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1.
ACS Appl Mater Interfaces ; 13(33): 39905-39914, 2021 Aug 25.
Artigo em Inglês | MEDLINE | ID: mdl-34374514

RESUMO

The lack of functional groups or binding sites largely hindered the broad application of microporous organic networks (MONs). Herein, we report the fabrication of the sulfonate group-enriched magnetic MON composite (MMON-SO3H@SO3Na) via the combination of the sulfonic acid group containing the monomer and thiol-yne click postmodification for efficient magnetic solid-phase extraction (MSPE) of benzimidazole fungicides (BZDs) from complex sample matrices. The well-defined core-shell-structured MMON-SO3H@SO3Na was obtained and served as an advanced adsorbent for MSPE for concentrating and monitoring trace BZDs. The MMON-SO3H@SO3Na with numerous sulfonate groups provides plenty of ion-exchange, hydrogen-bonding, and π-π sites, leading to the favorable affinity to BZDs via multiple interaction mechanisms. The MMON-SO3H@SO3Na-based MSPE-high-performance liquid chromatography method afforded a wide linear range, low limits of detection, large enrichment factors, good precisions, and reusability for BZDs. Trace BZDs in complex vegetables and fruit samples were successfully detected by the established method. The MMON-SO3H@SO3Na also exhibited good selectivity toward multiple types of polar contaminants containing hydrogen-bonding sites and aromatic structures. This work provided a new postsynthesis strategy for constructing novel and multifunctioned magnetic MONs for preconcentration of trace analytes in a complex matrix.


Assuntos
Alcanossulfonatos/síntese química , Alcinos/química , Benzimidazóis/isolamento & purificação , Análise de Alimentos/métodos , Fungicidas Industriais/isolamento & purificação , Compostos de Sulfidrila/química , Cromatografia Líquida de Alta Pressão/métodos , Química Click , Óxido Ferroso-Férrico/química , Frutas/química , Limite de Detecção , Magnetismo/métodos , Microesferas , Porosidade , Reprodutibilidade dos Testes , Extração em Fase Sólida/métodos , Verduras/química
2.
Nutrients ; 13(8)2021 Aug 13.
Artigo em Inglês | MEDLINE | ID: mdl-34444931

RESUMO

Over the centuries, humans have traditionally used garlic (Allium sativum L.) as a food ingredient (spice) and remedy for many diseases. To confirm this, many extensive studies recognized the therapeutic effects of garlic bulbs. More recently, black garlic (BG), made by heat-ageing white garlic bulbs, has increased its popularity in cuisine and traditional medicine around the world, but there is still limited information on its composition and potential beneficial effects. In this study, the metabolite profile of methanol extract of BG (BGE) was determined by high-performance liquid chromatography coupled to tandem mass spectrometry in high-resolution mode. Results allowed to establish that BGE major components were sulfur derivatives, saccharides, peptides, organic acids, a phenylpropanoid derivative, saponins, and compounds typical of glycerophospholipid metabolism. Characterization of the BGE action in cancer cells revealed that antioxidant, metabolic, and hepatoprotective effects occur upon treatment as well as induction of maturation of acute myeloid leukemia cells. These results are interesting from the impact point of view of BG consumption as a functional food for potential prevention of metabolic and tumor diseases.


Assuntos
Alho/química , Leucemia Mieloide Aguda/tratamento farmacológico , Extratos Vegetais/química , Extratos Vegetais/farmacologia , Antioxidantes/farmacologia , Cromatografia Líquida de Alta Pressão/métodos , Humanos , Leucemia Mieloide Aguda/patologia , Peptídeos/análise , Raízes de Plantas/química , Polissacarídeos/análise , Saponinas/análise , Especiarias/análise , Enxofre/análise , Espectrometria de Massas em Tandem/métodos , Células U937
3.
Nutrients ; 13(8)2021 Aug 13.
Artigo em Inglês | MEDLINE | ID: mdl-34444934

RESUMO

Vitamin D deficiency is a global problem with many health consequences, and it is currently recommended to supplement vitamin D. Change of diet should also be considered to ensure adequate vitamin D in the human body. The aim of this study was to assess the concentration of vitamin D metabolites in two different groups: one group on the low-carbohydrate-high-fat (LCHF) diet and the other group on the Eastern European (EE) diet. In the first stage, 817 participants declaring traditional EE diet or LCHF diet were investigated. Nutrition (self-reported 3-day estimated food record) and basic anthropometric parameters were assessed. After extra screening, 67 participants on the EE diet and 41 on the LCHF diet were qualified for the second stage. Plasma 25-hydroxycholecalciferol (25(OH)D3) and (25(OH)D2) concentration was measured by the validated HPLC-MS/MS method. Plasma 25(OH)D3 concentration was significantly higher in the group on the LCHF diet (34.9 ± 15.9 ng/mL) than in the group on the EE diet (22.6 ± 12.1 ng/mL). No statistical differences were observed in plasma 25(OH)D2 concentration between the study groups (p > 0.05). Women had a higher plasma 25(OH)D2 concentration than men regardless of diet type. The LCHF diet had a positive influence on plasma vitamin D concentration. However, long-term use of the LCHF diet remains contentious due to the high risk of cardiovascular disease. This study confirmed that the type of diet influences the concentration of vitamin D metabolites in the plasma.


