HPLC-ESI-MS

HPLC - ESI - MS
  • 文章类型: Journal Article
    本研究使用Caco-2细胞模型和超高效液相色谱-电喷雾电离-串联质谱法(UPLC-ESI-MS),研究了raphani对人参C.A.Meyer(人参)中人参皂苷吸收的影响。六种主要人参皂苷(Rg1,Re,Rb1,Rb2,Rc,Rd)进行了量化。结果表明,莱佛尼提高了人参皂苷的外排率,特别是在较高的浓度下,表明它抑制了它们的吸收。该研究阐明了人参皂苷的肠道吸收过程以及莱佛子对人参的拮抗机制。
    This study examined the impact of Semen raphani on the absorption of ginsenosides from Panax ginseng C.A. Meyer (ginseng) using a Caco-2 cell model and Ultra-High-Performance Liquid Chromatography-Electrospray Ionization-Tandem Mass Spectrometry (UPLC-ESI-MS). Six primary ginsenosides (Rg1, Re, Rb1, Rb2, Rc, Rd) were quantified. Results showed that Semen Raphani increased the efflux rate of ginsenosides, particularly at higher concentrations, suggesting it inhibits their absorption. The research elucidates the intestinal absorption process of ginsenosides and the antagonistic mechanism of Semen Raphani against ginseng.
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  • 文章类型: Journal Article
    红薯富含具有潜在抗血小板聚集活性的心脏保护植物化学物质,尽管这种益处可能因品种/基因型而异。酚醛谱[HPLC-ESI(-)-qTOF-MS2],化学信息学(ADMET特性,对血小板蛋白的亲和力)和从橙色(OSP)和紫色(PSP)甘薯贮藏根中获得的富含酚类的水醇提取物的抗PA活性,进行了评估。酚类丰富度[羟基肉桂酸>类黄酮>苯甲酸]为PSP>OSP。它们的主要绿原酸可以与血小板蛋白(整合素/粘附素,激酶/金属酶),但它们的生物利用度可能很差。仅OSP表现出剂量依赖性抗血小板聚集活性[诱导剂(IC50,mg。ml-1):凝血酶受体激活剂肽-6(0.55)>腺苷-5'-二磷酸(1.02)>胶原蛋白(1.56)]和减少的P-选择素表达(0.75-1.0mg。ml-1),但不分泌糖蛋白IIb/IIIa。OSP/PSP的已探索的抗PA活性似乎与其酚类丰富度成反比。其绿原酸的较差的首过生物利用度(在计算机中记录)可能是其体内抗PA的进一步障碍。
    Sweet potatoes are rich in cardioprotective phytochemicals with potential anti-platelet aggregation activity, although this benefit may vary among cultivars/genotypes. The phenolic profile [HPLC-ESI(-)-qTOF-MS2], cheminformatics (ADMET properties, affinity toward platelet proteins) and anti-PA activity of phenolic-rich hydroalcoholic extracts obtained from orange (OSP) and purple (PSP) sweet potato storage roots, was evaluated. The phenolic richness [Hydroxycinnamic acids> flavonoids> benzoic acids] was PSP > OSP. Their main chlorogenic acids could interact with platelet proteins (integrins/adhesins, kinases/metalloenzymes) but their bioavailability could be poor. Just OSP exhibited a dose-dependent anti-platelet aggregation activity [inductor (IC50, mg.ml-1): thrombin receptor activator peptide-6 (0.55) > Adenosine-5\'-diphosphate (1.02) > collagen (1.56)] and reduced P-selectin expression (0.75-1.0 mg.ml-1) but not glycoprotein IIb/IIIa secretion. The explored anti-PA activity of OSP/PSP seems to be inversely related to their phenolic richness. The poor first-pass bioavailability of its chlorogenic acids (documented in silico) may represent a further obstacle for their anti-PA in vivo.
