液相色谱-串联质谱测定枸杞、大青叶等中药材中6种黄曲霉毒素

建立了中药材中6种黄曲霉素毒素的液相色谱串联质谱测定方法。中药材样品经粉碎后，采用70％的甲醇溶液高速搅拌、超声提取，提取液经免疫亲和柱净化后采用液相色谱一串联质谱仪测定黄曲霉毒素，外标法定量。可同时检测样品中黄曲霉毒素B1、黄曲霉毒素B2、黄曲霉毒素G1、黄曲霉毒素G2、黄曲霉毒素M1、黄曲霉毒素M2等6种黄曲霉毒素。方法的检出限为0.3μg／kg，定量限为1μg／kg，各基质在1μg／kg、5μg／kg、10μg／kg等3个水平的添加回收率（n=5）为78．9％-100.2％，相对标准偏差为4．2％-12．6％。该方法的检测速度快，基质干扰较少，结果准确、可靠，定量限可满足国内外对中药材黄曲霉毒素相关限量的要求。

Determination of 6 Aflatoxins in Chinese Herbs by Liquid Chromatography Tandem Mass Spectrometry

Liquid chromatography tandem mass spectrometry method was established todetermlne atlatoxms ot o Chinese herbs samples after crushing, high speed stirring, ultrasonic extraction with 70% methanol solution, were extracted. The extractions were purified by immune affinity column and then aflatoxin was determined by liquid chromatography-tandem mass spectrometry （LC/MS/MS） f with external standard method of quantitation. The method could detect aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2, aflatoxin M1 and M2 of samples at the same time. The limit of quantification （LOQs） of the 6 aflatoxin were 1 gg/kg,and the limit of detection（LOD）, 0.3 gg/kg. The average recoveries of the 6 aflatoxins spiked in Chinese herbs （Wolfberry, Folium, Citrus, Astragalus） ranged from 78.9% to 100.2% at the three spiked levels of 1.0, 5.0, 10.0gg/kg respectively, and the relative standard deviations （RSDs. n=5） were between 4.2% and 12.6%. The method is rapid, sensitive and accurate, and suitable for the determination of the 6 aflatoxins in Chinese medicines. The quantification limits of aflatoxins can meet the domestic and foreign requirements.