2种超高效液相色谱-柱后衍生法对植物油中黄曲霉毒素的测定与分析

Determination and analysis of aflatoxins in vegetable oil by ultra high performance liquid chromatography with 2 kinds of post-column derivatization

中文关键词:  黄曲霉毒素  光化学衍生  碘化学衍生  超高效液相色谱法  植物油

英文关键词:aflatoxins  photochemical derivatization  iodine derivatization  ultra performance liquid chromatography  vegetable oil

中文摘要:

      目的 建立超高效液相色谱-柱后衍生法测定植物油中黄曲霉毒素G2、G1、B2、B1的含量, 并通过柱后光化学衍生法及柱后碘衍生法进行比对确认。方法 样品采用70%的甲醇水提取, 经多功能净化柱净化, 利用在线超高效液相色谱-荧光检测器-柱后光化学衍生及柱后碘衍生进行测定分析。结果 黄曲霉毒素通过柱后光化学衍生后, 在0.014~0.241 ng/mL范围内线性关系良好, 通过柱后碘衍生在0.02~0.804 ng/mL范围内线性关系良好, 相关系数均在0.999以上。参与2016年花生油中黄曲霉毒素的能力验证, 经过2种方法的检测, 各黄曲霉毒素检测值均在能力验证的参考值允许范围内, 考核结果为满意结果, 质控样的检测值均在参考值允许范围内, 表明2种方法均准确稳定。结论 2种衍生方法的测定结果比较接近, 均有较好的重复性和准确性, 通过2种衍生方法的比较, 光化学衍生法较之有灵敏度高、操作简便、绿色环保、性价比较高的优点, 适用于实验室对植物油中黄曲霉毒素的检测。

英文摘要:

      Objective To establish a method for the simultaneously determination of aflatoxins G2, G1, B2 and B1 in vegetable oil by ultra performance liquid chromatography (UPLC) with 2 kinds of post-column derivatization and confirm the positive samples through post-column iodine and photochemical derivatization. Methods After extraction by 70% methanol and purification by immunoaffinity column, the aflatoxins were analyzed by UPLC with post-column derivatization. Results The linear relationships of aflatoxins G2, G1, B2 and B1 ranged from 0.014~0.241 ng/mL with post-column photochemical derivatization and 0.02~0.804 ng/mL with post-column iodine derivatization, with correlation coefficients above 0.999. Through 2 detection methods, the test values of aflatoxins were within the reference range and the results were satisfactory in proficiency testing of aflatoxins. The test values of the quality control samples were within the range of reference values, so the 2 detection methods were accurate and stable. Conclusion The detection results with the 2 post-column derivatization methods are similar, both have good repeatability and accuracy. Through the comparison of 2 kinds of derivation, photochemical derivation method is superior because of high sensitivity, simple operation, green environment and high price performance, which is more suitable for the determination of aflatoxins in vegetable oil.