Assuntos
Dieta com Restrição de Carboidratos/métodos , Dieta Hiperlipídica/métodos , Deficiência de Vitamina D/sangue , Vitamina D/sangue , Idoso , Calcifediol/sangue , Cromatografia Líquida de Alta Pressão/métodos , Dieta/métodos , Suplementos Nutricionais , Ergocalciferóis/sangue , Grupo com Ancestrais do Continente Europeu , Feminino , Humanos , Masculino , Pessoa de Meia-Idade , Estado Nutricional , Projetos Piloto , Polônia , Espectrometria de Massas em Tandem/métodos , Vitaminas/sangue
4.
Molecules ; 26(15)2021 Jul 30.
Artigo em Inglês | MEDLINE | ID: mdl-34361795

RESUMO

Although Australia is the largest exporter of faba bean globally, there is limited information available on the levels of bioactive compounds found in current commercial faba bean varieties grown in this country. This study profiled the phenolic acid and flavonoid composition of 10 Australian faba bean varieties, grown at two different locations. Phenolic profiling by HPLC-DAD revealed the most abundant flavonoid to be catechin, followed by rutin. For the phenolic acids, syringic acid was found in high concentrations (72.4-122.5 mg/kg), while protocatechuic, vanillic, p-hydroxybenzoic, chlorogenic, p-coumaric, and trans-ferulic acid were all found in low concentrations. The content of most individual phenolics varied significantly with the variety, while some effect of the growing location was also observed. This information could be used by food processors and plant breeders to maximise the potential health benefits of Australian-grown faba bean.


Assuntos
Antioxidantes/química , Produtos Agrícolas/química , Flavonoides/química , Vicia faba/química , Antioxidantes/classificação , Antioxidantes/isolamento & purificação , Austrália , Catequina/química , Catequina/isolamento & purificação , Ácido Clorogênico/química , Ácido Clorogênico/isolamento & purificação , Cromatografia Líquida de Alta Pressão/métodos , Ácidos Cumáricos/química , Ácidos Cumáricos/isolamento & purificação , Produtos Agrícolas/crescimento & desenvolvimento , Produtos Agrícolas/metabolismo , Flavonoides/classificação , Flavonoides/isolamento & purificação , Ácido Gálico/análogos & derivados , Ácido Gálico/química , Ácido Gálico/isolamento & purificação , Humanos , Hidroxibenzoatos/química , Hidroxibenzoatos/isolamento & purificação , Parabenos/química , Parabenos/isolamento & purificação , Rutina/química , Rutina/isolamento & purificação , Ácido Vanílico/química , Ácido Vanílico/isolamento & purificação , Vicia faba/crescimento & desenvolvimento , Vicia faba/metabolismo
5.
Molecules ; 26(16)2021 Aug 04.
Artigo em Inglês | MEDLINE | ID: mdl-34443310

RESUMO

There are a significant number of analytical methodologies employing different techniques to determine phenolic compounds in beverages. However, these methods employ long sample preparation processes and great time consumption. The aim of this paper was the development of a simple method for evaluating the phenolic compounds' presence in Brazilian craft beers without a previous extraction step. Catechin, caffeic acid, epicatechin, p-coumaric acid, hydrated rutin, trans-ferulic acid, quercetin, kaempferol, and formononetin were analyzed in fifteen different craft beers. The method showed good linearity (R2 ≥ 0.9966). The limit of detection ranged from 0.08 to 0.83 mg L-1, and limits of quantification were between 0.27 and 2.78 mg L-1. The method showed a satisfactory precision (RSD ≤ 16.2%). A good accuracy was obtained by the proposed method for all phenolic compounds in craft beer (68.6% ˂ accuracy ˂ 112%). Catechin showed higher concentrations (up to 124.8 mg L-1) in the samples, followed by epicatechin (up to 51.1 mg L-1) and caffeic acid (up to 8.13 mg L-1). Rutin and formononetin were observed in all analyzed samples (0.52 mg L-1 to 2.40 mg L-1), and kaempferol was less present in the samples. The presence of plant origin products was determinant for the occurrence of the highest concentrations of phenolic compounds in Brazilian craft beers.


