GC-MS/MS同时测定杭白菊中68种农药残留  

Simultaneous Determination of 68 Pesticide Residues in Chrysanthemum Morifolium by GC-MS/MS

作　　者：朱海花 徐强[1] 冯瑛[1] 王溶溶[1] ZHU Haihua;XU Qiang;FENG Ying;WANG Rongrong(Zhejiang Research Institute of Traditional Chinese Medicine Co.,Ltd.,Hangzhou 310023,China)

机构地区：[1]浙江省中药研究所有限公司,杭州310023

出　　处：《中国现代应用药学》2018年第11期1702-1708,共7页Chinese Journal of Modern Applied Pharmacy

基　　金：浙江省科技计划项目(2016F10034);药品医疗器械审评审批制度改革子课题(ZG2016-2-04);浙江省农业新品种选育重大科技专项(2016C02058)

摘　　要：目的采用GC-MS/MS建立同时测定杭白菊中68种农药残留的分析方法。方法样品采用QuEChERS前处理程序,经1%冰醋酸浸泡30 min后,乙腈提取,经装有无水硫酸镁900 mg、PSA 300 mg、十八烷基键合硅胶300 mg、硅胶300 mg和石墨化炭黑90 mg的分散固相萃取净化管净化,采用GC-MS/MS动态多反应监测模式,进行定性定量分析。结果68种农药在各自浓度范围内线性关系良好,相关系数r均>0.993。在20,100,200μg·kg^(-1) 3个不同加标水平下,除六氯苯、甲基五氯苯硫醚、苯氟磺胺、p,p'-滴滴伊和氯氟氰菊酯外,大部分农药的回收率均在70.0%～120.0%之间,RSD在0.4%～13.9%之间。方法的检出限为0.2～25.6μg·kg^(-1),定量限为0.8～85.5μg·kg^(-1)。结论该方法简单、快速、高效、灵敏,可为杭白菊中多农药残留的快速筛查和测定提供一种有效的分析手段。OBJECTIVE To establish a multi-residue analytical method for the determination of 68 pesticides in Chrysanthemum morifolium by GC-triple quadrupole mass spectrometry(GC-MS/MS).METHODS Samples were treated with QuEChERS pretreatment method.They were extracted with acetonitrile after soaking in 1% acetic acid for 30 min,and then purified by dispersed solid-phase extraction and purification tubes containing 900mg of anhydrous magnesium sulfate,300mg of PSA,300mg of octadecyl-bonded silica,300mg of silica gel and 90mg of graphitized carbon black.The GC-MS/MS dynamic multiple reaction monitoring (dMRM)mode was used for the qualitative and quantitative analysis.RESULTS The linear relationship of each pesticide residue was good(r>0.993)in their respective concentration range.The recoveries of most pesticides were between 70.0%and 120.0%at 3 spiked levels of 20,100,200μg·kg-1,with the relative standard deviations(RSD) from 0.4% to 13.9%,except hexachlorobenzene,methyl-pentachlorophenyl sulfide,dichlofluanid,DDE-p,p'and cyhalothrin.The limits of detection(LOD)were 0.2-25.6μg·kg-1,and the limits of quantification(LOQ)were 0.8-85.5μg·kg-1.CONCLUSION The method is simple,rapid,efficient and sensitive,which can be used for the simultaneous anlysis and screening of pesticide multiresidues in Chrysanthemum morifolium.

关 键 词：杭白菊 农药残留 气相色谱-三重四极杆串联质谱 QUECHERS 

分 类 号：R917[医药卫生—药物分析学]