QuEChERS-液相色谱串联质谱法测定鲜菜类调味品中10种杀菌剂残留

Determination of 10 fungicide residues in fresh vegetable condiments by QuEChERS-liquid chromatography-tandem mass spectrometry

建立鲜菜类调味品中10种杀菌剂的QuEChERS-液相色谱串联质谱测定方法,并优化QuEChERS前处理方法和液相色谱-三重四级杆质谱联用仪的色谱、质谱条件。样品经QuEChERS方法提取和净化后,以乙腈(0.05%甲酸)-水(0.05%甲酸)为流动相,梯度洗脱,经Agilent SB-Aq色谱柱(3.0 mm×100 mm,1.8μm)分离后,采用三重四极杆串联质谱仪,电喷雾离子源(ESI),多反应监测(MRM)正离子模式进行检测。结果表明,10种杀菌剂在测定范围内相关系数R2均>0.999,检出限为0.2~0.6μg/kg,加标回收率为73.0%~104.7%,精密度试验结果相对标准偏差(RSD)为1.9%~9.8%。该方法具有操作简便、灵敏、准确的特点,适用于鲜菜类调味品中10种杀菌剂的测定。

The QuEChERS-LC-MS/MS method for the determination of 10 fungicides in fresh vegetable condiments was established, and the QuEChERS pretreatment method and the chromatographic and mass spectrometry conditions of the liquid chromatography-triple quadrupole mass spectrometer were optimized. After the sample was extracted and purified by QuEChERS method, the mobile phase was gradient eluted with 0.05% formic acid acetonitrile solution-0.05% formic acid aqueous solution, separated by Agilent SB-Aq column(3.0 mm×100 mm, 1.8 μm), and detected using triple quadrupole tandem mass spectrometer, electrospray ionization(ESI) and multiple reaction monitoring(MRM) positive ion mode. The correlation coefficients of the 10 fungicides were all greater than 0.999 within the measurement range, the detection limit was 0.2-0.6 μg/kg, the recovery rate was 73.0%-104.7%, and the relative standard deviation(RSD) of precision test results was 1.9%-9.8%. The method was simple, sensitive and accurate, and was suitable for the determination of10 fungicides in fresh vegetable condiments.