RESUMO
Ginkgo biloba is a popular medicinal plant widely used in numerous herbal products, including food supplements. Due to its popularity and growing economic value, G. biloba leaf extract has become the target of economically motivated adulterations. There are many reports about the poor quality of ginkgo products and their adulteration, mainly by adding flavonols, flavonol glycosides, or extracts from other plants. In this work, we developed an approach using two-trace two-dimensional correlation spectroscopy (2T2D COS) in UV-Vis range combined with multilinear principal component analysis (MPCA) to detect potential adulteration of twenty G. biloba food supplements. UV-Vis spectral data are obtained for 80% methanol and aqueous extracts in the range of 245-410 nm. Three series of two-dimensional correlation spectra were interpreted by visual inspection and using MPCA. The proposed relatively quick and straightforward approach successfully differentiated supplements adulterated with rutin or those lacking ginkgo leaf extract. Supporting information about adulteration was obtained from the difference between the DPPH radical scavenging capacity of both extracts and from chromatographic (HPLC-DAD) fingerprints of methanolic samples.
Assuntos
Suplementos Nutricionais/análise , Contaminação de Alimentos/análise , Ginkgo biloba/química , Espectrofotometria Ultravioleta/métodos , Quimioinformática/métodos , Cromatografia Líquida de Alta Pressão , Cromatografia de Fase Reversa , Quempferóis/análise , Polônia , Análise de Componente Principal , Quercetina/análise , Rutina/análiseRESUMO
Phenolic compounds in the fruit of American cranberry (Vaccinium macrocarpon Aiton) determine the antioxidant, anti-inflammatory, anticancer, and other biological effects. The berries are used in the production of medicinal preparations and food supplements, which highlights the importance of qualitative and quantitative analysis of phenolic compounds in cranberry fruit raw material. The aim of our study was to develop and validate an efficient, cost-effective, reproducible, and fast UPLC-DAD methodology for the evaluation of the qualitative and quantitative composition of phenolic compounds in raw material and preparations of American cranberry fruit. During the development of the methodology, chlorogenic acid and the following flavonols were identified in cranberry fruit samples: myricetin-3-galactoside, quercetin-3-galactoside, quercetin-3-glucoside, quercetin-3-α-L-arabinopyranoside, quercetin-3-α-L-arabinofuranoside, quercetin-3-rhamnoside, myricetin, and quercetin. The developed and optimized UPLC-DAD methodology was validated according to the guidelines of the International Council for Harmonization (ICH), evaluating the following parameters: range, specificity, linearity (R2 > 0.999), precision (%RSD < 2%), LOD (0.38-1.01 µg/mL), LOQ (0.54-3.06 µg/mL), and recovery (80-110%). The developed methodology was applied to evaluate the qualitative and quantitative composition of phenolic compounds in fruit samples of cranberry cultivars 'Baifay', 'Bergman', 'Prolific', and 'Searles', as well as 'Bain-MC' and 'BL-12' clones. In the tested samples, the majority (about 70%) of the identified flavonols were quercetin derivatives. The greatest amount of quercetin-3-galactoside (1035.35 ± 4.26 µg/g DW) was found in fruit samples of the 'Searles' cultivar, and the greatest amount of myricetin-3-galactoside (940.06 ± 24.91 µg/g DW) was detected in fruit samples of the 'Woolman' cultivar.
Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Frutas/química , Fenóis/análise , Fenóis/química , Espectrofotometria Ultravioleta/métodos , Vaccinium macrocarpon/química , Ácido Clorogênico/análise , Confiabilidade dos Dados , Flavonóis/análise , Extratos Vegetais/análise , Extratos Vegetais/químicaRESUMO
Green nanoparticle synthesis is an environmentally friendly approach that uses natural solvents. It is preferred over chemical and physical techniques due to the time and energy savings. This study aimed to synthesize zinc oxide nanoparticles (ZnO NPs) through a green method that used Phlomis leaf extract as an effective reducing agent. The synthesis and characterization of ZnO NPs were confirmed by UV-Vis spectrophotometry, Fourier Transform Infrared Spectroscopy (FTIR), X-ray Diffraction (XRD), Dynamic light scattering (DLS), Zeta potential, and Field Emission Scanning Electron Microscope (FESEM) techniques. In vitro cytotoxicity was determined in L929 normal fibroblast cells using MTT assay. The antibacterial activity of ZnO nanoparticles was investigated using a disk-diffusion method against S. aureus and E. coli, as well as minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) content concentrations. XRD results confirmed the nanoparticles' crystalline structure. Nanoparticle sizes were found to be around 79 nm by FESEM, whereas the hydrodynamic radius of nanoparticles was estimated to be around 165 ± 3 nm by DLS. FTIR spectra revealed the formation of ZnO bonding and surfactant molecule adsorption on the surface of ZnO NPs. It is interesting to observe that aqueous extracts of Phlomis leave plant are efficient reducing agents for green synthesis of ZnO NPs in vitro, with no cytotoxic effect on L929 normal cells and a significant impact on the bacteria tested.
