QuEChERS-HPLC-MS/MS法检测谷物源性食品中3种赭曲霉毒素

Determination of 3 Ochratoxins in Cereal-derived Food by QuEChERS-HPLC-MS/MS

建立一种快速、高效的QuEChERS-HPLC-MS/MS测定谷物源性食品中的3种赭曲霉毒素的方法。样品前处理采用乙腈-水溶剂提取,经SiO2+C18+MgSO4净化后检测。以0.10%甲酸-乙腈作为流动相,在质谱检测器的多反应监测模式下进行分析。结果表明, 3种赭曲霉毒素在1.0~50.0 ng/mL质量浓度范围内线性良好,相关系数r2为0.999 2~0.999 7,检出限均为0.50μg/kg,定量限均为2.0μg/kg。在2, 4和20μg/kg 3个添加水平进行加标回收试验(n=5),回收率达到84.6%~107%。该方法具有前处理简单、净化效果好、灵敏度高和检测速度快的优点,适用于谷物基质的食品中3种赭曲霉毒素的分析和定量检测。

A rapid and effective method was established for the determination of three ochratoxins in cereal-derived food by QuEChERS-HPLC-MS/MS. The samples were extracted by acetonitrile-water and purified by SiO2+C18+MgSO4. The separation of targeted compound using 0.10% formic acid-acetonitrile as mobile phase, and the analysis was carried out under the multi-reaction monitoring mode of mass spectrometry detector. The results showed that the linear range of three ochratoxins was in the range of 1.0-50.0 ng/mL with a correlation coefficient of 0.999 2-0.999 7. The detection limit was 0.50 μg/kg and the quantitative limit was 2.0 μg/kg. The recovery tests were carried out at 2, 4 and 20 μg/kg levels(n=5), and recovery rate was 84.6%-107%. The method had the advantages of simple pretreatment, good purifying effect, high sensitivity and fast detection rate, and it was suitable for the analysis and quantitative detection of three ochratoxins in cereal-derived foods.