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  • 文章类型: Journal Article
    背景:三种不同的有机葵花籽饼,由不同壳含量的种子产生,通过两种不同的提取方法提取,常规提取(CE)和超声辅助提取(UAE)。通过Folin-Ciocalteu试剂(FCR)和高效液相色谱(HPLC)方法评估提取物中的总酚类化合物(TPC)含量。此外,通过TEAC和DPPH测定评价提取物的抗氧化能力。
    结果:我们的结果表明,两种提取物均显示出高TPCs和抗氧化能力。与CE相比,UAE方法显示出明显更高的TPC和抗氧化能力值。单个酚类化合物,如绿原酸(CGA)异构体(3-,4-和5-O-咖啡酰基奎尼酸),二-CGA异构体,以及阿魏酸和香豆酰基奎尼酸根据其精确质量通过HPLC结合飞行时间质谱进行鉴定。
    结论:目前的结果表明,UAE方法可以有效地促进向日葵籽饼中酚类化合物的提取。本文受版权保护。保留所有权利。
    BACKGROUND: Three different organic sunflower seed cakes, produced from seeds differing in the content of their hulls, were extracted by two different extraction methods - conventional extraction (CE) and ultrasound-assisted extraction (UAE). The total phenolic compound (TPC) content of the extracts was evaluated using Folin-Ciocâlteu reagent (FCR) and high-performance liquid chromatography (HPLC). The antioxidant capacity of extracts was evaluated with the Trolox equivalent antioxidant capacity (TEAC) and 2,2-diphenyl-1-picrylhydrazyl (DPPH) assays.
    RESULTS: The results showed that both extracts displayed high TPC content and antioxidant capacity. The UAE method showed significantly higher TPC content and antioxidant capacity values than CE. Individual phenolic compounds such as chlorogenic acid (CGA) isomers (3-, 4- and 5-O-caffeoylquinic acids), di-CGA isomers, and feruloylquinic and coumaroylquinic acids were identified according to their exact masses by HPLC coupled to time-of-flight mass spectrometry.
    CONCLUSIONS: The results revealed that the UAE method could be used effectively to facilitate the extraction of phenolic compounds from sunflower seed cake. © 2023 The Authors. Journal of The Science of Food and Agriculture published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry.
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  • 文章类型: Journal Article
    已开发出一种简单而选择性的测定咖啡因(CAF)和茶碱(THEO)的方法,用于用包括碳点(CD)和壳聚糖(CS)的复合材料修饰的玻碳电极(GCE)。据我们所知,以前没有研究分析CD修饰的GCE是否存在CAF和THEO。通过循环伏安法(CV)和差分脉冲伏安法(DPV)研究了用CD-CS复合材料修饰的GCE在酸性介质中的电化学行为。考虑到传感器的分析参数,CAF和THEO的线性浓度范围为1×10-5至5×10-3molL-1,检测限(LOD)为1×10-6molL-1。再现性和重复性数据在RSD%方面令人满意。此外,评估了储存稳定性,无论使用何种实验条件,都能证明良好的结果。该传感器用于茶叶和药品中CAF和THEO的同时测定,并将结果与HPLC-ESI-MS在SIR模式下获得的结果进行比较,该方法是故意优化的独立方法。电化学传感器在廉价方面具有无与伦比的优势,便携性,和易用性,因为它不需要熟练的人员。
    A simple and selective method for the determination of caffeine (CAF) and theophylline (THEO) has been developed for a glassy carbon electrode (GCE) modified with a composite including carbon dots (CDs) and chitosan (CS). To our knowledge, there are no previous studies that analyze a CDs-modified GCE for the presence of CAF and THEO. The electrochemical behavior of a GCE modified with a CDs-CS composite was studied in acidic medium by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). Considering the sensor analytical parameters, the same linear concentrations range was found for CAF and THEO ranging from 1 × 10-5 to 5 × 10-3 mol L-1 with the same detection limit (LOD) of 1 × 10-6 mol L-1. The reproducibility and repeatability data were satisfactory in terms of RSD%. Moreover, the storage stability was evaluated, evidencing good results whatever the experimental conditions used. The developed sensor was applied for the simultaneous determination of CAF and THEO in tea and drug, and results were compared with those obtained with HPLC-ESI-MS in SIR mode as an independent method optimized on purpose. The electrochemical sensor presents the undoubled advantages in terms of cheapness, portability, and ease of use, since it does not require skilled personnel.