Assuntos
Química Verde/métodos , Nanopartículas Metálicas/química , Phlomis/metabolismo , Antibacterianos/farmacologia , Anti-Infecciosos/farmacologia , Bactérias/efeitos dos fármacos , Testes de Sensibilidade Microbiana , Extratos Vegetais/química , Substâncias Redutoras/farmacologia , Espectrometria por Raios X/métodos , Espectrofotometria Ultravioleta/métodos , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Difração de Raios X/métodos , Óxido de Zinco/químicaRESUMO
CONTEXT: Stomach ulcer is one of the most common gastrointestinal problems in the world. OBJECTIVE: This study aimed to isolate flavonoid compounds from methanol extract of the aerial parts of Stachytarpheta jamaicensis (L.) Vahl. and evaluate its protective and therapeutic effects against gastric ulcer. MATERIALS AND METHODS: Chromatographic techniques were used for the identification of the isolated compounds. To explore the effects of the plant extract, it was administrated by oral gavage for one week either before or post-ethanol ulcer induction. Ranitidine was also evaluated as a reference drug. Stomach pH, gastric juice volume, lesions number, glutathione, superoxide dismutase, malondialdehyde, succinate dehydrogenase, lactate dehydrogenase, acid phosphatase, Interleukin-10, intracellular adhesion molecule-1, prostaglandin E2, and total protein levels were estimated in gastric tissue. Stomach histopathological features were also monitored. RESULTS: Six flavonoid compounds were isolated, where five of them were isolated for the first time (vitexin, isovitexin, apigenin 7,4'-dimethyl ether, 5,7,2'-trimethoxyflavone, and scutellarein), while apigenin was previously reported. Treatment with plant extract recorded amelioration in all the biochemical parameters. CONCLUSION: The methanol extract of plant aerial parts had prophylactic and treatment effects against gastric ulcer in rats, where its treatment effect exceeded its protective role. The extract recorded anti-inflammatory, and antioxidant effects due to the presence of flavonoid compounds.
Assuntos
Antiulcerosos/farmacologia , Flavonoides/farmacologia , Úlcera Gástrica/prevenção & controle , Verbenaceae/química , Animais , Antiulcerosos/uso terapêutico , Biomarcadores/metabolismo , Espectroscopia de Ressonância Magnética Nuclear de Carbono-13/métodos , Flavonoides/química , Flavonoides/isolamento & purificação , Mucosa Gástrica/efeitos dos fármacos , Mucosa Gástrica/enzimologia , Mucosa Gástrica/patologia , Mediadores da Inflamação/metabolismo , Masculino , Estrutura Molecular , Estresse Oxidativo , Componentes Aéreos da Planta/química , Extratos Vegetais/farmacologia , Extratos Vegetais/uso terapêutico , Espectroscopia de Prótons por Ressonância Magnética/métodos , Ratos , Ratos Wistar , Espectrofotometria Ultravioleta/métodosRESUMO
Iron, one of the most common metals in the environment, plays a fundamental role in many biological as well as biogeochemical processes, which determine its availability in different oxidation states. Its relevance in environmental and industrial chemistry, human physiology, and many other fields has made it necessary to develop and optimize analysis techniques for accurate determination. Spectrophotometric methods are the most frequently applied in the analytical determination of iron in real samples. Taking advantage of the fact that desferrioxamine B, a trihydroxamic acid used since the 1970s in chelation therapy for iron overload treatment, forms a single stable 1:1 complex with iron in whichever oxidation state it can be found, a smart spectrophotometric method for the analytical determination of iron concentration was developed. In particular, the full compliance with the Lambert-Beer law, the range of iron concentration, the influence of pH, and the interference of other metal ions have been taken into account. The proposed method was validated in terms of LoD, LoQ, linearity, precision, and trueness, and has been applied for total iron determination in natural water certified material and in biological reference materials such as control human urine and control serum.