Assuntos
Cerveja/análise , Cromatografia Líquida de Alta Pressão/métodos , Fenóis/análise , Brasil , Limite de Detecção , Fenóis/química , Reprodutibilidade dos Testes
6.
Int J Mol Sci ; 22(16)2021 Aug 23.
Artigo em Inglês | MEDLINE | ID: mdl-34445776

RESUMO

Different manufacturing processes and storage conditions of biotherapeutics can lead to a significant variability in drug products arising from chemical and enzymatic post-translational modifications (PTMs), resulting in the co-existence of a plethora of proteoforms with different physicochemical properties. To unravel the heterogeneity of these proteoforms, novel approaches employing strong cation-exchange (SCX) high-performance liquid chromatography (HPLC) hyphenated to mass spectrometry (MS) using a pH gradient of volatile salts have been developed in recent years. Here, we apply an established SCX-HPLC-MS method to characterize and compare two rituximab-based biotherapeutics, the originator MabThera® and its Indian copy product Reditux™. The study assessed molecular differences between the two drug products in terms of C-terminal lysine variants, glycosylation patterns, and other basic and acidic variants. Overall, MabThera® and Reditux™ displayed differences at the molecular level. MabThera® showed a higher degree of galactosylated and sialylated glycoforms, while Reditux™ showed increased levels of oligomannose and afucosylated glycoforms. Moreover, the two drug products showed differences in terms of basic variants such as C-terminal lysine and N-terminal truncation, present in Reditux™ but not in MabThera®. This study demonstrates the capability of this fast SCX-HPLC-MS approach to compare different drug products and simultaneously assess some of their quality attributes.


Assuntos
Anticorpos Monoclonais/química , Antineoplásicos Imunológicos/química , Cátions/química , Rituximab/química , Medicamentos Biossimilares/química , Cromatografia de Afinidade/métodos , Cromatografia Líquida de Alta Pressão/métodos , Glicosilação , Espectrometria de Massas/métodos
7.
Molecules ; 26(15)2021 Jul 29.
Artigo em Inglês | MEDLINE | ID: mdl-34361749

RESUMO

Cefquinome and ceftiofur are ß-lactam antibiotics used for the treatment of bacterial infections in swine. Although these antimicrobials are administered intramuscularly, the exposure of the gut microbiota to these cephalosporins is not well described. This exposure can contribute to the emergence and spread of antimicrobials in the environment and to the possible spread of antimicrobial resistance genes. To assess the impact of drug administration on the intestinal excretion of these antimicrobials it is essential to measure the amounts of native compound and metabolites in feces. Two (ultra)-high-performance liquid chromatography-tandem mass spectrometry ((U)HPLC-MS/MS) methods were developed and validated, one for the determination of cefquinome and ceftiofur and the other for the determination of ceftiofur residues, measured as desfuroylceftiofuracetamide, in porcine feces. The matrix-based calibration curve was linear from 5 ng g-1 to 1000 ng g-1 for cefquinome (correlation coefficient (r) = 0.9990 ± 0.0007; goodness of fit (gof) = 3.70 ± 1.43) and ceftiofur (r = 0.9979 ± 0.0009; gof = 5.51 ± 1.14) and quadratic from 30 ng g-1 to 2000 ng g-1 for desfuroylceftiofuracetamide (r = 0.9960 ± 0.0020; gof = 7.31 ± 1.76). The within-day and between-day precision and accuracy fell within the specified ranges. Since ß-lactam antibiotics are known to be unstable in feces, additional experiments were conducted to adjust the sampling protocol in order to minimize the impact of the matrix constituents on the stability of the analytes. Immediately after sampling, 500 µL of an 8 µg mL-1 tazobactam solution in water was added to 0.5 g feces, to reduce the degradation in matrix.


Assuntos
Acetamidas/isolamento & purificação , Antibacterianos/isolamento & purificação , Cefalosporinas/isolamento & purificação , Cromatografia Líquida de Alta Pressão/normas , Furanos/isolamento & purificação , Espectrometria de Massas em Tandem/normas , Acetamidas/administração & dosagem , Animais , Antibacterianos/administração & dosagem , Calibragem , Cefalosporinas/administração & dosagem , Cromatografia Líquida de Alta Pressão/métodos , Fezes/química , Feminino , Furanos/administração & dosagem , Injeções Intramusculares , Masculino , Variações Dependentes do Observador , Reprodutibilidade dos Testes , Suínos , Espectrometria de Massas em Tandem/métodos , Tazobactam/química
8.
Molecules ; 26(12)2021 Jun 09.
Artigo em Inglês | MEDLINE | ID: mdl-34207697

