高效液相色谱-串联质谱法同时测定保健品及中成药中非法添加的17种壮阳类化学药

引用本文: 黄芳, 吴惠勤, 黄晓兰, 罗辉泰, 朱志鑫, 林晓珊, 马立果, 蒋娅兰. 高效液相色谱-串联质谱法同时测定保健品及中成药中非法添加的17种壮阳类化学药[J]. 色谱, 2016, 34(3): 270-278. doi: 10.3724/SP.J.1123.2015.11016 shu

Citation: HUANG Fang, WU Huiqin, HUANG Xiaolan, LUO Huitai, ZHU Zhixin, LIN Xiaoshan, MA Liguo, JIANG Yalan. Simultaneous determination of 17 aphrodisiac chemical drugs illegally added in health products and Chinese patent medicines by high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2016, 34(3): 270-278. doi: 10.3724/SP.J.1123.2015.11016 shu

高效液相色谱-串联质谱法同时测定保健品及中成药中非法添加的17种壮阳类化学药

1.
1. 中国广州分析测试中心, 广东省分析测试技术公共实验室, 广东广州 510070;
2.
2. 广东药学院中药学院, 广东广州 510006;
3.
3. 广东药学院公共卫生学院, 广东广州 510024
基金项目:
广东省促进科技服务业发展计划项目(2012B040302007). (2012B040302007)

摘要: 建立了高效液相色谱-串联质谱(LC-MS/MS)同时测定补肾壮阳类保健品及中成药中非法添加的17种壮阳化学药的定性、定量分析方法。实验优化了前处理方法,并针对几对同分异构体成分优化了分离条件和质谱参数。样品经甲醇超声萃取,提取液经Aglient Extend C18色谱柱(100 mm×2.1 mm, 3.5 μm)分离,流动相为乙腈和水(含有10 mmol/L乙酸铵),梯度洗脱,流速为0.25 mL/min,以电喷雾离子源正离子多反应监测(MRM)模式进行MS/MS检测。该方法能很好地分离并定量17种壮阳类化学药以及其中的3组同分异构体。该方法简便、快速、准确可靠,已经应用于补肾壮阳类保健品及中成药中非法添加壮阳类化学药的筛查及检测。统计近3年检测的样品,发现补肾壮阳类产品中非法添加成分检出率高,需引起相关监管部门的重视。

关键词:

English

Simultaneous determination of 17 aphrodisiac chemical drugs illegally added in health products and Chinese patent medicines by high performance liquid chromatography-tandem mass spectrometry

1.
1. Guangdong Provincial Public Laboratory of Analysis and Testing Technology, China National Analytical Center (Guangzhou), Guangzhou 510070, China;
2.
2. College of Traditional Chinese Medicine, Guangdong Pharmaceutical University, Guangzhou 510006, China;
3.
3. School of Public Health, Guangdong Pharmaceutical University, Guangzhou 510024, China
Received Date: 16 November 2015
Fund Project:
广东省促进科技服务业发展计划项目(2012B040302007).

Abstract: A method was proposed for the simultaneous determination of seventeen aphrodisiac chemical drugs which were illegally mixed into the health products and Chinese patent medicines by high performance liquid chromatography-mass spectrometry (HPLC-MS/MS). The extraction, chromatographic conditions and mass spectrometry parameters were optimized in order to separate three groups of isomers. The drugs were extracted with methanol under ultrasonic condition, separated on an Agilent Extend C18 chromatographic column (100 mm×2.1 mm, 3.5 μm) with acetonitrile and water (additional 10 mmol/L ammonium acetate) as mobile phases under gradient elution at a flow rate of 0.25 mL/min. The determination was conducted by tandem mass spectrometry in positive ESI mode under multiple reaction monitoring (MRM) mode. The method made seventeen aphrodisiac chemical drugs as well as the three groups of isomers to get the ideal separation and accurate quantitative. The method was proved to be rapid, selective, sensitive and stable, and it has been applied to the screening and detection of aphrodisiac chemical drugs illegally added in health products and Chinese patent medicines. All the tested samples show that the aphrodisiac chemical drugs have a high detection rate in the recent three years. The relevant regulatory authorities should pay more attention to it.

Key words:

high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)
/ aphrodisiac chemical drugs
/ health products
/ Chinese patent medicines
/ illegally added

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

高效液相色谱-串联质谱法同时测定保健品及中成药中非法添加的17种壮阳类化学药

English

Simultaneous determination of 17 aphrodisiac chemical drugs illegally added in health products and Chinese patent medicines by high performance liquid chromatography-tandem mass spectrometry

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

高效液相色谱-串联质谱法同时测定保健品及中成药中非法添加的17种壮阳类化学药

English

Simultaneous determination of 17 aphrodisiac chemical drugs illegally added in health products and Chinese patent medicines by high performance liquid chromatography-tandem mass spectrometry

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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通讯作者: 陈斌, bchen63@163.com

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