Assuntos
Desferroxamina/química , Quelantes de Ferro/química , Ferro/análise , Calibragem , Colorimetria/métodos , Humanos , Concentração de Íons de Hidrogênio , Ferro/urina , Ligantes , Limite de Detecção , Espectrometria de Massas/métodos , Reprodutibilidade dos Testes , Espectrofotometria Atômica/métodos , Espectrofotometria Ultravioleta/métodos , Água/químicaRESUMO
Recently, the biosynthesis of zinc oxide nanoparticles (ZnO NPs) from crude extracts and phytochemicals has attracted much attention. Green synthesis of NPs is cost-effective, eco-friendly, and is a promising alternative for chemical synthesis. This study involves ZnO NPs synthesis using Rubus fairholmianus root extract (RE) as an efficient reducing agent. The UV spectrum of RE-ZnO NPs exhibited a peak at 357 nm due to intrinsic bandgap absorption and an XRD pattern that matches the ZnO crystal structure (JCPDS card no: 36-1451). The average particle size calculated from the Debye-Scherrer equation is 11.34 nm. SEM analysis showed that the RE-ZnO NPs spherical in shape with clusters (1-100 nm). The antibacterial activity of the NPs was tested against Staphylococcus aureus using agar well diffusion, minimum inhibitory concentration, and bacterial growth assay. The R. fairholmianus phytochemicals facilitate the synthesis of stable ZnO NPs and showed antibacterial activity.
Assuntos
Nanopartículas Metálicas/química , Extratos Vegetais/farmacologia , Raízes de Plantas/química , Rubus/química , Óxido de Zinco/química , Cristalografia por Raios X , Testes de Sensibilidade Microbiana , Espectrofotometria Ultravioleta/métodos , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Staphylococcus aureus/efeitos dos fármacosRESUMO
Pigmentation, a process controlled by melanogenesis, plays a vital role in protecting the skin against harmful ultraviolet rays. The level of protection is compromised in case of hypopigmentation. This study aimed to evaluate an Aspalathus linearis extract, fractions and phytoconstituents, for their efficacy on melanogenesis stimulation. Fifteen compounds were kinetically assessed against tyrosinase; the rate-limiting enzyme of melanogenesis. Aspalathin and catechin significantly (p value < 0.001) increased the enzymatic rate, showing 50% stimulatory effects at 119.70 ± 2.06 µg/mL and 143.30 ± 2.74 µg/mL, respectively, by acting as subversive substrates. Five compounds inhibited the enzyme's activity, of which four exhibited competitive inhibition. To investigate the molecular interactions between the compounds and the active site, molecular docking was done, using tyrosinase (PBD: 2Y9X) and tyrosinase related protein 1 (PBD: 5M8P). All the compounds docked successfully with acceptable docking scores. Further quantitative structure-activity relationship analysis identified potential functional groups, linked to the specific activity. The crude extract, its fractions, and compounds exhibited low antiproliferative activity with 50% cell viability at concentrations higher than 100 µg/mL. Finally, both aspalathin and catechin exhibited a significant increase (4.5%) in melanin production at 119.82 µg/mL and 76.92 µg/mL, respectively. This is the first report of A. linearis' compounds on skin re-pigmentation.
Assuntos
Aspalathus/química , Melaninas/biossíntese , Monofenol Mono-Oxigenase/efeitos dos fármacos , Extratos Vegetais/farmacologia , Cromatografia Líquida/métodos , Simulação por Computador , Humanos , Melanócitos/efeitos dos fármacos , Simulação de Acoplamento Molecular , Relação Quantitativa Estrutura-Atividade , Pigmentação da Pele/efeitos dos fármacos , Espectrofotometria Ultravioleta/métodosRESUMO
In the present study, 200 Brown commercial egg-type layers (60 wk old) were used to study the effects of different levels of ecofriendly synthesis of calcium (Ca) nanoparticles (0.0, 0.50, 1.0, and 1.5 g/kg diet) with biocompatible Sargassum latifolium algae extract (SL-CaNps) on exterior egg quality traits, electronic microscopic view of eggshells, Ca and phosphorus (P) retention, serum Ca and P concentrations, and the histology of the uterus. Hens fed with dietary SL-CaNps powder had higher egg weight and shell weight % values than those of the control group. All SL-CaNps treatment groups had the greatest values of shell weight per unit surface area and shell thickness. Dietary supplementation of SL-CaNps at graded levels up to 1.5 g/kg diet had higher serum Ca and inorganic P levels than that of the control. Laying hens fed with SL-CaNps-added diets had beneficial effects on shell ultrastructure in terms of well-developed palisade and mammillary layers. The numbers of apical cells along the branched tubular gland were greater in SL-CaNps-treated groups than those of control. Conclusively, supplementing SL-CaNps powder up to 1.5 g/kg to the diet of laying hens improved eggshell thickness, shell weight% and shell weight per unit surface and has no adverse effect on their eggshell quality or electronic microscopic view of their eggshell.
