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高选择性高效液相色谱-电化学检测法测定丹参中5种酚类物质
引用本文:龙珍,GAMACHE Paul,郭志谋,潘媛媛,张艳海,刘晓达,金燕,刘绿叶,梁立娜,李仁勇.高选择性高效液相色谱-电化学检测法测定丹参中5种酚类物质[J].色谱,2017,35(8):897-905.
作者姓名:龙珍  GAMACHE Paul  郭志谋  潘媛媛  张艳海  刘晓达  金燕  刘绿叶  梁立娜  李仁勇
作者单位:1. 赛默飞世尔科技(中国)有限公司, 北京 100080; 2. Thermo Fisher Scientific Corporation, Massachusetts Chelmsford 01824; 3. 中国科学院分离分析化学重点实验室, 大连化学物理研究所, 辽宁 大连 116023
摘    要:发展了一种高灵敏度的高效液相色谱-电化学检测(HPLC-ECD)方法,用于丹参中5种酚类物质的定量分析。为了获得较高的检测灵敏度,对流动相的pH、缓冲溶液类型和浓度、有机相种类和梯度以及流速做了系统研究。在较低的pH(2.8)、较低的缓冲盐浓度(20 mmol/L NaH2PO4)和较缓的乙腈梯度下,以0.2 mL/min流速可为5种酚类的分离检测提供较好的分离度和较高的检测灵敏度。在获得优化的分离参数后,将其用于14批丹参药材中5种酚类物质的定量分析。结果表明,该方法可获得较好的回收率(>95%)、较宽的线性范围(高达4个数量级)、较好的重复性(RSD<4.01%)和较高的灵敏度(咖啡酸的LOQ低至1.5μg/L)。与紫外检测方法相比,ECD检测方法具有更高的选择性,可减少非抗氧化活性的物质的干扰。

关 键 词:高效液相色谱-电化学检测  梯度洗脱  酚类化合物  抗氧化剂  植物药
收稿时间:2017-03-29

A highly sensitive high performance liquid chromatography-electrochemical detection method for the determination of five phenolic compounds from Salvia miltiorrhiza
LONG Zhen,GAMACHE Paul,GUO Zhimou,PAN Yuanyuan,ZHANG Yanhai,LIU Xiaoda,JIN Yan,LIU L&#,ye,LIANG Lina,LI Renyong.A highly sensitive high performance liquid chromatography-electrochemical detection method for the determination of five phenolic compounds from Salvia miltiorrhiza[J].Chinese Journal of Chromatography,2017,35(8):897-905.
Authors:LONG Zhen  GAMACHE Paul  GUO Zhimou  PAN Yuanyuan  ZHANG Yanhai  LIU Xiaoda  JIN Yan  LIU L&#  ye  LIANG Lina  LI Renyong
Institution:1. Thermo Fisher Scientific Corporation, Beijing 100080, China; 2. Thermo Fisher Scientific Corporation, Chelmsford 01824, USA; 3. Key Lab of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China
Abstract:The determination of antioxidants continues to be interested, since the oxidative damage is thought to be one of the main mechanisms involved in nearly all chronic renal pathologies. A highly sensitive high performance liquid chromatography-electrochemical detection (HPLC-ECD) method was developed for evaluating the antioxidant properties of Salvia miltiorrhiza (Dan Shen). The method was optimized with respect to selectivity and sensitivity. Chromatographic conditions, including mobile phase pH value, buffer concentration, buffer type, organic solvent type, gradient profile and flow rate, were systematically investigated. Low pH value (2.8), low buffer concentration (20 mmol/L NaH2PO4), a shallow water-acetonitrile gradient, and a flow rate of 0.2 mL/min were the determined optimal conditions for the quantitative analysis of aimed five antioxidants from 14 batches of Dan Shen samples. The described method provided a good recovery (>95%), a very wide linear range (up to 104 for all analytes), a good precision (RSDs<4.01%), and a high sensitivity (LOQ of caffeic acid, 1.5 μ g/L). Compared with UV detection, the described ECD method was also more effective for evaluating the antioxidant properties of Dan Shen, as it provided highly selective detection of electro-active antioxidants
Keywords:high performance liquid chromatography-electrochemical detection (HPLC-ECD)  gradient elution  phenolic compound  antioxidant  herbal medicine (HM)
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