RESUMO

Apple Replant Disease (ARD) is a significant problem in apple orchards that causes root tissue damage, stunted plant growth, and decline in fruit quality, size, and overall yield. Dysbiosis of apple root-associated microbiome and selective richness of Streptomyces species in the rhizosphere typically concurs root impairment associated with ARD. However, possible roles of Streptomyces secondary metabolites within these observations remain unstudied. Therefore, we employed the One Strain Many Compounds (OSMAC) approach coupled to high-performance liquid chromatography-high-resolution tandem mass spectrometry (HPLC-HRMSn) to evaluate the chemical ecology of an apple root-associated Streptomycesciscaucasicus strain GS2, temporally over 14 days. The chemical OSMAC approach comprised cultivation media alterations using six different media compositions, which led to the biosynthesis of the iron-chelated siderophores, ferrioxamines. The biological OSMAC approach was concomitantly applied by dual-culture cultivation for microorganismal interactions with an endophytic Streptomyces pulveraceus strain ES16 and the pathogen Cylindrocarpon olidum. This led to the modulation of ferrioxamines produced and further triggered biosynthesis of the unchelated siderophores, desferrioxamines. The structures of the compounds were elucidated using HRMSn and by comparison with the literature. We evaluated the dynamics of siderophore production under the combined influence of chemical and biological OSMAC triggers, temporally over 3, 7, and 14 days, to discern the strain's siderophore-mediated chemical ecology. We discuss our results based on the plausible chemical implications of S. ciscaucasicus strain GS2 in the rhizosphere.


Assuntos
Malus/microbiologia , Raízes de Plantas/microbiologia , Sideróforos/metabolismo , Streptomyces/química , Cromatografia Líquida de Alta Pressão/métodos , Malus/metabolismo , Raízes de Plantas/metabolismo , Rizosfera , Espectrometria de Massas em Tandem/métodos
9.
Molecules ; 26(12)2021 Jun 09.
Artigo em Inglês | MEDLINE | ID: mdl-34207872

RESUMO

Five new compounds including three pairs of enantiomeric xanthine analogues, parvaxanthines D-F (1-3), two new guanosine derivatives, asponguanosines C and D (6 and 7), along with two known adenine derivatives were isolated from the insect Cyclopelta parva. Racemic 1-3 were further separated by chiral HPLC. Their absolute configurations were assigned by spectroscopic and computational methods. It is interesting that all of these isolates are natural product hybrids. Antiviral, immunosuppressive, antitumor and anti-inflammatory properties of all the isolates were evaluated.


Assuntos
Anti-Inflamatórios/farmacologia , Antineoplásicos/farmacologia , Antivirais/farmacologia , Produtos Biológicos/farmacologia , Guanosina/química , Insetos/química , Xantinas/química , Animais , Produtos Biológicos/química , Células Cultivadas , Chlorocebus aethiops , Cromatografia Líquida de Alta Pressão/métodos , Camundongos , Camundongos Endogâmicos C57BL , Estrutura Molecular , Estereoisomerismo
10.
Int J Mol Sci ; 22(14)2021 Jul 16.
Artigo em Inglês | MEDLINE | ID: mdl-34299238

RESUMO

This study focused on the biological evaluation and chemical characterization of Geranium pyrenaicum Burm. f. Different solvent extracts (hexane, ethyl acetate, methanol, and water extracts) were prepared. The phytochemical profile, antioxidant, and enzyme inhibitory activity were investigated. Cytotoxicity was assessed using VERO, FaDu, HeLa and RKO cells. The antiviral activity was carried out against HSV-1 (Herpes simplex virus 1) propagated in VERO cell line. The aqueous extract, possessing high phenolic content (170.50 mg gallic acid equivalent/g extract), showed the highest reducing capacity (613.27 and 364.10 mg Trolox equivalent/g extract, for cupric reducing antioxidant capacity and ferric reducing antioxidant power, respectively), radical scavenging potential (469.82 mg Trolox equivalent/g extract, against 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid)), metal chelating ability (52.39 mg ethylenediaminetetraacetic acid equivalent/g extract) and total antioxidant capacity (3.15 mmol Trolox equivalent/g extract). Liquid chromatography-electrospray ionization-quadrupole time-of-flight-mass spectrometry (LC-ESI-QTOF-MS/MS) alloved to tentatively identify a total of 56 compounds in the extracts, including ellagitannins, gallic acid and galloyl derivatives amongst others. The ethyl acetate extracts substantially depressed cholinesterase enzymes (4.49 and 12.26 mg galantamine equivalent/g extract against AChE and BChE, respectively) and α-amylase enzyme (1.04 mmol acarbose equivalent/g extract). On the other hand, the methanolic extract inhibited tyrosinase (121.42 mg kojic acid equivalent/g extract) and α-glucosidase (2.39 mmol acarbose equivalent/g extract) activities. The highest selectivity towards all cancer cell lines (SI 4.5-10.8) was observed with aqueous extract with the FaDu cells being the most sensitive (CC50 40.22 µg/mL). It can be concluded that the presence of certain bioactive antiviral molecules may be related to the high anti HSV-1 activity of the methanolic extract. This work has generated vital scientific data on this medicinal plant, which is a prospective candidate for the creation of innovative phyto-pharmaceuticals.


