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目的建立测定食用植物油中黄曲霉毒素B1、B2、G1、G2的优质高效的分析方法。方法采用超高压液相色谱-串联质谱(UPLC-MS/MS)法。样品用乙酸乙酯提取,弗罗里硅土小柱净化,经C18色谱柱分离,以电喷雾离子源在正离子多反应监测(MRM)模式下进行测定,外标法定量。结果黄曲霉毒素B1、B2、G1、G2的检出限均为0.04μg/kg,定量限均为0.10μg/kg,在0.1~20μg/L范围内线性关系良好,相关系数r分别为0.9986,0.9986,0.9992,0.9996。在0.1~5.0μg/kg加标水平内黄曲霉毒素B1、B2、G1、G2的回收率为79.1%~94.6%,RSD为5.0%~9.6%。结论该方法实用、准确、灵敏,适用于食用植物油中黄曲霉毒素残留量的测定。
Objective To establish a method for the determination of aflatoxins B1, B2, G1 and G2 in edible vegetable oils with high quality and efficiency. Methods Ultra-high pressure liquid chromatography-tandem mass spectrometry (UPLC-MS / MS) was used. The sample was extracted with ethyl acetate and purified on a Florisil cartridge. The residue was separated on a C18 column and electrospray ionization (ESI) ionization was performed in a positive ion multiple reaction monitoring (MRM) mode. Results The detection limits of aflatoxins B1, B2, G1 and G2 were 0.04 μg / kg and the limits of quantitation were 0.10 μg / kg respectively. The linearity was good in the range of 0.1 ~ 20 μg / L with the correlation coefficients r of 0.9986, 0.9986,0.9992,0.9996. The recoveries of aflatoxins B1, B2, G1 and G2 were 79.1% ~ 94.6% and the RSD was 5.0% ~ 9.6% at 0.1 ~ 5.0 μg / kg spiked level. Conclusion The method is practical, accurate and sensitive and suitable for the determination of aflatoxin residues in edible vegetable oils.