气相色谱-三重四极杆串联质谱法快速测定蔬菜水果中129种农药的残留量

采用QuEChERS方法结合气相色谱-串联质谱法(GC-MS/MS)建立了蔬菜、水果中129种农药残留同时检测的分析方法。试样用1%乙酸乙腈均质提取,采用混合型固相分散萃取剂净化后,用GC-MS/MS在多反应离子监测(MRM)模式下进行检测,外标法定量。结果表明,129种药物在一定的含量范围内线性关系良好,相关系数(r2)均大于0.98；不同基质在10 μg/kg添加水平下大部分农药的平均回收率为66.2%～124.7%,相对标准偏差(RSD)为0.9%～24.4%；方法的定量限(LOQ)为0.03～16.7 μg/kg。结果表明,该方法简便快速、灵敏可靠、经济有效,适用于蔬菜、水果中农药多残留的同时快速筛查测定。

Rapid determination of 129 pesticide residues in vegetables and fruits by gas chromatography-triple quadrupole mass spectrometry

An analytical method for the simultaneous determination of 129 pesticides in vegetables and fruits was established based on optimized QuEChERS with gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS). The samples were extracted with acetonitrile (containing 1% (v/v) acetic acid), then the extracts were determined by GC-MS/MS in multi-reaction monitoring (MRM) mode after being cleaned up with mixed solid-phase dispersion, and the external standard method was applied to quantify the pesticides. The results showed that all the 129 pesticides had good linearity in certain ranges with the correlation coefficients (r2) higher than 0.98. The average recoveries of the most of 129 pesticides in different matrices were in the range of 66.2%-124.7% at the spiked level of 10 μg/kg, with relative standard deviations (RSDs)of 0.9%-24.4%. The limits of quantification (LOQs) of the method were 0.03-16.7 μg/kg. The results demonstrated that the developed method is simple, rapid, sensitive and high efficient for screening multiple pesticide residues in vegetables and fruits.