Assuntos
Cálcio/administração & dosagem , Galinhas/fisiologia , Casca de Ovo/ultraestrutura , Ovos/normas , Nanopartículas , Sargassum/química , Fatores Etários , Ração Animal/análise , Animais , Galinhas/anatomia & histologia , Dieta/veterinária , Suplementos Nutricionais , Feminino , Microscopia Eletrônica de Varredura/veterinária , Microscopia Eletrônica de Transmissão/veterinária , Distribuição Aleatória , Espectrofotometria Ultravioleta/métodos , Espectrofotometria Ultravioleta/veterináriaRESUMO
Scopoletin has previously been reported as a biomarker for the standardization of Paederia foetida twigs. This study is the first report on the determination and quantification of scopoletin using quantitative nuclear magnetic resonance (qNMR) in the different extracts of Paederia foetida twigs. The validated qNMR method showed a good linearity (r2 = 0.9999), limit of detection (LOD) (0.009 mg/mL), and quantification (LOQ) (0.029 mg/mL), together with high stability (relative standard deviation (RSD) = 0.022%), high precision (RSD < 1%), and good recovery (94.08-108.45%). The quantification results of scopoletin concentration in chloroform extract using qNMR and microplate ultraviolet-visible (UV-vis) spectrophotometer was almost comparable. Therefore, the qNMR method is deemed accurate and reliable for quality control of Paederia foetida and other medicinal plants without extensive sample preparation.
Assuntos
Biomarcadores Farmacológicos/análise , Espectroscopia de Ressonância Magnética/métodos , Rubiaceae/química , Escopoletina/análise , Espectrofotometria Ultravioleta/métodos , Limite de Detecção , Extratos Vegetais/análise , Extratos Vegetais/química , Preparações de Plantas/análise , Plantas Medicinais/química , Sensibilidade e Especificidade , Solventes/químicaRESUMO
Tea is an important beverage in humans' daily lives. For a long time, tea grade identification relied on sensory evaluation, which requires professional knowledge, so is difficult and troublesome for laypersons. Tea chemical component detection usually involves a series of procedures and multiple steps to obtain the final results. As such, a simple, rapid, and reliable method to judge the quality of tea is needed. Here, we propose a quick method that combines ultraviolet (UV) spectra and color difference to classify tea. The operations are simple and do not involve complex pretreatment. Each method requires only a few seconds for sample detection. In this study, famous Chinese green tea, Huangshan Maofeng, was selected. The traditional detection results of tea chemical components could not be used to directly determine tea grade. Then, digital instrument methods, UV spectrometry and colorimetry, were applied. The principal component analysis (PCA) plots of the single and combined signals of these two instruments showed that samples could be arranged according to grade. The combined signal PCA plot performed better with the sample grade descending in clockwise order. For grade prediction, the random forest (RF) model produced a better effect than the support vector machine (SVM) and the SVM + RF model. In the RF model, the training and testing accuracies of the combined signal were all 1. The grades of all samples were correctly predicted. From the above, the UV spectrum combined with color difference can be used to quickly and accurately classify the grade of Huangshan Maofeng tea. This method considerably increases the convenience of tea grade identification.
