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目的建立柱前衍生-UPLC-FLD法测定啤酒中黄曲霉毒素B1、B2、G1、G2的方法。方法样品直接经过乙腈稀释提取,提取液经过离心后,取上清液用多功能柱净化,净化液经氮气吹干、用三氟乙酸衍生后,经定容、微孔滤膜过滤、进液相色谱分析,以ACQUITY UPLC HSS T3柱(2.1 mm×100 mm,1.8μm)分离,荧光检测器检测,外标法定量。结果 4种黄曲霉毒素线性范围较宽,相关系数r在0.999 2~0.999 6之间,黄曲霉毒素B1、B2、G1、G2检出限分别为0.05、0.02、0.08、0.02μg/kg。加标回收率90.47%~108.17%之间,回收率的RSD在0.97%~8.13%之间。结论本法操作简便、准确度好、精密度高,干扰性小,能满足啤酒中黄曲霉毒素B1、B2、G1、G2的同时测定。
OBJECTIVE To establish a method for the determination of aflatoxins B1, B2, G1 and G2 in beer by precolumn derivatization-UPLC-FLD method. Method The sample was directly diluted by acetonitrile, after the extract was centrifuged, the supernatant was purified with a multi-functional column, the purification solution was dried by nitrogen, after derivatization with trifluoroacetic acid, filtered through a constant volume, microporous membrane filtration, into the liquid Chromatographic analysis, separated on an ACQUITY UPLC HSS T3 column (2.1 mm × 100 mm, 1.8 μm), detected by fluorescence detector and quantified by external standard method. Results The linear range of four aflatoxins was wide, the correlation coefficient was between 0.999 2 and 0.999 6, and the detection limits of aflatoxins B1, B2, G1 and G2 were 0.05, 0.02, 0.08 and 0.02 μg / kg, respectively. The spiked recoveries ranged from 90.47% to 108.17%, and the RSDs of recoveries ranged from 0.97% to 8.13%. Conclusion The method is simple, accurate, high precision and low interference, and can meet the simultaneous determination of aflatoxin B1, B2, G1 and G2 in beer.