A novel method for the determination of aflatoxin B1,M1 in foods was developed using homemade mixed solid phase extraction column coupled with high performance liquid chromatography.The sample was extracted with 60％ acetonitrile solution,and cleaned up on a homemade mixed solid phase extraction column.The separation was performed on a Shim-pack VP-ODS C18 column with acetonitrile-water(20 ∶ 80) as mobile phase within 13 min.The contents of two aflatoxins were detected with fluorescence detector,and quantified by the external standard method.The effects of column type,column capacity,sample amount,extraction solution and flow rate on the determination of aflatoxin residue were investigated.Under the optimized conditions,there were good linearities between peak areas and aflatoxins concentrations in the range of 0.40-100 μg/L with correlation coefficients of 0.999 4-0.999 7.The limits of detection(S/N =3) of aflatoxin B1,M1 were both 0.050 μg/kg.The recoveries of aflatoxins in different samples at three spiked levels of 0.40,1.0,100 μg/L were in the range of 53％-112％ with relative standard deviations(RSDs) of 2.7％-7.1％.The proposed method showed the advantages of sensitivity,simplicity and fastness,and was successfully applied in the determination of low aflatoxins residues in peanut,pistachio and milk samples.%建立了基于自制混合型固相萃取柱的样品净化/高效液相色谱测定食品中黄曲霉毒素B1、M1的方法.样品经60％乙腈水溶液提取、离心后,通过自制固相萃取柱排除杂质干扰,流出液以Shim-pack VP-ODS C18色谱柱为分离柱,水和乙腈为流动相,用荧光检测器检测,外标法定量.考察了柱类型、柱容量、取样量、提取溶液和流速等对检测的影响,优化了实验条件.在优化条件下,2种毒素在0.40～100 μg/L质量浓度范围内与峰面积呈良好的线性关系,相关系数为0.9994～0.9997,检出限(S/N=3)为0.050 μg/kg.在样品中分别加入0.40、1.0、100μg/L 3种浓度水平的标准品,其加标回收率为53％～112％,相对标准偏差为2.7％ ～7.1％.该法灵敏度高,操作简单、快速,适用于花生、开心果和奶粉等食品中痕量黄曲霉毒素B1和M1的测定.
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