Assuntos
Análise de Alimentos/métodos , Espectrofotometria Ultravioleta/métodos , Chá/química , Camellia sinensis/química , Cor , Análise de Alimentos/estatística & dados numéricos , Humanos , Análise de Componente Principal , Espectrofotometria Ultravioleta/estatística & dados numéricos , Máquina de Vetores de Suporte , PaladarRESUMO
Selenium-doped nanostructure has been considered as an attractive approach to enhance the antibacterial activity of calcium phosphate (CaP) materials in diverse medical applications. In this study, the selenium-doped biphasic calcium phosphate nanoparticles (SeB-NPs) were first synthesized. Then, silver was in situ incorporated into SeB-NPs to obtain nanostructured composite nanoparticles (AgSeB-NPs). Both SeB-NPs and AgSeB-NPs were characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), ultraviolet-visible spectroscopy (UV-Vis), X-ray photoelectron spectroscopy (XPS), and Raman spectra. The results confirmed that the SeO32- was doped at the PO43- position and silver nanoparticles were deposited on the surface of SeB-NPs. Next, Transmission Electron Microscopy (TEM) analysis displayed that the prepared AgSeB-NPs had a needle-cluster-like morphology. CCK-8 analysis revealed SeB-NPs and AgSeB-NPs had good cytocompatibility with osteoblasts. The antibacterial activity of the prepared AgSeB-NPs was confirmed by using Gram-negative E. coli and Gram-positive S. aureus. The above results manifested the significance of the final AgSeB-NPs for biomedical applications.
Assuntos
Antibacterianos/farmacologia , Hidroxiapatitas/química , Hidroxiapatitas/farmacologia , Nanopartículas Metálicas/química , Nanoestruturas/química , Selênio/química , Células Cultivadas , Escherichia coli/efeitos dos fármacos , Humanos , Testes de Sensibilidade Microbiana/métodos , Microscopia Eletrônica de Transmissão/métodos , Tamanho da Partícula , Espectroscopia Fotoeletrônica/métodos , Prata/química , Espectrofotometria Ultravioleta/métodos , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Staphylococcus aureus/efeitos dos fármacos , Difração de Raios X/métodosRESUMO
The aim of our study is to develop a new vortex assisted-ionic liquid dispersive liquid-liquid microextraction (VA-IL-DLLM) method for preconcentration and determination of the quercetin in tea, honey, fruit juice and wine samples by spectrophotometry. The method is based on pH sensitive ion-pair formation between quercetin and rhodamine B at pH 6.5 by donor-acceptor mechanism, and then dispersion of the complex in the fine-drops of ionic liquid (IL). In this context, the effects of pH, concentrations of ion-pairing reagent, the IL, vortex time and dispersive solvent type on the preconcentration process of quercetin were investigated using a 2-level-5-factor central composite half fraction design (CCD) as experimental design for response surface methodology (RSM). Quantitative model was developed to determine the quercetin in food samples, and it is verified by analysis of variance (ANOVA) at a 95% confidence level (Pâ¯<â¯0.05). Response surface plots and contour plots obtained by the model are used to determine the interactions of experimental variables. After the optimization, calibration graph was obtained between 35 and 750 µg L-1 with the detection limit of 10.2 µg L-1. The recovery and relative standard deviations (RSD%) were in range of 94-104%, and in range of 2.5-4.2%, respectively. The accuracy and precision of the method were tested by the experimental studies such as recoveries, intermediate precision, trueness and expanded uncertainty. A comparison of the current results to those reported for other studies is also presented.
Assuntos
Sucos de Frutas e Vegetais/análise , Mel/análise , Microextração em Fase Líquida/métodos , Quercetina/análise , Chá/química , Vinho/análise , Análise de Variância , Artefatos , Análise de Alimentos/métodos , Concentração de Íons de Hidrogênio , Líquidos Iônicos/química , Limite de Detecção , Microextração em Fase Líquida/estatística & dados numéricos , Reprodutibilidade dos Testes , Espectrofotometria Ultravioleta/métodosRESUMO
Pyrethroid residues in traditional Chinese medicines have been a serious threat to the health and treatment of patients. However, because of the matrix complexity of traditional Chinese medicine, the detection of pyrethroid residues remains a challenge. Therefore, we developed a QuEChERS method coupled with high-performance liquid chromatography and ultraviolet detection (HPLC-UV) for the determination of pyrethroid pesticides in three kinds of traditional Chinese medicine oral liquid preparations, and we investigated and optimized the extraction conditions. The matrix effect was estimated in the organic solvent and the actual samples by comparing the slopes of calibration curves, and the results showed that the matrix effect is not significant when using the modified QuEChERS method. The pyrethroid pesticides could be completely separated in 30 min. The linear correlation coefficients were more than 0.999, and the recoveries of all the pyrethroid pesticides ranged from 87.2% to 104.8%. The intra-day precisions (n = 5) were 2.44-4.62%, and the inter-day precisions (n = 5) were 1.06-3.02%. Moreover, the limits of detection were in the range of 0.007-0.018 ng mL-1, while the limits of quantitation were in the range of 0.022-0.057 ng mL-1. This simple, low-cost, and highly sensitive analytical method can be a potential tool for the analysis of pyrethroid residues in traditional Chinese medicine oral liquid preparations.
