中药制剂和保健品中11种化学降糖药的快速检验

HPLC-MS/MS fast detection of eleven kinds of anti-diabetic agents in traditional Chinese medicines and health care products

目的：建立检测中药制剂和保健品中非法掺入化学降糖药的专属性方法。方法：采用液相色谱一离子肼质谱联用法。色谱条件：AgilentTCC18（150mm×4．6mm，5μm）色谱柱，以0．01％三氟乙酸-乙腈为流动相，柱温30℃，流速0．6mL·min^-1，检测波长230nm；质谱条件：电喷雾离子源（ESI）正离子检测，扫描方式采用全扫描一级质谱、选择离子二级质谱（MS／MS），质荷比范围50～800m／z，干燥气温度350℃，干燥气流速8L·min^-1，雾化气压力206．7kPa，分流比1：1。结果：11种化学降糖药实现了同时分离与专属鉴定；利用本法，从42个样品中检测出6种非法添加化合物。结论：本法可以有效地用于快速检测中药制剂和保健品中非法添加的化学降糖药。

Objective：To develop a specific method for the identification of 11 chemical drugs added illegally into traditional Chinese medicines and health care products. Methods：The liquid chromatography- ion trap mass spectrometry method was used. HPLC separations were performed on an Agilent TC C18 column with the mobile phase of 0. 01% trifluactic acid and acetonitrile by gradient elution at the flow rate of 0. 6 mL · min^-1, the detection wave- length was 230 rim. Electrosprayionization （ESI） source was applied and operated in the postived ion mode with two scan modes including full scan MS and full scan MS - MS, the scan range was 50 - 800m/z, the temperature of drying gas was 350℃, the flow rate of drying gas was 8 L · min ^-1, the pressure of nebulizer gas was 206. 7 kPa. Restilt： Eleven kinds of anti - diabetic agents were well separated and clearly identified by HPLC - MS/MS. Six kinds of anti - diabetic agents have been successfully detected among the 42 drugs on the market. Conclusion ： The developed method can be able to apply for the fast detection of anti - diabetic agents added illegally into traditional Chinese medicines and health care products.