QuEChERS-三重四极杆-气质联用法测定西洋参中227种农药残留

Determination of 227 pesticide residues in Panacis Quinquefolii Radix by QuEChERS-triple quadrupole-gas chromatography

目的:建立QuEChERS-气相色谱-三重四极杆串联质谱(GC-MS/MS)相结合技术同时测定西洋参中227种农药的检测方法,并对50批次西洋参样品进行农药残留筛查。方法:先向粉碎好的西洋参样品中加入乙腈,涡旋混匀后再加无水硫酸镁与无水乙酸钠的混合粉末摇散,震荡,离心,取上清液经QuEChERS技术净化,应用三重四极杆-气质联用多反应监测模式(MRM)进行检测分析,通过基质匹配标准曲线进行校正。结果:227种农药在2.50~250 ng·mL^(-1)范围内呈现良好的线性关系(r>0.995 9);定量限为0.01~0.05μg·kg^(-1);精密度(RSDs)在0.16%~11.62%(n=6),回收率在61.4%~125.3%;50批次西洋参中样品检出率为80.0%,共检出29种农药,其中灭菌磷检出率最高,达到66.0%。结论:该方法操作简便,重复性好,准确可靠,可用于西洋参中农药残留的快速筛查,为西洋参的种植生产及质量监管提供技术支撑。

Objective:To develop a QuEChERS-gas chromatography-triple quadrupole tandem mass spectrometry(GC-MS/MS)method for the simultaneous determination of 227 pesticide residues in Panacis Quinquefolii Radix,and to screen 50 batches of panax quinquefolium for pesticide residues.Method:The crushed samples were extracted by acetonitrile,then the powder of anhydrous magnesium sulfate and anhydrous sodium acetate was added,shaken,centrifuged.The supernatant was purified by QuEChERS technology.The samples were analyzed by multiple reaction monitoring(MRM)and corrected by matrix matching standard curve.Results:The 227 pesticides showed good linear relationship in the range of 2.50-250 ng·mL^(-1)(r>0.9959).The limits of quantification were 0.01-0.05μg·kg^(-1).The precision(RSDs)were in the range of 0.16%-11.62%(n=6)and the recoveries were in the range of 61.4%-125.3%.The detection rate of 50 batches of panax quinquefolium samples was 80.0%,a total of 29 pesticides were detected.The detection rate of sterilized phosphorus was the highest as 66.0%.Conclusion:The method is simple,reproducible,accurate and reliable.The method can be used for the rapid screening of pesticide multi-residues in panax quinquefolium,providing technical support for the cultivation,production and quality control of Panacis Quinquefolii Radix.