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MOLECULES · 2018 ·Vol. 23 ·期 7 ·1804 · IF 3.098

Effects of In Vitro Digestion on the Content and Biological Activity of Polyphenols from Acacia mearnsii Bark

Xiao Chen,Jia Xiong,Lingxiao He,Yu Zhang,Xun Li,Liping Zhang,Fei Wang

The stability and bioaccessibility of polyphenol fromAcacia mearnsiibark were measured at various stages during in vitro simulated digestion. Subsequently, the changes in the total polyphenol content (TPC) and biological activity were studied. The results showed that the phenolic compounds fromA. mearnsiiremained stable, and TPC underwent few changes during gastric digestion. Nonetheless, intestinal digestion led to the degradation of proanthocyanidins (PAs) and a significant decrease in TPC (26%). Degradation was determined by normal-phase HPLC and gel permeation chromatography. Only monomers, dimers, and trimers of flavan-3-ols were identified in the serum-accessible fraction for characterization of their bioaccessibility. The results also indicated the obvious antioxidant capacity of PAs fromA. mearnsiibark, and ~53% of the α-glucosidase–inhibitory effect was preserved. All these findings show that PAs fromA. mearnsiibark as a native plant source may be particularly beneficial for human health as a natural nutritional supplement.Keywords:Acacia mearnsii;proanthocyanidins;in vitro digestion;antioxidant;antidiabetic;HPLC/MS

研究领域: 食品科学 · 营养学 · 药理学
✓ 已验证 DOI PubMed 高影响因子
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Chinese Herbal Medicines · 2014 · IF 0

Rapid Analysis of Polar Components in Ophiocordyceps sinensis by Conventional Liquid Chromatography System

Wen-qing Li,Wen-jia Li,Zheng-ming Qian,Shi-lin Chen,Li Xiang

Objective To develop a rapid high-performance liquid chromatography coupled with diode array detection (HPLC-DAD) method for the simultaneous determination of six polar compounds in Ophiocordyceps sinensis. Methods A poroshell SB Aq column (50 mm × 4.6 mm, 2.7 μm) and gradient elution were used; The detection wavelength of compounds was set at 260 nm. The chromatographic peaks of the six investigated compounds in sample were identified by comparing their retention times with reference compounds. Results All calibration curves showed good linearity ( r > 0.999) within the tested ranges. The intra- and inter-day precisions of the six analytes were less than 0.8% and 2.1%, respectively, and the recoveries of the six analytes were between 95% and 103%. The validated method was successfully applied to the determination of six polar compounds in O. sinensis samples. Conclusion The poroshell SB Aq column is suitable for the rapid analysis of polar components in Chinese materia medica on conventional HPLC system and the developed HPLC method is also helpful to the quality control of O. sinensis .

CAS / MDL: 64-18-6
研究领域: 中药学 · 分析化学
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FOOD CHEMISTRY · 2016 · IF 4.052

Preparative separation of grape skin polyphenols by high-speed counter-current chromatography

Lanxin Luo,Yan Cui,Shuting Zhang,Lingxi Li,Yuanyuan Li,Peiyu Zhou,Baoshan Sun

To develop an efficient method for large preparation of various individual polyphenols from white grape skins (Fernão Pires; Vitis vinifera ) by preparative high-speed counter-current chromatography (HSCCC) and preparative-HPLC, an optimized preparative HSCCC condition with two-phase solvent system composed of Hex-EtOAc-H 2 O (1:50:50, v/v) was used to separate grape skin polyphenols into various fractions. Both the tail-head and head-tail elution modes were used with a flow rate of 3.0   ml/min and a rotary speed of 950   rpm. Afterwards, a preparative-HPLC separation was applied to isolate individual polyphenols in each of the fractions from HSCCC. Total of 7 fractions (Fraction A to G) were obtained from grape skin extract by HSCCC. After preparative-HPLC isolation, fifteen individual compounds were obtained, most of which presented high yields and purity (all over 90%). The HSCCC method followed with preparative-HPLC appeared to be convenient and economical, constituting an efficient strategy for the isolation of grape skin polyphenols.

