monolithic column has large pore size and good biocompatibility, exhibiting high extraction efficiency, permeability and fast mass transfer to targets. Besides, the use of ionic liquids (ILs) as co-monomer in the polymerization endows the monolith with enhanced mechanical stability, uniformity and multiple interactions. The prepared column was successfully applied in CME coupled to capillary electrochromatography (CEC) for the efficient enrichment and separation of glycopeptide antibiotics in foodstuff. The method demonstrated a wide linear range (50.0-18000.0 µg L-1), low detection limits (5.0-10.0 µg L-1, S/N = 3) and satisfied recoveries (76.0-109.7%). This work shows the advantage of fine-tuning biomimetic monoliths in application-specific CME-CEC.


Assuntos
Antibacterianos/análise , Eletrocromatografia Capilar/métodos , Glicopeptídeos/análise , Líquidos Iônicos/química , Antibacterianos/isolamento & purificação , Materiais Biomiméticos , Fracionamento Químico , Análise de Alimentos/métodos , Glicopeptídeos/isolamento & purificação , Interações Hidrofóbicas e Hidrofílicas , Imidazóis/química , Metacrilatos/química , Microscopia Eletrônica de Varredura , Fosforilcolina/análogos & derivados , Fosforilcolina/química , Polimerização , Polímeros/química , Espectroscopia de Infravermelho com Transformada de Fourier , Compostos de Vinila/química
19.
Food Chem ; 330: 127266, 2020 Nov 15.
Artigo em Inglês | MEDLINE | ID: mdl-32540528

RESUMO

The present study aimed to characterize the nutritional value and potential use of elderberries as a source of antioxidant compounds. The chemical composition, fatty acids and phenolic compounds were determined for elderberries. The optimization of extraction parameters was designed with a Box-Behnken design coupled with response surface methodology (RSM) and desirability function analysis. The process parameters tested included extraction temperature, % of ethanol and pH, while response variables were global extraction yield, total phenolic and anthocyanins content (TAC), carotenoids and antioxidant activity. Analyses revealed that elderberry was a rich source of total soluble solids, proteins and polyunsaturated fatty acids (omega-3: 38.12 g/100 g and omega-6: 39.54 g/100 g fatty acids). Regarding phenolic compounds, elderberries were found abundant in flavonoids (rutin and quercetin), and phenolic acids (i.e. gallic acid and gentisic acid). Finally, numerical optimization indicated that the best extraction parameters were the following: temperature 60 °C, 50% of ethanol and pH 2.


Assuntos
Antioxidantes/análise , Antioxidantes/química , Sambucus nigra/química , Antocianinas/análise , Carotenoides/análise , Fracionamento Químico , Etanol/química , Flavonoides/análise , Análise de Alimentos/métodos , Ácido Gálico/análise , Concentração de Íons de Hidrogênio , Hidroxibenzoatos/análise , Valor Nutritivo , Fenóis/análise , Extratos Vegetais/química , Quercetina/análise , Solventes , Espectrometria de Massas em Tandem , Temperatura
20.
Food Chem ; 330: 127324, 2020 Nov 15.
Artigo em Inglês | MEDLINE | ID: mdl-32569938

RESUMO

Enzymes currently used in cheesemaking have various drawbacks, and there is a continual need to find new coagulants. This study describes the extraction and biochemical characterization of two proteases from the red alga Gracilaria edulis. The proteases were extracted with phosphate buffer and partially purified by ammonium sulphate precipitation and dialysis. The enzymes exhibited optimum caseinolytic activity at 60 °C and a pH range of 6-8. They showed a high ratio of milk-clotting over caseinolytic activity, indicating they had an excellent milk-clotting ability. The proteases were confirmed to be serine protease and metalloprotease with molecular weight (MW) of 44 and 108 kDa. They exhibited high hydrolytic activity on κ-caseins, cleaving κ-casein at four main sites, one of which being the same as that of calf rennet, which is the first reported for an algal protease. The findings demonstrated that the proteases could potentially be used as a milk coagulant in cheesemaking.


Assuntos
Caseínas/metabolismo , Gracilaria/enzimologia , Peptídeo Hidrolases/isolamento & purificação , Peptídeo Hidrolases/metabolismo , Alga Marinha/enzimologia , Sulfato de Amônio , Animais , Caseínas/química , Fracionamento Químico , Quimosina/metabolismo , Eletroforese em Gel de Poliacrilamida , Gracilaria/química , Concentração de Íons de Hidrogênio , Hidrólise , Leite/química , Leite/metabolismo , Peso Molecular , Peptídeo Hidrolases/química , Extratos Vegetais/química , Extratos Vegetais/isolamento & purificação , Extratos Vegetais/metabolismo , Alga Marinha/química , Serina Proteases/química , Serina Proteases/isolamento & purificação , Serina Proteases/metabolismo , Espectrometria de Massas em Tandem , Temperatura
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