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目的:建立LC-MS/MS对中药材中黄曲霉毒素残留量的检测方法。方法:中药材粗粉甲醇提取,经免疫亲和柱净化吸附,甲醇洗脱,以甲醇/乙腈-1.0mmol乙酸铵为流动相,黄曲霉毒素含量用液相色谱-串联三重四极杆质谱测定,用电喷雾正离子模式ESI,多反应(MRM)监测。结果:黄曲霉毒素G_2、B_2在0.03～3.2ng·ml~(-1)范围内线性关系良好、黄曲霉毒素B_1、G_1在0.1～10ng·ml~(-1)范围内线性关系良好。检测限0.1ng·ml~(-1)定量限0.2ng·ml~(-1)。黄曲霉毒素回收率:86.6%～93.2%,RSD为7.1%～11.8%。结论:本法专属性强,灵敏、简便,准确,通过色谱(保留时间)及质谱特征碎片离子定性,能有效排除假阳性干扰。可作为中药中黄曲霉毒素残留量测定的方法。
Objective: To establish a method for the determination of aflatoxin residues in Chinese herbal medicines by LC-MS / MS. Methods: Methanol extract of crude meal of Chinese herbal medicines was purified by affinity column and eluted with methanol. The mobile phase consisted of methanol / acetonitrile - 1.0 mmol ammonium acetate. The aflatoxin content was determined by liquid chromatography - triple quadrupole mass spectrometry , Electrospray positive ion mode ESI, multi-reaction (MRM) monitoring. Results: The linear relationship between aflatoxins G_2 and B_2 in the range of 0.03-3.2ng · ml -1 was good. The linearity of aflatoxins B_1 and G_1 in the range of 0.1 ~ 10ng · ml -1 was good. The detection limit of 0.1ng · ml ~ (-1) was 0.2ng · ml -1. Aflatoxin recovery rate: 86.6% ~ 93.2%, RSD was 7.1% ~ 11.8%. Conclusion: This method is specific, sensitive, simple and accurate. It can effectively eliminate the false-positive interference by chromatographic (retention time) and mass spectrometric fragment ion characterization. As a method of determination of aflatoxin residues in traditional Chinese medicine.