Assuntos
Geranium/metabolismo , Extratos Vegetais/química , Animais , Antioxidantes , Antivirais , Linhagem Celular , Cromatografia Líquida de Alta Pressão/métodos , Flavonoides/análise , Humanos , Fenóis/análise , Compostos Fitoquímicos/química , Extratos Vegetais/isolamento & purificação , Extratos Vegetais/farmacologia , Plantas Medicinais/química , Estudos Prospectivos , Espectrometria de Massas por Ionização por Electrospray/métodos , Espectrometria de Massas em Tandem/métodos
11.
Methods Mol Biol ; 2314: 549-577, 2021.
Artigo em Inglês | MEDLINE | ID: mdl-34235670

RESUMO

Decades of study have highlighted the richness and uniqueness of the repertoire of lipid and glycolipid families produced by mycobacteria. Many of these families potently regulate host immune responses, in stimulatory or suppressive ways. Thus, the global study of this repertoire in different genetic backgrounds or under model conditions of infection is gaining interest. Despite the difficulties associated with the specificities of this repertoire, the field of mass spectrometry-based lipidomics of mycobacteria has recently made considerable progress, particularly at the analytical level. There is still considerable scope for further progress, especially with regard to the development of an efficient bioinfomatics pipeline for the analysis of the large datasets generated. This chapter describes an HPLC-MS methodology allowing the simultaneous screening of more than 20 of the lipid families produced by mycobacteria and provides recommendations to analyze the generated data given the state-of-the-art.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Glicolipídeos/metabolismo , Lipidômica/métodos , Lipídeos/análise , Espectrometria de Massas/métodos , Mycobacterium/metabolismo , Glicolipídeos/análise , Humanos
12.
Molecules ; 26(12)2021 Jun 21.
Artigo em Inglês | MEDLINE | ID: mdl-34205529

RESUMO

Polyscias fruticosa (L.) leaves contain significant bioactive compounds with high antioxidant activity such as chlorophylls, total polyphenols, etc. but these have still been underutilized. In this study, the kinetics of chlorophyll and antioxidant activity extraction from P. fruticosa leaves by microwave-assisted extraction (MAE) were investigated. Microwave power was 300, 450, or 600 (W); the ratio of material/solvent varied from 1:40 to 1:80 (g/mL). In this study, the second-order kinetic model successfully predicted the change of chlorophyll and antioxidant activity during MAE. The increase of microwave power or/and the solvent amount increased saturated extraction efficiency and the extraction rate constant. However, the saturated concentration of chlorophyll and antioxidant activity increased with the increment of microwave power and the decrease in solvent amount.


Assuntos
Antioxidantes/farmacologia , Araliaceae/química , Clorofila/farmacologia , Extratos Vegetais/farmacologia , Folhas de Planta/química , Cromatografia Líquida de Alta Pressão/métodos , Etanol/química , Cinética , Micro-Ondas , Extratos Vegetais/química , Polifenóis/química , Polifenóis/farmacologia , Solventes/química
13.
Molecules ; 26(12)2021 Jun 21.
Artigo em Inglês | MEDLINE | ID: mdl-34205624

RESUMO

Studies have reported that cholesterol, a molecule found mainly in animals, is also present in some plants and algae. This study aimed to determine whether cholesterol exists in three dehydrated algae species, namely, Pyropia tenera, Saccharina japonica, and Undaria pinnatifida, and in one plant species, namely, Perilla frutescens (four perilla seed oil samples were analyzed). These species were chosen for investigation because they are common ingredients in East Asian cuisine. Gas chromatography-flame ionization detection (GC-FID) analysis found that cholesterol was present in P. tenera (14.6 mg/100 g) and in all four perilla seed oil samples (0.3-0.5 mg/100 g). High-performance liquid chromatography with evaporative light-scattering detection (HPLC-ELSD) also demonstrated that cholesterol was present in P. tenera (14.2 mg/100 g) and allowed the separation of cholesterol from its isomer lathosterol. However, cholesterol could not be detected by HPLC-ELSD in the perilla seed oil samples, most likely because it is only present in trace amounts. Moreover, liquid chromatography-tandem mass spectrometry (LC-MS/MS) confirmed the presence of cholesterol in both P. tenera and perilla seed oil. MRM results further suggested that lathosterol (a precursor of cholesterol) was present in P. tenera.


