高效液相色谱-荧光检测法同时测定六神曲(炒)中4种黄曲霉毒素

Simultaneous Determination of Four Kinds of Aflatoxin in Massa Medicata Fermentata(Fried)by HPLC-FLD

目的:建立高效液相色谱-荧光检测法同时测定六神曲(炒)中黄曲霉毒素B_(1)、B_(2)、G_(1)、G_(2)的含量。方法:样品采用70%甲醇作为提取溶剂,经免疫亲和柱净化、高效液相色谱分离、光化学柱后衍生后,通过荧光检测器测定其中黄曲霉毒素的含量。结果:黄曲霉毒素B_(1)的线性范围为0.0104~0.0520 ng(r=0.9998)、黄曲霉毒素B_(2)的线性范围为0.0038~0.0190 ng(r=0.9991)、黄曲霉毒素G_(1)的线性范围为0.0108~0.0540 ng(r=0.9991)、黄曲霉毒素G_(2)的线性范围为0.0038~0.0190 ng(r=0.9993),线性关系良好,回收率为80.54%~91.37%,RSD≤3.5%。结论:该方法操作简便,灵敏度高、重复性好、结果准确,且10批次六神曲(炒)中均检测出黄曲霉毒素G_(2)的含量,可用于六神曲(炒)中黄曲霉毒素的测定。

Objective:To establish a high performance liquid chromatography-fluorescence detection(HPLC-FLD)method for simultaneous determination of aflatoxin B_(1),B_(2),G_(1)and G_(2)in Massa Medicata Fermentata(Fried).Methods:After extraction with 70%methanol,purification by immunoaffinity column,high performance liquid chromatography and post-column photochemical derivatization,the content of aflatoxin B_(1),B_(2),G_(1)and G_(2)in the samples were determined by fluorescence detector.Results:The linearity range of aflatoxin B_(1)was 0.0104-0.0520 ng(r=0.9998).The linearity range of aflatoxin B_(2)was 0.0038-0.0190 ng(r=0.9991).The linearity range of aflatoxin G_(1)was 0.0108-0.0540 ng(r=0.9991).The linearity range ofaflatoxin G_(2)was 0.0038-0.0190 ng(r=0.9993).The linear relationship was good.The recoveries were within 80.54%-91.37%,with RSD≤3.5%.Conclusion:The method established has the advantages of convenient operation,high sensitivity,good repeatability and accurate results.Aflatoxin G_(2)was detected in 10 batches of Massa Medicata Fermentata(Fried).This method is suitable for the determination of aflatoxin in Massa Medicata Fermentata(Fried).