CAS / MDL: 108-73-6
研究领域: 食品科学 · 植物化学 · 分析化学
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MOLECULES · 2018 ·Vol. 23 ·期 11 ·2891 · IF 3.098

Analytical Profiling of Proanthocyanidins from Acacia mearnsii Bark and In Vitro Assessment of Antioxidant and Antidiabetic Potential

Xiao Chen,Jia Xiong,Shenlin Huang,Xun Li,Yu Zhang,Liping Zhang,Fei Wang

The proanthocyanidins from ethanol extracts (80%,v/v) ofAcacia mearnsii(A. mearnsii) bark on chemical-based and cellular antioxidant activity assays as well as carbolytic enzyme inhibitory activities were studied. About 77% of oligomeric proanthocyanidins in ethanol extracts ofA. mearnsiibark were found by using normal-phase HPLC. In addition, HPLC-ESI-TOF/MS and MALDI-TOF/TOF MS analyses indicated that proanthocyanidins fromA. mearnsiibark exhibited with a degree of polymerization ranging from 1 to 11. These results of combined antioxidant activity assays, as well as carbolytic enzyme inhibitory activities of proanthocyanidins fromA. mearnsiibark, indicated an encouraging antioxidant capacity for the high polyphenol content and a potential for use as alternative drugs for lowering the glycemic response.Keywords:proanthocyanidins;HPLC/MS;MALDI-TOF/MS;antidiabetic;antioxidant;degree of polymerization

CAS / MDL: 76-05-1 53188-07-1
研究领域: 药理学 · 生物化学 · 分析化学
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Food Analytical Methods · 2019 ·Vol. 12 ·期 12 ·2777-2784 · IF 2.413

Liquid–Liquid Microextraction Based on Acid–Base-Induced Deep Eutectic Solvents for Determination of β-Carotene and Lycopene in Fruit Juices

Li Hong,Zhao Chunxi,Tian Hao,Yang Yaling,Li Wanyi

An uncomplicated, valid, and convenient way for detection of lycopene and β-carotene in fruit juice samples using acid–base-induced deep eutectic solvent (DES) liquid-liquid microextraction (DES-ABLLME) prior to HPLC was developed. The ternary fatty acid DESs were prepared by C 9 :C 10 :C 11 (2:1:1), which serve as hydrogen bond donors and hydrogen bond acceptors synchronously. In extraction procedure, NH 3 ·H 2 O was used as the emulsifier and reacted with DESs with a milk solution, which can significantly increase the extraction efficiency. HCl was used as the de-emulsifier, which could break the state of emulsification. At optimum conditions, the calibration graphs were linear in the concentration range from 0.1 to 100 μg mL −1 for lycopene and from 0.025 to 5.00 μg mL −1 for β-carotene. The limits of detection (LODs) were 0.05 and 0.002 μg mL −1 for lycopene and β-carotene, respectively. The RSD values were varied from 1.3 to 4.1%. Finally, the proposed method was applied to analyze β-carotene and lycopene in fruit juices.

研究领域: 食品科学 · 分析化学
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JOURNAL OF CHROMATOGRAPHY A · 2015 · IF 4.169

Comparison of antioxidant activities of different parts from snow chrysanthemum (Coreopsis tinctoria Nutt.) and identification of their natural antioxidants using high performance liquid chromatography coupled with diode array detection and mass spectrometry and 2,2′-azinobis(3-ethylbenzthiazoline-sulfonic acid)diammonium salt-based assay

L.X. Chen,D.J. Hu,S.C. Lam,L. Ge,D. Wu,J. Zhao,Z.R. Long,W.J. Yang,B. Fan,S.P. Li

