QuEChERS 技术结合气相色谱-串联质谱法筛查花椒中115种农药残留

Screening of 115 pesticide residues in Chinese prickly ash by QuEChERS-gas chromatography-tandem mass spectrometry

建立了QuEChERS技术结合气相色谱-串联质谱(GC-MS/MS)同时检测花椒中115种农药残留的快速分析方法。样品采用优化的QuEChERS前处理方法处理,在多反应监测模式下用GC-MS/MS检测,基质匹配内标法定量分析。结果表明:在0.002~0.4 mg/L范围内,115种农药的质量浓度与内标物质量浓度的比值和对应的目标物峰面积与内标物峰面积的比值间呈良好的线性关系,相关系数r均大于0.99;定量限为0.01~0.02 mg/kg;在0.01、0.02、0.05、0.1和0.2 mg/kg 5个添加水平下,115种农药的平均回收率为51%~150%,RSD为0.8%~34%,其中80种农药的平均回收率在70%~120%之间,满足农药残留分析要求。该方法操作简便快捷、具有良好的准确度、精密度和灵敏度,为花椒中多种农药残留的快速筛查提供了可靠的分析手段。

A rapid multiresidue analysis method for 115 pesticides in Chinese prickly ash based on QuEChERS(quick,easy,cheap,effective,rugged and safe)procedure combined with gas chromatography-tandem mass spectrometry(GC-MS/MS)was developed and validated.The samples were pretreated with optimized QuEChERS technique,detected by GC-MS/MS based on multiple reaction monitoring mode,and analyzed quantitatively by matrix-matched internal standard method.The validation results showed a good linear relationship within the calibration linearity range of 0.002-0.4 mg/L with the correlation coefficient(r)greater than 0.99.The limits of quantification for 115 pesticides were in the range of 0.01-0.02 mg/kg.The recoveries were in the range of 51%-150%with the RSDs of 0.8%-34%,when the fortified level was 0.01,0.02,0.05,0.1 and 0.2 mg/kg.Among them,the recoveries of 80 pesticides were in the range of 70%-120%which met the residue analysis requirements.This method was simple,fast,accurate,precision and sensitivity,which provided a reliable analytical tool for rapid screening of pesticide multiresidues in Chinese prickly ash.