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  • 文章类型: Journal Article
    基于共振拉曼光谱和反射可见光谱的显微分析技术已用于表征导致花朵中蓝色或紫色着色的颜料;特别是Lobeliaerinus,Campanulaportenschlagiana,Cineraria,中提琴三色,海葵冠状病毒,Agapanthus,桔梗,丹参,白头翁,长毛,Commelinacommunis和Salviapatens。光谱学方法在体内应用于花瓣,并在体外应用于通过基于SPE(固相萃取)的程序获得的提取物,该程序针对最少量的植物原料进行了优化。拉曼光谱获得的不同模式已经相关,也在密度泛函理论(DFT)计算的基础上,花青素的苯并吡喃核具有不同的取代方案,并且具有各种可能的色素沉着形式,负责稳定蓝色。通过与HPLC-ESI-MS(液相色谱-电喷雾电离-质谱)的提取物分析进行比较来验证获得的结果。
    Microanalysis techniques based on resonance Raman and reflection visible spectroscopy have been applied to the characterization of pigments responsible for the blue or violet coloration in flowers; in particular of Lobelia erinus, Campanula portenschlagiana, Cineraria, Viola tricolor, Anemone coronaria, Agapanthus, Platycodon, Salvia farinacea, Plumbago capensis, Ceratostigma plumbaginoides, Commelina communis and Salvia patens. The spectroscopic methods were applied both in vivo on the flower petals and in vitro on extracts obtained through a procedure based on SPE (solid-phase extraction) optimized for minimal quantities of vegetable raw material. Different patterns obtained for the Raman spectra have been correlated, also on the basis of density functional theory (DFT) calculations, with different schemes of substitution of the benzopyrilium nucleus of the anthocyanins and with various possible forms of copigmentation responsible for the stabilization of the blue color. The results obtained were verified by comparison with the analysis of the extracts by HPLC-ESI-MS (liquid chromatography-electrospray ionization-mass spectrometry).
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  • 文章类型: Journal Article
    黄精物种自古以来就被用作亚洲和欧洲的传统药物和功能食品。在这项研究中,开发了一种基于液相色谱-电喷雾电离质谱(LC-ESI-MS)的快速简便方法,以系统分析和鉴定日本分布的四种主要黄精中的甾体苷,包括玉竹,P.falcatum,P.macranthum,还有P.sibiricum.因此,初步鉴定了31种甾体苷,包括18个已知的和13个以前未报告的糖苷。通过色谱行为和ESI-MS片段化模式的解释鉴定了它们的结构。31种甾体糖苷的鉴定表明黄精属物种中常见的生物遗传途径。我们的研究揭示了黄精植物中类固醇糖苷的化学概况,这将有利于更好的植物化学和植物化学的理解和质量控制为他们的药用。
    Polygonatum species have been used as traditional medicines and functional foods in Asia and Europe since ancient times. In this study, a fast and simple method based on liquid chromatography coupled with electrospray ionization mass spectrometry (LC-ESI-MS) was developed to systematically analyze and identify the steroidal glycosides in four major Polygonatum species distributed in Japan, including P. odoratum, P. falcatum, P. macranthum, and P. sibiricum. As a result, 31 steroidal glycosides were tentatively identified, including 18 known and 13 previously unreported glycosides. Their structures were identified by the interpretation of chromatographic behavior and ESI-MS fragmentation patterns. The identification of 31 steroidal glycosides was indicative of a common biogenetic pathway in Polygonatum species. Our study disclosed the chemical profiling of steroidal glycosides in the plants of Polygonatum species, which will benefit better phytochemotaxonomical and phytochemical understanding and quality control for their medicinal usage.