Assuntos
Perilla frutescens/metabolismo , Petróleo/metabolismo , Óleos Vegetais/metabolismo , Sementes/metabolismo , Ácido alfa-Linoleico/metabolismo , Colesterol/metabolismo , Cromatografia Líquida de Alta Pressão/métodos , Cromatografia Gasosa-Espectrometria de Massas/métodos , Espectrometria de Massas em Tandem/métodos
14.
Molecules ; 26(12)2021 Jun 21.
Artigo em Inglês | MEDLINE | ID: mdl-34205651

RESUMO

High-pressure processing (HPP) has emerged over the last 2 decades as a good alternative to traditional thermal treatment for food safety and shelf-life extension, supplying foods with similar characteristics to those of fresh products. Currently, HPP has also been proposed as a useful tool to reduce food contaminants, such as pesticides and mycotoxins. The aim of the present study is to explore the effect of HPP technology at 600 MPa during 5 min at room temperature on alternariol (AOH) and aflatoxin B1 (AFB1) mycotoxins reduction in different juice models. The effect of HPP has also been compared with a thermal treatment performed at 90 °C during 21 s. For this, different juice models, orange juice/milk beverage, strawberry juice/milk beverage and grape juice, were prepared and spiked individually with AOH and AFB1 at a concentration of 100 µg/L. After HPP and thermal treatments, mycotoxins were extracted from treated samples and controls by dispersive liquid-liquid microextraction (DLLME) and determined by HPLC-MS/MS-IT. The results obtained revealed reduction percentages up to 24% for AFB1 and 37% for AOH. Comparing between different juice models, significant differences were observed for AFB1 residues in orange juice/milk versus strawberry juice/milk beverages after HPP treatment. Moreover, HPP resulted as more effective than thermal treatment, being an effective tool to incorporate to food industry in order to reach mycotoxins reductions.


Assuntos
Aflatoxinas/química , Bebidas/análise , Sucos de Frutas e Vegetais/análise , Frutas/química , Leite/química , Vitis/química , Animais , Cromatografia Líquida de Alta Pressão/métodos , Contaminação de Alimentos/análise , Manipulação de Alimentos/métodos , Lactonas/química , Microextração em Fase Líquida/métodos , Micotoxinas/química , Espectrometria de Massas em Tandem/métodos
15.
Molecules ; 26(12)2021 Jun 08.
Artigo em Inglês | MEDLINE | ID: mdl-34201343

RESUMO

Taurine (Tau) has some important ameliorating effects on human health and is present in bivalve. For the selective analysis of Tau with other amino acids, we designed a derivatization reagent, 2,5-dioxopyrrolidin-1-yl(4-(((2-nitrophenyl)sulfonyl)oxy)-6-(3-oxomorpholino)quinoline-2-carbonyl)pyrrolidine-3-carboxylate (Ns-MOK-ß-Pro-OSu). After derivatization with Ns-MOK-ß-Pro-OSu, amino acids with Tau in Japanese littleneck clams were determined through ultra-high-performance-liquid chromatography with high-resolution tandem mass spectrometry (UHPLC-HRMS/MS) using an octadecyl silica column. We could detect 18 amino acids within 10 min. Tau, valine, glutamine, glutamic acid, and arginine in the clams were determined in the negative ion mode using the characteristic fragment ion, C6H4N1O5S, which corresponded to the 2-nitrobenzenesulfonylate moiety. The fragment ion, C6H4N1O5S, was recognized as a common feature regardless of the amino acid to be derivatized, and it was convenient for detecting amino acid derivatives with high selectivity and sensitivity. Therefore, highly selective quantification using UHPLC-HRMS/MS was possible using Ns-MOK-ß-Pro-OSu.


