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超高效液相色谱-电喷雾串联质谱法测定雷公藤药材中5种有效成分

[Determination of five effective components in medicinal material of Tripterygium by UPLC-ESI-MS/MS].

作者信息

Hu Jun, Liu Chao, Guo Lan-Ping, Hao Qing-Xiu, Kang Li-Ping, Nan Tie-Gui, Liu Yong, Zhan Zhi-Lai, Huang Lu-Qi

机构信息

State Key Laboratory of Dao-di Herbs Breeding Base, National Resource Center for Chinese Materia Medica, China Academy of Chinese Medical Sciences, Beijing 100700, China.

School of Chinese Materia Medica, Beijing University of Chinese Medicine, Beijing 100102, China.

出版信息

Zhongguo Zhong Yao Za Zhi. 2016 Apr;41(8):1469-1473. doi: 10.4268/cjcmm20160817.

Abstract

This paper is aimed to develop a method for the determination of five effective components in medicinal material of Tripterygium using ultra performance liquid chromalography coupled with electrospray ionization tandem mass spectrometry(UPLC-ESI-MS/MS), which then was used to study their contents in raw materials from different areas and different sources.The separation was performed on a Waters ACQUITY UPLC-CSH-C18S column(2.1 mm×100 mm,1.7 μm), usingacetonitrile-0.2% ammonium form ateaqueous solutionas mobile phase. The target components were detected in multiple-reaction monitoring(MRM) mode by mass spectrometry with electrospray ionization (ESI) source operated in positive ionization mode. The quantitative results showed that good linearity was achieved in their respective linear ranges and fine determination coefficient (r > 0.997 8),and the overall recoveries ranged from 96.72%-103.2% with the RSD ranging from 1.0%-2.4%.The method is sensitive and accurate, and suitable for the effective components quantification in medicinal material of Tripterygium; contents of five effective components from different sources vary significantly, so the quality and safety of medicinal material of Tripterygium needs to be improved. It is very important to control the quality with multi-index for clinic safety.

摘要

本文旨在建立一种采用超高效液相色谱-电喷雾电离串联质谱法(UPLC-ESI-MS/MS)测定雷公藤药材中5种有效成分的方法,并用于研究不同产地、不同来源的雷公藤药材中这些成分的含量。采用Waters ACQUITY UPLC-CSH-C18S柱(2.1 mm×100 mm,1.7 μm)进行分离,以乙腈-0.2%甲酸铵水溶液为流动相。采用电喷雾电离(ESI)源,在正离子模式下,通过质谱多反应监测(MRM)模式检测目标成分。定量结果表明,各成分在其各自线性范围内线性关系良好,测定系数优良(r>0.997 8),加样回收率为96.72%~103.2%,相对标准偏差(RSD)为1.0%~2.4%。该方法灵敏、准确,适用于雷公藤药材有效成分的定量测定;不同来源的5种有效成分含量差异显著,雷公藤药材质量和安全性有待提高。多指标控制质量对临床用药安全至关重要。

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