【摘要】 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-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。更多还原

【Abstract】 Liquid chromatography tandem mass spectrometry method was established todetermine aflatoxins of 6 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 μg/kg,and the limit of detection(LOD),0.3 μg/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 1.0,5.0,10.0μg/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.更多还原