加速溶剂萃取-气相色谱-三重四极杆串联质谱法测定粮谷中的51 种农药残留

为建立用气相色谱-三重四极杆串联质谱仪检测进出口粮谷中51 种农药残留的方法，通过考察不同加速溶剂萃取温度和萃取试剂的实验效果，建立了最优加速溶剂萃取条件，分别以高粱和大麦为研究基质，比较了3 种净化方式的净化效果，通过气相色谱-三重四极杆串联质谱仪有效解决了粮谷中多农药残留检测的问题，在系统优化的基础上建立了高粱中多种农药残留检测方法，并用大麦和燕麦其他的粮谷基质考察检测方法的适应性，同时对3 个添加水平6 个高粱、大麦、燕麦平行样品分析，该方法的回收率为62.4%～119.7%，相对标准偏差为0.5%～17.3%，检出限为0.03～2.07 μg/kg，方法相关指标均满足检测要求，适用于粮谷中农药残留高通量检测需要。

Determination of 51 Pesticide Residues in Cereals Using Accelerated Solvent Extraction and Gas Chromatography-Triple Quadrupole-Tandem Mass Spectrometry

A method was developed for detecting 51 pesticide residues in import and export cereals by gas chromatography-triple quadrupole-tandem mass spectrometry (GC-MS/MS). The optimal conditions for accelerated solvent extraction were established by investigating the effect of extraction temperature and solvent on extraction efficiency. The purification efficiencies of three different methods were compared for pesticide residues extracted from sorghum and barley. Multi-pesticide residues in sorghum were detected by GC-MS/MS, and the suitability of the analytical method for determining other cereals including barley and oat was investigated. The detection of six parallel samples of sorghum, barley and oat at three spiked levels showed that the recoveries for all pesticides were between 62.4% and 119.7%, with relative standard deviations (RSDs) varying from 0.5% to 17.3%, and the limits of detection (LODs) of the method were between 0.03 μg/kg and 2.07 μg/kg. This method can meet the analytical requirements and is suitable for high-throughput determination of multi-pesticide residues in cereals.