Assuntos
Aminoácidos/química , Cromatografia Líquida de Alta Pressão/métodos , Indicadores e Reagentes/química , Espectrometria de Massas em Tandem/métodos , Taurina/química , Ácidos Carboxílicos/química , Pirrolidinas/química , Quinolinas/química , Espectrometria de Massas por Ionização por Electrospray/métodos
16.
Molecules ; 26(12)2021 Jun 08.
Artigo em Inglês | MEDLINE | ID: mdl-34201410

RESUMO

In-process control (IPC) is an important task during chemical syntheses in pharmaceutical industry. Despite the fact that each chemical reaction is unique, the most common analytical technique used for IPC analysis is high performance liquid chromatography (HPLC). Today, the so-called "Quality by Design" (QbD) principle is often being applied rather than "Trial and Error" approach for HPLC method development. The QbD approach requires only for a very few experimental measurements to find the appropriate stationary phase and optimal chromatographic conditions such as the composition of mobile phase, gradient steepness or time (tG), temperature (T), and mobile phase pH. In this study, the applicability of a multifactorial liquid chromatographic optimization software was studied in an extended knowledge space. Using state-of-the-art ultra-high performance liquid chromatography (UHPLC), the analysis time can significantly be shortened. By using UHPLC, it is possible to analyse the composition of the reaction mixture within few minutes. In this work, a mixture of route of synthesis of apixaban was analysed on short narrow bore column (50 × 2.1 mm, packed with sub-2 µm particles) resulting in short analysis time. The aim of the study was to cover a relatively narrow range of method parameters (tG, T, pH) in order to find a robust working point (zone). The results of the virtual (modeled) robustness testing were systematically compared to experimental measurements and Design of Experiments (DoE) based predictions.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Pirazóis/química , Piridonas/química , Concentração de Íons de Hidrogênio , Projetos de Pesquisa , Software , Temperatura
17.
Molecules ; 26(13)2021 Jun 22.
Artigo em Inglês | MEDLINE | ID: mdl-34206357

RESUMO

In the current work, a simple, economical, accurate, and precise HPLC method with UV detection was developed to quantify Favipiravir (FVIR) in spiked human plasma using acyclovir (ACVR) as an internal standard in the COVID-19 pandemic time. Both FVIR and ACVR were well separated and resolved on the C18 column using the mobile phase blend of methanol:acetonitrile:20 mM phosphate buffer (pH 3.1) in an isocratic mode flow rate of 1 mL/min with a proportion of 30:10:60 %, v/v/v. The detector wavelength was set at 242 nm. Maximum recovery of FVIR and ACVR from plasma was obtained with dichloromethane (DCM) as extracting solvent. The calibration curve was found to be linear in the range of 3.1-60.0 µg/mL with regression coefficient (r2) = 0.9976. However, with acceptable r2, the calibration data's heteroscedasticity was observed, which was further reduced using weighted linear regression with weighting factor 1/x. Finally, the method was validated concerning sensitivity, accuracy (Inter and Intraday's % RE and RSD were 0.28, 0.65 and 1.00, 0.12 respectively), precision, recovery (89.99%, 89.09%, and 90.81% for LQC, MQC, and HQC, respectively), stability (% RSD for 30-day were 3.04 and 1.71 for LQC and HQC, respectively at -20 °C), and carry-over US-FDA guidance for Bioanalytical Method Validation for researchers in the COVID-19 pandemic crisis. Furthermore, there was no significant difference for selectivity when evaluated at LLOQ concentration of 3 µg/mL of FVIR and relative to the blank.


Assuntos
Amidas/análise , Amidas/sangue , Antivirais/análise , Antivirais/sangue , Bioensaio/métodos , COVID-19/tratamento farmacológico , Cromatografia Líquida de Alta Pressão/métodos , Extração Líquido-Líquido/métodos , Pirazinas/análise , Pirazinas/sangue , Aciclovir/análise , Aciclovir/sangue , COVID-19/sangue , Calibragem , Estabilidade de Medicamentos , Congelamento , Humanos , Padrões de Referência , Reprodutibilidade dos Testes , Solventes/química
18.
Molecules ; 26(11)2021 Jun 07.
Artigo em Inglês | MEDLINE | ID: mdl-34200200

RESUMO

Epilobium angustifolium L. is a popular and well-known medicinal plant. In this study, an attempt to evaluate the possibility of using this plant in preparations for the care and treatment of skin diseases was made. The antioxidant, antiaging and anti-inflammatory properties of ethanolic extracts from Epilobium angustifolium (FEE) were assessed. Qualitative and quantitative evaluation of extracts chemically composition was performed by gas chromatography with mass spectrometry (GC-MS) and high-performance liquid chromatography (HPLC). The total polyphenol content (TPC) of biologically active compounds, such as the total content of polyphenols (TPC), flavonoids (TFC), and assimilation pigments, as well as selected phenolic acids, was assessed. FEE was evaluated for their anti-inflammatory and antiaging properties, achieving 68% inhibition of lipoxygenase activity, 60% of collagenase and 49% of elastase. FEE also showed high antioxidant activity, reaching to 87% of free radical scavenging using 2,2-diphenyl-1-picrylhydrazyl (DPPH) and 59% using 2,2'-azinobis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS). Additionally, in vitro penetration studies were performed using two vehicles, i.e., a hydrogel and an emulsion containing FEE. These studies showed that the active ingredients contained in FEE penetrate through human skin and accumulate in it. The obtained results indicate that E. angustifolium may be an interesting plant material to be applied as a component of cosmetic and dermatological preparations with antiaging and anti-inflammatory properties.