Snow chrysanthemum ( Coreopsis tinctoria Nutt.), a world-widely well-known flower tea material, has attracted more and more attention because of its beneficial health effects such as antioxidant activity and special flavor. In this study, a high performance liquid chromatography coupled with diode array detection and mass spectrometry (HPLC-DAD-MS) and 2,2′-azinobis(3-ethylbenzthiazoline-sulfonic acid)diammonium salt (ABTS) based assay was employed for comparison and identification of antioxidants in different samples of snow chrysanthemum. The results showed that snow chrysanthemum flowers possessed the highest while stems presented the lowest antioxidant capacities. Fourteen detected peaks with antioxidant activity were temporarily identified as 3,4′,5,6,7-pentahydroxyflavanone-O-hexoside, chlorogenic acid, 2R-3′,4′,8-trihydroxyflavanone-7-O-glucoside, flavanomarein, flavanocorepsin, flavanokanin, quercetagitin-7-O-glucoside, 3′,5,5′,7-tetrahydroxyflavanone-O-hexoside, marein, maritimein, 1,3-dicaffeoylquinic acid, coreopsin, okanin and acetyl-marein by comparing their UV spectra, retention times and MS data with standards or literature data. Antioxidants existed in snow chrysanthemum are quite different from those reported in Chrysanthemum morifolium , a well-known traditional beverage in China, which indicated that snow chrysanthemum may be a promising herbal tea material with obvious antioxidant activity.

研究领域: 植物化学 · 食品科学 · 药用植物研究
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JOURNAL OF CHROMATOGRAPHY A · 2020 · IF 4.049

Simultaneous determination of free and total paclitaxel in blood in a three-phase laminar flow microchip

Qidan Cai,Huaidong Peng,Jiang Meng,Youshao Yan,Yu Zeng,Paul C.H. Li,Yue Sun

In this study, a three-phase laminar flow microfluidic chip (TPL chip) combined with HPLC was developed for monitoring free and total concentrations of paclitaxel (PTX) in blood simultaneously. A diluted whole blood sample (aqueous phase) was introduced into the chip, ethyl acetate (organic phase) was introduced into the chip for extraction, and an interphase was used to prevent the blood sample from coming into direct contact with the organic phase. Because only free drug can quantitatively diffuse into the organic extraction phase and the free drug fraction has a linear relationship with the dilution factor of blood, both the free and total drug concentrations can be obtained by detecting the concentration of paclitaxel in the organic extraction phase. The governing factor such as flow rate for extraction was optimized. Docetaxel was used as an internal standard. The reliability of the quantitative diffusion of molecules in the TPL chip was proved by the methodological investigation of PTX in PBS sample, which showed a good linearity in the concentration range of 0.5 - 100 µg/mL and a detection limit of 7 ng/mL. Good repeatibilities for retention time (RSD of PTX is 1.23%, docetaxel is 1.14%, n  = 5) and peak area ratio of PTX to docetaxel (RSD is 4.38%) were obtained. For blood sample analysis, only 100 µL of sample was needed and whole pretreatment was finished in 35 min, and a recovery of 94~117% were obtained. The provided method showed advantages in fast analysis speed, minimum sample handing, and potential ability of automation, and integration.

研究领域: 分析化学 · 药代动力学 · 生物医学工程
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Talanta Open · 2025 · IF 3.7

Quantification of oleanolic acid and apigenin in biological matrices following intraperitoneal administration of co-loaded nanoformulations: Method validation and biodistribution studies

Amna Naz,Sadia Haider,Mavra Rana,Neelum Malik,Attia Afzal,Muhammad Farooq,Muhammad Sarfraz

