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

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。

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

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.