Assuntos
Medicamentos de Ervas Chinesas/análise , Resíduos de Praguicidas/análise , Piretrinas/análise , Cromatografia Líquida de Alta Pressão/métodos , Medicamentos de Ervas Chinesas/química , Humanos , Espectrofotometria Ultravioleta/métodosRESUMO
Background: Aloe vera polysaccharides are considered to be the primary active components that provide numerous anecdotal health benefits. Objective: Several analytical methods are currently being used to quantitate the acemannan content of aloe vera processed raw materials. Some involve the use of very expensive and intricate equipment that is not normally found in production facilities. This document describes a single-laboratory validation for a very simple and inexpensive method that will be supported by a future multi-laboratory validation determination. Methods: The acetyl groups on the acemannan are converted into a ferric-acetohydroxamic complex that is quantitated using a simple and inexpensive UV-Vis spectrophotometer at 540 nm. Results: The analytical range for this method is 0.03-100% acemannan in both liquid and powdered materials. The recovery rate were 98-105% for both liquid and powdered samples. The repeatability precision was <2% at a level close to the LOQ. Conclusions: The results met the Standard Method Performance Requirements set by the AOAC Stakeholder Panel on Dietary Supplements. Highlights: The AOAC Expert Review Panel approved the present method as AOAC Official First Action 2018.14.
Assuntos
Aloe/química , Mananas/análise , Espectrofotometria Ultravioleta/métodos , Acetilação , Complexos de Coordenação/análise , Ferro/química , Mananas/químicaRESUMO
INTRODUCTION: Galloylquinic acid derivatives and flavonoids are the main phenolic metabolites found in Copaifera langsdorffii leaves (Leguminosae, Detarioideae), a medicinal plant with potential therapeutic application in the treatment of kidney stones. The factors that affect metabolite production in this plant species are not well understood but may include environmental and genetic factors. OBJECTIVE: To quantify the variation in metabolite production over a 12-month period for 10 groups of C. langsdorffii cultivated under the same environmental conditions. METHODS: Copaifera langsdorffii seeds were collected from 10 different regions in southeast, Brazil and grown in the same field. HPLC-UV was used to quantify nine galloylquinic acid derivatives and two flavonoids in leaf samples from mature trees. Climate data for humidity, radiation, precipitation and temperature were provided by the National Institute of Meteorology, Brazil. Multivariate analyses were performed to correlate chemical and environmental variables. RESULTS: The overall effect of environmental factors on the production of phenolic metabolites was uniform among C. langsdorffii groups. Chemical variation between groups was present, but small, and probably due to differences in their genetics and physiology. Seasonal changes influenced the production of the major phenolic metabolites, with increases in temperature and radiation levels favouring metabolite production. CONCLUSION: When C. langsdorffii trees are cultivated in the same environment, the production of the major secondary metabolites found in their leaves is very similar quantitatively, varying based on geographic location of original population and seasonal changes. This favours the standardisation of plant raw material for the production of a phytomedicine.
Assuntos
Fabaceae/metabolismo , Fenóis/análise , Folhas de Planta/metabolismo , Cromatografia Líquida de Alta Pressão/métodos , Geografia , Fenóis/metabolismo , Fenóis/normas , Padrões de Referência , Estações do Ano , Espectrofotometria Ultravioleta/métodosRESUMO
A fully automated method for the determination of lovastatin in dietary supplements containing red yeast rice has been developed. It uses a sequential injection analysis system combined with solid-phase extraction applying highly selective molecularly imprinted polymer sorbent. A miniaturized column for on-line extraction was prepared by packing 4.5 mg of the sorbent in a 5.0 × 2.5-mm-i.d. cartridge, which was used in the flow manifold. Sequential injection analysis manifold enabled all steps of lovastatin extraction and continuous spectrophotometric detection at 240 nm. A limit of detection of 60 µg g-1, a limit of quantitation of 200 µg g-1, and a linear calibration range of 200-2000 µg g-1 were achieved. Intra-day and inter-day precision values (RSD) were ≤ 6.7% and ≤ 4.9%, respectively, and method recovery values of spiked red yeast rice extracts at 200, 1000, and 2000 µg g-1 concentration levels were 82.9, 95.2, and 87.7%. Our method was used for determination of lovastatin lactone in four dietary supplements containing red yeast rice as a natural source of lovastatin, also known as monacolin K. The extracted samples were subsequently analyzed by the reference UHPLC-MS/MS method. Statistical comparison of results (F test, t test, α = 0.05) obtained by both methods did not reveal significant difference. A substantial advantage of the new automated approach is high sample throughput thanks to the analysis time of 7.5 min, miniaturization via down-scaling the extraction column, and smaller sample and solvent consumption, as well as reduced generation of waste. Graphical abstract á .