Assuntos
Cosméticos/química , Fármacos Dermatológicos/química , Epilobium/química , Extratos Vegetais/química , Anti-Inflamatórios/química , Antioxidantes/química , Compostos de Bifenilo/química , Cromatografia Líquida de Alta Pressão/métodos , Flavonoides/química , Cromatografia Gasosa-Espectrometria de Massas/métodos , Humanos , Plantas Medicinais/química , Polifenóis/química , Pele/efeitos dos fármacos
19.
Molecules ; 26(12)2021 Jun 10.
Artigo em Inglês | MEDLINE | ID: mdl-34200974

RESUMO

In this study, we investigated the antioxidant and anti-inflammatory phytochemicals and paramagnetic species in dragon fruit using high-performance liquid chromatography (HPLC) and electron paramagnetic resonance (EPR). HPLC analysis demonstrated that dragon fruit is enriched with bioactive phytochemicals, with significant variations between each part of the fruit. Anthocyanins namely, cyanidin 3-glucoside, delphinidin 3-glucoside, and pelargonidin 3-glucoside were detected in the dragon fruit peel and fresh red pulp. Epicatechin gallate, epigallocatechin, caffeine, and gallic acid were found in the dragon fruit seed. Additionally, 25-100 mg × L-1 of dragon fruit pulp and peel extracts containing enrichment of cyanidin 3-glucoside were found to inhibit the production of reactive oxygen species (ROS), reactive nitrogen species (RNS), inducible nitric oxide synthase (iNOS), and cyclooxygenase-2 (COX-2) in cell-based studies without exerted cytotoxicity. EPR primarily detected two paramagnetic species in the red samples. These two different radical species were assigned as stable radicals and Mn2+ (paramagnetic species) based on the g-values and hyperfine components. In addition, the broad EPR line width of the white peel can be correlated to a unique moiety in dragon fruit. Our EPR and HPLC results provide new insight regarding the phytochemicals and related stable intermediates found in various parts of dragon fruit. Thus, we suggest here that there is the potential to use dragon fruit peel, which contains anthocyanins, as a natural active pharmaceutical ingredient.


Assuntos
Anti-Inflamatórios/farmacologia , Antioxidantes/farmacologia , Cactaceae/química , Frutas/química , Compostos Fitoquímicos/farmacologia , Extratos Vegetais/farmacologia , Animais , Antocianinas/farmacologia , Linhagem Celular , Cromatografia Líquida de Alta Pressão/métodos , Espectroscopia de Ressonância de Spin Eletrônica/métodos , Camundongos , Células RAW 264.7 , Sementes/química
20.
Molecules ; 26(12)2021 Jun 15.
Artigo em Inglês | MEDLINE | ID: mdl-34203624

RESUMO

Millettia pulchra is traditionally used for treating diseases, including joint pain, fever, anemia, and allergies. It is also a potential resource of natural flavonoid derivatives, which represents major constituents of this plant. This study aimed to isolate the major compounds from M. pulchra radix, develop and validate the HPLC-PDA method to determine their contents, and optimize its extraction. Four major flavonoid derivatives (karanjin, lanceolatin B, 2",2"-dimethylpyrano-[5″,6″:7,8]-flavone, and pongamol) were isolated using silica gel column chromatography, crystallization techniques in large amounts with high purities (>95%). A simple, accurate high-performance liquid chromatography-photodiode array (HPLC-PDA) detection method has been developed and validated with significantly statistical impacts according to International Conference on Harmonization (ICH) guidelines. The Response Surface Methodology (RSM), Artificial Neural Network (ANN) models were employed to predictive performance and optimization of the extraction process. The optimized conditions for the extraction of major flavonoids were: extraction time (twice), solvent/material ratio (9.5), and ethanol concentration (72.5%). Our research suggests an effective method, which will be helpful for quality control in the pharmaceutical development of this species.


Assuntos
Flavonoides/química , Flavonoides/isolamento & purificação , Millettia/química , Antioxidantes/química , China , Cromatografia Líquida de Alta Pressão/métodos , Etanol/química , Millettia/metabolismo , Extratos Vegetais/química , Raízes de Plantas/química , Solventes/química
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