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  • 文章类型: Journal Article
    Meliponaquadrifascifiataanthidioides和Scaptotrigonadepilis是能够生产蜂胶的无刺蜜蜂,具有相当大的生物勘探潜力。在这种情况下,这项研究的目的是确定化学组成和评价蜂胶生产的抗微生物活性。制备了M.q.anthidioides(EEP-M)和S.depilis(EEP-S)蜂胶的乙醇提取物,用HPLC-ESI-MS对其化学成分进行了表征。对细菌和真菌的抗菌活性进行了评估,从对抗生素作用具有抗性的参考菌株和医院来源分离。从EEP-M,酚类化合物被注释,包括没食子酸,鞣花酸,和类黄酮,以及二萜和三萜。EEP-S在其化学组成中主要显示三萜。两种提取物都能抑制医学相关细菌和真菌的生长,包括医院获得的和抗微生物药物。总的来说,与EEP-M相比,EEP-S显示出更好的抗菌活性。EEP-S对耐万古霉素粪肠球菌的MIC为3.50mg/mL,EEP-M的MIC为5.33±0.16mg/mL。总之,这项研究表明,由M.q.anthioides和S.depilis生产的蜂胶具有预防或治疗微生物感染的潜力。
    Melipona quadrifasciata anthidioides and Scaptotrigona depilis are species of stingless bees capable of producing propolis, which has considerable bioprospecting potential. In this context, the objective of this study was to determine the chemical compositions and evaluate the antimicrobial activity of propolis produced by M. q. anthidioides and S. depilis. The ethanolic extracts of propolis of M. q. anthidioides (EEP-M) and S. depilis (EEP-S) were prepared, and their chemical constituents were characterized by HPLC-ESI-MS. The antimicrobial activity was evaluated against bacteria and fungi, isolated from reference strains and hospital origin resistant to the action of antibiotics. From EEP-M, phenolic compounds were annotated, including gallic acid, ellagic acid, and flavonoids, as well as diterpenes and triterpenes. EEP-S showed mainly triterpene in its chemical composition. Both extracts inhibited the growth of medically relevant bacteria and fungi, including hospital-acquired and antimicrobial-resistant. In general, EEP-S showed better antimicrobial activity compared to EEP-M. The MIC of EEP-S against vancomycin-resistant Enterococcus faecalis was 3.50 mg/mL, while the MIC of EEP-M was 5.33 ± 0.16 mg/mL. In conclusion, this study shows that propolis produced by M. q. anthidioides and S. depilis has the potential to be used for the prevention or treatment of microbial infections.
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  • 文章类型: Journal Article
    Recently, 1-DNJ has been widely studied by scientists for its capacity to inhibit α-glucosidase and reduce postprandial blood glucose and fat accumulation. To the best of our knowledge, this is the first analytical determination of 1-DNJ in Morus sp.pl. leaves carried out on Italian crops, and it could be used as a reference to assess the quality of the plant material in comparison to Far Eastern Asia cultivations. The effects of two thermal treatments were compared to test the incidence of the drying process on the 1-DNJ extractability. In addition, two harvesting seasons in the same year (2017) and two subsequent harvesting years (2017-2018) were considered. The amount of 1-DNJ herein found was comparable to that reported in the scientific literature for Asian cultivations. The increase in 1-DNJ along the summer and the higher level of this compound in the apical leaves also complies with previous findings. However, a strong implication for the climatic conditions in the different years and a significant interaction between climate and genotypes suggest exploring very carefully the agronomic practices and selecting cultivars according to different environmental conditions with a view to standardize the 1-DNJ amount in leaves.
