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目的:建立高效液相色谱-碘柱后衍生化-荧光检测器检测中药材斑蝥中黄曲霉毒素B1、B2、G1、G2的含量,并采用液质联用法进行确证。方法:样品以70%甲醇溶液提取,经免疫亲和柱净化后,利用碘柱后衍生化-HPLC-FLD进行分析测定。并进一步采用LC-MS/MS对阳性样品进行确证。结果:在优化条件下,黄曲霉毒素B1、B2、G1、G2分别在0~0.525、0~0.1125、0~0.1875、0~0.1125μg的范围内线性关系良好,r>0.9996,回收率82.5%~107.3%,RSD<8.1%。检测了21批样品并通过LC-MS/MS确证,在与对照品相同的保留时间处,样品与对照品有相同的特征离子碎片,排除了样品假阳性的可能。结论:该方法简便快速,灵敏度高,重复性好,适用于斑蝥中黄曲霉毒素的检测。
OBJECTIVE: To establish a method for the determination of aflatoxins B1, B2, G1 and G2 in Chinese medicinal materials Macrophthalmil by high performance liquid chromatography with iodinated column derivatization-fluorescence detector and to confirm by LC-MS. Methods: The samples were extracted with 70% methanol solution, purified by immunoaffinity column and analyzed by iodinated column derivatization-HPLC-FLD. Positive samples were confirmed by LC-MS / MS. Results: Under the optimized conditions, the aflatoxins B1, B2, G1 and G2 showed good linearity in the range of 0-0.525,0-0.1125,0-0.1875,0-0.1125μg, r> 0.9996, the recoveries were 82.5% ~ 107.3%, RSD <8.1%. Twenty-one batches of samples were tested and confirmed by LC-MS / MS that the sample had the same characteristic ion fragmentation as the control at the same retention time as the control, precluding the possibility of false positives. Conclusion: The method is simple, rapid, sensitive and reproducible. It is suitable for the detection of aflatoxins in mackerel.