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    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B1

    Rapid Determination of Aflatoxin B1 in Vegetable Oil by UHPLC-MS/MS

    • 摘要: 2.500 g植物油样品用10 mL甲醇(7+3)溶液提取,以6 000 r·min-1转速离心10 min,在-20℃冷冻30 min后,上清液经0.22 μm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B1的含量。以Accucore aQ色谱柱为固定相,以不同体积比的含5 mmol·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B1的质量浓度在0.50~10.00 μg·L-1内与其对应的峰面积呈线性关系,检出限(3S/N)为0.02 μg·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%。

       

      Abstract: 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 0.22 μm 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 0.50-10.00 μg·L-1, with detection limit (3S/N) of 0.02 μg·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%.

       

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