超高效液相色谱-串联质谱法快速测定植物油中黄曲霉毒素B_1

2.500g植物油样品用10 mL甲醇(7+3)溶液提取,以6 000r·min^-1转速离心10min,在-20℃冷冻30min后,上清液经0.22μm有机滤膜过滤,采用超高效液相色谱-串联质谱法快速测定滤液中黄曲霉毒素B_1的含量。以Accucore aQ色谱柱为固定相,以不同体积比的含5mmol·L^-1乙酸铵的0.1%(体积分数)甲酸溶液和甲醇的混合液为流动相进行梯度洗脱,串联质谱分析中采用电喷雾正离子源和选择离子监测模式。黄曲霉毒素B_1的质量浓度在0.50～10.00μg·L^-1内与其对应的峰面积呈线性关系,检出限(3S/N)为0.02μg·kg^-1。以空白样品为基体进行加标回收试验,所得回收率为86.0%～96.6%,回收量的相对标准偏差(n=6)为5.6%～8.4%。

Rapid Determination of Aflatoxin B_1 in Vegetable Oil by UHPLC-MS/MS

The vegetable oil sample(2.500 g) was extracted with 10 mL of methanol(7+3) solution and then centrifugated for 10 min at the speed of 6 000 r·min-1.After freezing for 30 min at -20℃,the supernatant was filtered with 0.22μm organic filter membrane.UHPLC-MS/MS was applied to the rapid determination of aflatoxin B1 in the filtrate.Accucore aQ chromatographic column was used as stationary phase,and the mixture of 0.1%(φ) formic acid solution(containing 5 mmol·L-1 ammonium acetate) and methanol mixed in different ratios was used as mobile phase in gradient elution.ESI+ and the selected ion monitoring mode were adopted in MS/MS.Linear relationship between values of peak area and mass concentration of aflatoxin B1 was kept in the range of 0.50-10.00μg·L-1,with detection limit(3S/N) of 0.02μg·kg-1.On the base of blank sample,test for recovery was made by standard addition method;values of recovery found were in the range of 86.0%-96.6%,with RSDs(n=6) of recovery amounts in the range of 5.6%-8.4%.