Oleanolic acid (OA) and apigenin (APG) demonstrate a wide range of pharmacological effects, including antioxidant, anti-inflammatory, antiviral, antidiabetic, hepatoprotective, and cardioprotective activities. Both compounds show anticancer potential and have been used individually to treat various cancer types, creating a rationale for their combined use. However, quantifying both drugs in quality and plasma samples presents challenges due to differences in their physicochemical properties and absorption wavelengths (OA: 210-215 nm, APG: 212, 269, and 337 nm). We developed and validated a novel High-Performance Liquid Chromatography UV detection (HPLC-UV) method to address this problem. Using a C18 column (4.6 mm x 250 mm, packing L1, 5 µm particle size) and a mobile phase of acetonitrile: methanol: tetrahydrofuran: water (60:20:8:12, v/v) with a detection wavelength of 215 nm. The method achieved retention times of 4.7 and 10 minutes for OA and APG in quality samples, and 4.9 and 9.8 minutes in plasma samples, respectively. The plasma sample was prepared by simple protein precipitation step. All validation parameters, including sensitivity, selectivity, precision, accuracy, robustness, and stability, met the required criteria. The validated HPLC-UV bioanalytical method was effectively applied in quantification, stability, and pharmacokinetic studies of co-loaded nanoformulations of OA and APG with particle size 163 nm and entrapment efficiency up to 93 %, establishing it as a promising analytical technique for detecting these anticancer agents in complex matrices such as blood, plasma, and polymeric systems.

CAS / MDL: 520-36-5
研究领域: 药理学 · 分析化学 · 肿瘤学
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FOOD RESEARCH INTERNATIONAL · 2017 · IF 3.086

Profiling and quantification of phenolic compounds in Camellia seed oils: Natural tea polyphenols in vegetable oil

Xiaoqin Wang,Qiumei Zeng,María del Mar Contreras,Lijuan Wang

In Asia, tea seed oils (seed oils from Camellia oleifera , C. chekiangoleosa , and C. sinensis ) are used in edible, medicinal, and cosmetic applications. However, these oils differ in their fatty acid contents, and there is little known about their phenolic compounds . Here we analyzed the phenolic compounds of seed oils from three species gathered from 15 regions of China. Twenty-four phenolic compounds were characterized by HPLC-Q-TOF-MS, including benzoic acids (6), cinnamic acids (6), a hydroxyphenylacetic acid, flavanols (4), flavonols (3), flavones (2), and dihydroflavonoids (2). Some of these phenolic compounds had not previously been reported from C. sinensis (20), C. oleifera (15), and C. chekiangoleosa (24) seed oils. Quantification was done by HPLC-QqQ-MS using 24 chemical standards. The total concentrations in the studied samples ranged from 20.56 to 88.56   μg/g. Phenolic acids were the most abundant class, accounting for 76.2–90.4%, with benzoic acid, found at up to 18.87   μg/g. The concentration of catechins, typical of tea polyphenols, ranged between 2.1% and 9.7%, while the other flavonoids varied from 4.2% to 17.8%. Although the cultivation region affected the phenolic composition of the Camellia seed oils, in our hierarchical clustering analysis, the samples clustered according to species. The phenolic composition of the seed oils from C. oleifera and C. chekiangoelosa were similar. We found that the phenolic categories in Camellia seed oils were similar to tea polyphenols, thereby identifying a source of liposoluble tea polyphenols and potentially accounting for some of the reported activities of these oils. In addition, this work provides basic data that allows distinction of various Camellia seed oils, as well as improvements to be made in their quality standards.

研究领域: 植物化学 · 食品科学 · 分析化学
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JOURNAL OF AOAC INTERNATIONAL · 2019 ·Vol. 100 ·期 4 ·1029-1037 · IF 1.201

Identification, Characterization, and Quantification of Impurities of Safinamide Mesilate: Process-Related Impurities and Degradation Products

