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

doi:10.3724/SP.J.1123.2017.03038

色谱 ›› 2017, Vol. 35 ›› Issue (8): 897-905.DOI: 10.3724/SP.J.1123.2017.03038

• 技术与应用 • 上一篇

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

龙珍¹, GAMACHE Paul², 郭志谋³, 潘媛媛¹, 张艳海¹, 刘晓达¹, 金燕¹, 刘绿叶¹, 梁立娜¹, 李仁勇¹

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

收稿日期:2017-03-29 出版日期:2017-08-08 发布日期:2013-11-25
通讯作者: 郭志谋,Tel:+86-411-84379541,E-mail:guozhimou@dicp.ac.cn;金燕,Tel:+86-21-68654588,E-mail:yan.jin@thermofisher.com

A highly sensitive high performance liquid chromatography-electrochemical detection method for the determination of five phenolic compounds from Salvia miltiorrhiza

LONG Zhen¹, GAMACHE Paul², GUO Zhimou³, PAN Yuanyuan¹, ZHANG Yanhai¹, LIU Xiaoda¹, JIN Yan¹, LIU Lüye¹, LIANG Lina¹, LI Renyong¹

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

Received:2017-03-29 Online:2017-08-08 Published:2013-11-25

摘要/Abstract

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: 酚类化合物, 高效液相色谱-电化学检测, 抗氧化剂, 梯度洗脱, 植物药

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

Key words: antioxidant, gradient elution, herbal medicine (HM), high performance liquid chromatography-electrochemical detection (HPLC-ECD), phenolic compound

中图分类号:

O658

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.

LONG Zhen, GAMACHE Paul, GUO Zhimou, PAN Yuanyuan, ZHANG Yanhai, LIU Xiaoda, JIN Yan, LIU Lüye, 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.

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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

A highly sensitive high performance liquid chromatography-electrochemical detection method for the determination of five phenolic compounds from Salvia miltiorrhiza

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