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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G_2、G_1、B_2、B_1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/m L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。
OBJECTIVE To establish a method for the determination of aflatoxins G_2, G_1, B_2 and B_1 in vegetable oils by ultra performance liquid chromatography-post column derivatization, and confirm the results by post-column photochemical derivatization and column iodine derivatization. Methods The samples were extracted with 70% methanol water, purified by a multi-functional purification column and analyzed by on-line ultra performance liquid chromatography-fluorescence detector-column photochemical derivatization and post column iodine derivatization. Results The aflatoxins showed good linearity in the range of 0.014-0.241 ng / mL after derivatization with postcolumn photochemical derivatization. The linearity was good in the range of 0.02-0.804 ng / mL with post-column iodine derivatization, with correlation coefficients above 0.999. Participate in 2016 peanut oil aflatoxin ability verification, after two methods of detection, each aflatoxin test values are in the ability to verify the reference value of the allowable range, the test results for the satisfactory results, quality control samples were measured in the The allowable range of the reference value indicates that both methods are accurate and stable. Conclusion The results of two kinds of derivatization methods are close and have good repeatability and accuracy. Compared with the two derivatization methods, the photochemical derivatization method has the advantages of high sensitivity, simple operation, environmental friendliness and high cost performance , For laboratory testing aflatoxin in vegetable oil.