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  • 文章类型: Journal Article
    李是欧洲生产中最重要的水果作物之一。在葡萄之后,苹果,橘子和西瓜。大多数品种富含次生代谢产物,显示对人体健康的抗氧化特性。这项研究的目的是开发一种化学分析方法,其中涉及使用不同的分析仪器技术,以加深与在地中海地区(意大利南部)种植的桃子和油桃的某些品种中存在的代谢物特征有关的知识。比较研究是通过选择黄肉桃来进行的(RomeStar,ZeeLady)和黄质油桃(Nectaross,金星)来自两个地理区域(PianadiSibari和PianadiMetaponto),并通过确定允许识别任何独特品种和/或地理特征的肉和皮肤的化学参数。采用了分析和化学计量学相结合的方法,槽流变,热重(TGA),色谱(HPLC-ESI-MS),光谱(UV-Vis,ATR-FTIR,NMR)和光谱(ToF-SIMS)分析。这种方法使我们能够确定用于分析植物基质的特征参数,以便开发的方法可以定义一个易于导出和可扩展的模型,用于表征其他类型的蔬菜基质。
    Prunus persica L. is one of the most important fruit crops in European production, after grapes, apples, oranges and watermelons. Most varieties are rich in secondary metabolites, showing antioxidant properties for human health. The purpose of this study was to develop a chemical analysis methodology, which involves the use of different analytical-instrumental techniques to deepen the knowledge related to the profile of metabolites present in selected cultivars of peaches and nectarines cultivated in the Mediterranean area (Southern Italy). The comparative study was conducted by choosing yellow-fleshed peaches (RomeStar, ZeeLady) and yellow-fleshed nectarines (Nectaross, Venus) from two geographical areas (Piana di Sibari and Piana di Metaponto), and by determining the chemical parameters for the flesh and skin that allow for identification of any distinctive varietal and/or geographical characteristics. A combined analytical and chemometric approach was used, trough rheological, thermogravimetric (TGA), chromatographic (HPLC-ESI-MS), spectroscopic (UV-Vis, ATR-FTIR, NMR) and spectrometric (ToF-SIMS) analysis. This approach allowed us to identify the characterizing parameters for the analysis of a plant matrix so that the developed methodology could define an easily exportable and extendable model for the characterization of other types of vegetable matrices.
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  • 文章类型: Journal Article
    这项工作的目的是确定沉积物中的黄腐酸(FA),以在分子水平上更好地了解其组成,并提出有机前体的子结构和结构。沉积物样本是从墨西哥保护生态系统和生物多样性的优先区域获得的。使用对国际腐殖质协会方法的修改来提取和纯化FAs。通过1D和2D核磁共振(NMR)和高效液相色谱-电喷雾电离质谱(HPLC-ESI-MS)在正(ESI)和负(ESI-)模式下进行表征。COSY和HSQC实验提出了12个子结构,与以前报道的可能属于从土壤中获得的木质素衍生物的化合物相关。通过HPLC-ESI-MS获得的光谱分析表明可能存在化学上与NMR阐明的子结构相似的化合物。研究的FAs主要由羧酸组成,羟基,酯类,乙烯基,脂肪族,取代的芳香环,和胺,呈现与有机前体相关的结构,如木质素衍生物和多糖。
    The aim of this work was to determine Fulvic Acids (FAs) in sediments to better know their composition at the molecular level and to propose substructures and structures of organic precursors. The sediment samples were obtained from a priority area for the conservation of ecosystems and biodiversity in Mexico. FAs were extracted and purified using modifications to the International Humic Substances Society method. The characterization was carried out by 1D and 2D nuclear magnetic resonance (NMR) and high-performance liquid chromatography-electrospray ionization-mass spectrometry (HPLC-ESI-MS) in positive (ESI+) and negative (ESI-) modes. Twelve substructures were proposed by the COSY and HSQC experiments, correlating with compounds likely belonging to lignin derivatives obtained from soils as previously reported. The analysis of spectra obtained by HPLC-ESI-MS indicated likely presence of compounds chemically similar to that of the substructures elucidated by NMR. FAs studied are mainly constituted by carboxylic acids, hydroxyl, esters, vinyls, aliphatics, substituted aromatic rings, and amines, presenting structures related to organic precursors, such as lignin derivatives and polysaccharides.
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