QuEChERS-气相色谱串联质谱法测定西洋参中17种有机氯农药残留

Determination of seventeen organochlorine pesticide residues in Panax quinquefolium L.by QuEChERS-GC-MS/MS

目的建立一种测定西洋参中17种有机氯农药残留的QuEChERS-气相色谱串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)。方法样品加水润湿后用乙腈提取,QuEChERS法净化,采用DB-5毛细管柱(30 m×0.25 mm,0.25μm)分离,气相色谱串联质谱法检测。结果17种有机氯农药成分在各自浓度范围内均呈现良好的线性关系,相关系数R 2在0.9937~1.0000,检出限(LOD,S/N≥3)为0.008~2.2μg·kg^-1,定量限(LOQ,S/N≥10)为0.008~5.6μg·kg^-1,样品3水平添加回收试验的平均回收率范围在75.0%~120.0%之间,相对标准偏差在1.8%~10.0%(n=6)。结论该方法简单准确、灵敏度高,适用于西洋参药材中17种有机氯农药的同时检测。

Objective To establish a method for the determination of seventeen organochlorine pesticide residues in Panax quinquefolium L.by using QuEChERS-gas chromatography-tandem mass spectrometry.Methods The samples after hydration were extracted with acetonitrile,cleaned up by QuEChERS method and target analytes were separated by DB-5 column(30 m×0.25 mm,0.25μm).Then the samples were analysed by GC-MS/MS.Results Seventeen organochlorine pesticides have good linear relationship in their linear range,while the correlation coefficient was between 0.9937 and 1.0000.The limits of detection(LOD,S/N≥3)was from 0.008 to 2.2μg·kg^-1,while the limits of quantitation(LOQ,S/N≥10)was between 0.008 and 5.6μg·kg^-1.The recovery for seventeen organochlorine pesticides was ranged from 75.0%to 120.0%which was carried out with three levels spiked and the value of the RSD was from 1.8%to 10.0%.Conclusion The method which had the superiority of accuracy,simplicity,and sensitivity,was suitable for the detection of seventeen organochlorine pesticides in Panax quinquefolium L.simultaneously.