Assuntos
Anticolesterolemiantes/análise , Produtos Biológicos/análise , Suplementos Nutricionais/análise , Lovastatina/análise , Impressão Molecular/métodos , Extração em Fase Sólida/métodos , Cromatografia Líquida de Alta Pressão/instrumentação , Cromatografia Líquida de Alta Pressão/métodos , Desenho de Equipamento , Análise de Injeção de Fluxo/instrumentação , Análise de Injeção de Fluxo/métodos , Limite de Detecção , Impressão Molecular/instrumentação , Polímeros/química , Extração em Fase Sólida/instrumentação , Espectrofotometria Ultravioleta/instrumentação , Espectrofotometria Ultravioleta/métodos , Espectrometria de Massas em Tandem/instrumentação , Espectrometria de Massas em Tandem/métodosRESUMO
INTRODUCTION: Phenolic compounds present in Achyrocline satureioides are known to have therapeutic benefits like antioxidant, anti-inflammatory, and antitumour properties. The main polyphenols present in the plant are quercetin (QCT), luteolin (LUT), 3-O-methylquercetin (3OMQ), and achyrobichalcone (ACB). However, the effective isolation and purification of these compounds from A. satureioides inflorescences are not an easy task. OBJECTIVE: To develop an efficient high-performance counter-current chromatography (HPCCC) method for quick separation and purification of naturally occurring phenolic compounds from the extract of A. satureioides. METHODOLOGY: A two-step HPCCC semi-preparative isolation method was developed using a solvent system composed of n-hexane/ethyl acetate/methanol/water (0.8:1.0:0.8:1.0) and dichloromethane/methanol/water (3.5:3.5:2.5). RESULTS: The HPCCC method was used to obtain two fractions. The first fraction (F1 ) contained high levels of ACB, among other constituents, while the second fraction (F2 ) contained mostly QCT, LUT, and 3OMQ. Besides the high ACB content, F1 contained three other flavonoid-aglycones (kaempferol, 97.3%; isokaempferide, 92.4%; and 3,3'-di-O-methylquercetin, 95.2%) identified by an ultra-performance liquid chromatography system coupled to a quadrupole time-of-flight with high-definition mass spectrometry (UPLC-QTOF/HDMS) and nuclear magnetic resonance (NMR) analysis. Purity levels of ACB, 3OMQ, QCT, and LUT were 98.0, 97.0, 97.5, and 90.2%, respectively. CONCLUSION: This is the first time that high purity ACB and six other flavonoids were obtained from A. satureioides inflorescences by HPCCC. These excellent results reveal the potential and versatility of HPCCC as a technique to produce different types of products from this plant species on a semi-preparative scale: enriched fractions, new metabolites, or high purity compounds.
Assuntos
Achyrocline/química , Distribuição Contracorrente/métodos , Polifenóis/isolamento & purificação , Biflavonoides/análise , Espectroscopia de Ressonância Magnética Nuclear de Carbono-13/métodos , Luteolina/análise , Extratos Vegetais/química , Polifenóis/normas , Espectroscopia de Prótons por Ressonância Magnética/métodos , Quercetina/análogos & derivados , Quercetina/análise , Padrões de Referência , Espectrofotometria Ultravioleta/métodosRESUMO
Thymus vulgaris is used for various health benefits and culinary, nevertheless, report on its macromolecules is absent. Here, we report chemical compositions of the polysaccharides isolated from its leaf by sequential extraction with inorganic solvents. In particular, chemical profile of a unique rhamnogalacturonan I type polysaccharide containing ester linked phenolic acids has been described. Sugar compositional, TLC, UV-spectrometric and ESI-MS analyses of oligosaccharides generated from this polysaccharide by enzyme digestion, controlled acid hydrolysis and Smith degradation revealed atypical fine structural details. Biochemical analysis demonstrated dose-dependent antioxidant activity. A combination of large neutral side chains of the ramified region and ester linked phenolic acids are regarded as the functional sites. Ultraviolet spectrometric and fluorimetric analyses showed that this polysaccharide forms a homogeneous water-soluble complex with bovine serum albumin (binding constant, Kâ¯=â¯2.91â¯×â¯106/M). Consequently, water extraction affords a polysaccharide which induces pharmacological effect; this underlines the impact of thyme as natural dietetic antioxidant.
