应用QuEChERS技术与气相色谱-串联质谱法同时检测南果梨中16种农药残留  

Simultaneous determination of 16 pesticide residues in Nanguo pear by QuEChERS combined with gas chromatography-tandem mass spectrometry

作　　者：张煜卓 于湛 李硕 王妍 ZHANG Yu-zhuo;YU Zhan;LI Shuo;WANG Yan(School of Chemistry and Chemical Engineering,Shenyang Normal University,Shenyang,Liaoning 110034,China)

机构地区：[1]沈阳师范大学化学化工学院,辽宁沈阳110034 [2]岛津企业管理(中国)有限公司沈阳分公司,辽宁沈阳110016

出　　处：《现代预防医学》2019年第2期327-331,共5页Modern Preventive Medicine

基　　金：国家自然科学基金(21205080);教育部留学回国人员科研启动基金(教外司留[2012]1707);辽宁省高等学校优秀人才支持计划项目(LJQ2015105)资助

摘　　要：目的建立南果梨中霜霉威、氧乐果、特丁硫磷、西玛津、抗蚜威、噻节因、氟虫腈、二甲戊灵、氟菌唑、嘧菌环胺、虫螨腈、吡草醚、噁霜灵、溴螨酯、三氯杀螨砜及精噁唑禾草灵等16种农药残留同时检测的QuEChERS-气相色谱-串联质谱分析方法。方法使用乙腈提取样品中的农药,经N-丙基乙二胺(PSA)分散固相萃取净化,再经气相色谱-三重四级杆串联质谱分析。结果 16种农药在线性范围内相关系数均大于0.994。方法检出限范围(S/N=3)为0.01～1.62μg/kg,方法定量限范围为0.02～5.40μg/kg。当加标水平为62.5μg/kg时,其回收率在78.5%～98.6%之间,相对标准偏差(RSD)在3.8%～11.4%之间。结论该方法具有操作简单、快速、灵敏的特点,适用于南果梨中农药多残留的检测。Objective To establish a QuEChERS-gas chromatography-tandem mass spectrometric method for simultaneous determination of 16 pesticide residues including propamocarb, omethoate, terbufos, simazine, pirimicarb, dimethipin, fipronil,pendimethalin, triflumizole, cyprodinil, chlorfenapyr, pyraflufen-ethyl, oxadixyl, bromopropylate, tetradifon, and fenoxapropp-ethyl in Nanguo pears. Methods The target pesticides in the fruit were extracted with acetonitrile, purified with N,N-diisopropylamino ethylamine primary secondary amine(PSA) and analyzed by gas chromatography-tandem mass spectrometry.Results The result implis that all the linear relationships are good with correlation coefficients greater than 0.994. The limits of detection in this work are from 0.01 to 1.62 μg/kg and the limits of quantification are in the range of 0.02-5.40 μg/kg.When prevented level was 62.5% μg/kg, the recovery rates and the relative standard deviation(RSD) of the method range from 78.5 % to 98.6 % and from 3.8 % to 11.4 % at 62.5 μg/kg, respectively. Conclusion The method introduced in this work is convenient, quick, sensitive, and mostly suitable for the analysis of multi pesticide residues in Nanguo pears.

关 键 词：水果 QUECHERS GC—MS/MS 农残 

分 类 号：R155[医药卫生—营养与食品卫生学]