Zou Liang,Sun Lili,Zhang Hui,Hui Wenkai,Zou Qiaogen,Zhu Zheying

The characterization of process-related impurities and degradation products of safinamide mesilate (SAFM) in bulk drug and a stability-indicating HPLC method for the separation and quantification of all the impurities were investigated. Four process-related impurities (Imp-B, Imp-C, Imp-D, and Imp-E) were found in the SAFM bulk drug. Five degradation products (Imp-A, Imp-C, Imp-D, Imp-E, and Imp-F) were observed in SAFM under oxidative conditions. Imp-C, Imp-D, and Imp-E were also degradation products and process-related impurities. Remarkably, one new compound, identified as (S)-2-[4-(3-fluoro-benzyloxy) benzamido] propanamide (i.e., Imp-D), is being reported here as an impurity for the first time. Furthermore, the structures of the aforementioned impurities were characterized and confirmed via IR, NMR, and MS techniques, and the most probable formation mechanisms of all impurities proposed according to the synthesis route. Optimum separation was achieved on an Inertsil ODS-3 column (250 × 4.6 mm, 5 μm), using 0.1% formic acid in water (pH adjusted to 5.0) and acetonitrile as the mobile phase in gradient mode. The proposed method was found to be stability-indicating, precise, linear, accurate, sensitive, and robust for the quantitation of SAFM and its process-related substances, including its degradation products.

CAS / MDL: 1336-21-6 64-18-6
研究领域: 药物化学 · 分析化学
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Analytical Methods · 2015 ·Vol. 7 ·期 14 ·5973-5980 · IF 1.821

Identification of dried shark fins by analysis of seven sugars using pre-column derivatization high-performance liquid chromatography and stable carbon isotope ratio analysis

Yanping Xian,Hao Dong,Haiying Luo,Donghui Luo,Yuluan Wu,Mouming Zhao,Xindong Guo

A simple and sensitive method using pre-column high-performance liquid chromatography (HPLC) was developed for the simultaneous detection of seven sugars, which was also applied for the preliminary identification of dried shark fins. δ13C values of the dried shark fin samples also were determined by element analyser-isotope ratio mass spectrometry (EA-IRMS). The dried shark fins were decomposed by enzymolysis using a papaya protease and an amylase enzyme; then, samples were analysed by HPLC after the derivatization of the enzymatic hydrolysate, using 1-phenyl-3-methyl-5-pyrazolone (PMP) as the derivatizing agent. The results indicated that the seven sugars were well separated by this method. Of the conditions tested, application of a derivatization time of 75 minutes and of a phosphate buffer–acetonitrile (80 : 20, v/v) mobile phase system (pH = 6.8) yielded the best detection results and separation effects of the seven standard substances. Note that the areas under the peaks of two kinds of uronic acid derivative products decreased significantly (P < 0.01) with time, so it is necessary to perform the HPLC analysis within 24 h after the derivatization reaction. The developed method is suitable for the identification and analysis of artificial dried shark fins with good accuracy, reproducibility and sensitivity. In addition, δ13C values were highly significant (P < 0.01) for real and fake dried shark fins. Thus, the combination of these methods could potentially be useful for identification of dried shark fins regardless of whether they are fake or artificial.

研究领域: 海洋生物学 · 分析化学 · 食品科学
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CARBOHYDRATE POLYMERS · 2015 · IF 4.074

Monosaccharide compositions of sulfated chitosans obtained by analysis of nitrous acid degraded and pyrazolone-labeled products

Zhangrun Han,Yangyang Zeng,Meng Zhang,Yiran Zhang,Lijuan Zhang

Chemically sulfated chitosans are important biomaterials. However, a reliable analytical method for quality control over such compounds is still lacking. In this study, we prepared four different kinds of selectively sulfated chitosans and developed a novel method to analyze their monosaccharide compositions by HPLC. In this method, nitrous acid was used to generate 2, 5-hydro mannose (M), 3-O-sulfated M (M3), 6-O-sulfated M (M6), and 3, 6-O-disulfated M (M9) from the sulfated chitosans. PMP, that is 1-phenyl-3-methyl-5-pyrazolone with a UV absorbance at 245   nm, was used to label all the Ms quantitatively. The monosaccharide compositions for each sulfated chitosan were obtained by C18 HPLC separation and online UV detection of all PMP-labeled Ms. The identities of all Ms were confirmed by MS analysis with the help of standard Ms generated from a heparin pentasaccharide and chitosan. The overall results indicated that the newly developed method had advantages over 13 C NMR in defining the monosaccharide compositions of sulfated chitosans and was useful for quality control purpose.

研究领域: 生物化学 · 分析化学
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