Assuntos
Antioxidantes/química , Folhas de Planta/química , Polissacarídeos/química , Soroalbumina Bovina/química , Thymus (Planta)/química , Hidrólise , Hidroxibenzoatos/química , Pectinas/química , Espectrofotometria Ultravioleta/métodos , Água/químicaRESUMO
Green tea is a popular beverage consumed worldwide. Its quality should be controlled adequately as the quality is influenced by several factors in addition to adulterations. This study aimed to develop a simple method for assessing the quality of green tea samples obtained from the South and the East Asian regions. The UV-vis, FTIR and HPLC data from 38 samples were subjected to multivariate analyses using the unsupervised recognition techniques comprising Hierarchical Cluster Analysis (HCA) and Principal Component Analysis (PCA). The model for their authentication was constructed and validated by applying the supervised recognition techniques as Soft Independent Modeling of Class Analogy (SIMCA) and Partial Least Square Discriminant Analysis (PLS-DA). The percentages of caffeine in the identified samples were determined using a validated HPLC assay in addition to in vitro determination of their antioxidant activity using DPPH radical-scavenging capacity assay. HCA and PCA based on UV data successfully distributed the tested samples into informative clusters. However, that obtained from visible data could only differentiate samples with respect to their powdered condition. On the contrary, PCA from FTIR and HPLC data could hardly discriminate any of the samples. The models constructed using SIMCA and PLS-DA showed a good class separation between the South and the East Asian samples. The percentages of caffeine in the identified samples and the IC50 in DPPH assay are greatly diverse among all the tested samples. Thus, UV spectroscopy and chemometrics have provided a simple and quick tool for the quality control of commercial green tea samples.
Assuntos
Antioxidantes/análise , Cafeína/análise , Análise de Componente Principal/métodos , Controle de Qualidade , Chá/química , Compostos de Bifenilo/química , Cromatografia Líquida de Alta Pressão/métodos , Análise por Conglomerados , Análise Discriminante , Sequestradores de Radicais Livres/química , Análise Multivariada , Picratos/química , Espectrofotometria Ultravioleta/métodos , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Chá/normasRESUMO
The potential of selected spectroscopic methods - UV-Vis, synchronous fluorescence and NIR as well a data fusion of the measurements by these methods - for the classification of tea samples with respect to the production process was examined. Four classification methods - Linear Discriminant Analysis (LDA), Quadratic Discriminant Analysis (QDA), Regularized Discriminant Analysis (RDA) and Support Vector Machine (SVM) - were used to analyze spectroscopic data. PCA analysis was applied prior to classification methods to reduce multidimensionality of the data. Classification error rates were used to evaluate the performance of these methods in the classification of tea samples. The results indicate that black, green, white, yellow, dark, and oolong teas, which are produced by different methods, are characterized by different UV-Vis, fluorescence, and NIR spectra. The lowest error rates in the calibration and validation data sets for individual spectroscopies and data fusion models were obtained with the use of the QDA and SVM methods, and did not exceed 3.3% and 0.0%, respectively. The lowest classification error rates in the validation data sets for individual spectroscopies were obtained with the use of RDA (12,8%), SVM (6,7%), and QDA (2,7%), for the UV-Vis, SF, and NIR spectroscopies, respectively. NIR spectroscopy combined with QDA outperformed other individual spectroscopic methods. Very low classification errors in the validation data sets - below 3% - were obtained for all the data fusion data sets (SFâ¯+â¯UV-Vis, SFâ¯+â¯NIR, NIRâ¯+â¯UV-Vis combined with the SVM method). The results show that UV-Vis, fluorescence and near infrared spectroscopies may complement each other, giving lower errors for the classification of tea types.