高效液相色谱-柱后光化学衍生法测定油茶中黄曲霉毒素B1的方法研究

Determination of aflatoxin Bi in youcha by post-column photochemical derivatization-high performance liquid chromatography

目的建立高效液相色谱-柱后光化学衍生法测定油茶中黄曲霉毒素B_1含量的方法。方法市售油茶样品粉碎,经80%甲醇-水溶液涡旋提取、离心,吸取上清液稀释,专用免疫亲和柱净化后,采用高效液相色谱荧光检测器串联光化学衍生器测定黄曲霉毒素B_1。同时,对样品提取条件的选择、样品净化过程、流动性比例选择等进行优化实验研究。结果黄曲霉毒素B_1在0.5～20 ng/mL范围内线性关系良好,相关系数r=0.9996,在5、10、20μg/kg添加水平下的回收率为84.0%～91.6%,相对标准偏差0.1%～1.7%。结论该方法简单、快速、准确、重现性好,适用于油茶中黄曲霉毒素B_1的定量分析。

Objective To establish a method for the determination of aflatoxin B1 in youcha by post-column photochemical derivatization-high performance liquid chromatography. Methods Commercially available samples of youcha were crushed, extracted and centrifuged by vortex extraction with 80% methanol-water. The supernatant was diluted, dedicated by immunoaffinity column, and aflatoxin B1 in youcha was determined by post-column photochemical derivatization-high performance liquid chromatography. At the same time, the optimization of the extraction conditions of the sample selection, sample purification process, and the choice of liquidity ratio were optimized. Results Aflatoxin B1 had a good linear relationship in the range of 0.5-20 ng/mL（r=0.9996）, the recoveries at the levels of 5, 10, and 20 were between 84.0% and 91.6% with the relative standard deviations of 0.1%-1.7%. Conclusion This method is simple, rapid, accurate and reproducible, which is suitable for the quantitative analysis of aflatoxin B1 in youcha.