液相色谱-串联质谱法测定果蔬中双三氟虫脲、四氯虫酰胺和氰虫酰胺残留  

Determination of New Bistrifluron,Cyantraniliprole and SYP9080 Residues in Fruits and Vegetables by Liquid ChromatographyTandem Mass Spectrometry

作　　者：崔淑华[1] 李瑞娟[2] 张晓梅[1] 程刚[1] 王宇[1] 李正义[1] CUI Shu-Hua;LI Rui-Juan;ZHANG Xiao-Mei;CHENG Gang;WANG Yu;LI Zheng-Yi(Iuspectiou aud Quarautiue Technology Center of SeauMoug Exit/Entry Iuspectiou aud Quarautiue Bureau , Qingdao 266002 , China;Institute of Plant Protection,SeauMoug Academy of Agriculture , Jinan 250100 , C hina)

机构地区：[1]山东出入境检验检疫局检验检疫技术中心,青岛266002 [2]山东省农业科学院植物保护研究所,济南250100

出　　处：《分析化学》2017年第4期545-552,共8页Chinese Journal of Analytical Chemistry

基　　金：山东出入境检验检疫科研项目(No.SK201425)资助

摘　　要：建立了蔬菜和水果中双三氟虫脲、四氯虫酰胺和氰虫酰胺3种新型杀虫剂的分散固相萃取-液相色谱-串联质谱检测方法。样品经乙腈均质提取,混合使用乙二胺-N-丙基硅烷(PSA)和C18基质分散净化剂进行净化,液相色谱-三重四极杆串联质谱(LC-MS/MS)同时进行检测。双三氟虫脲和四氯虫酰胺采用多反应监测负离子模式,氰虫酰胺采用多反应监测正离子模式。双三氟虫脲在苹果、洋葱和经微波处理的洋葱样品中均不存在基质效应,可采用纯溶剂标准外标法或者采用基质匹配标准溶液定量检测;四氯虫酰胺和氰虫酰胺存在程度不同的基质减弱效应,采用空白基质匹配的校正标准曲线外标法定量。3种杀虫剂均在0.2~100μg/L线性范围内具有良好的线性关系,相关系数均大于0.9990。在0.005~2.000 mg/kg范围内,平均添加回收率为81.6%~99.9%,相对标准偏差为3.6%~9.8%。氰虫酰胺、四氯虫酰胺和双三氟虫脲的检出限分别为0.064,0.048和0.001μg/kg,定量限分别为0.210,0.160和0.004μg/kg。A liquid chromatography-tandem mass spectrometric(LC-MS/MS)method was developed for thedetermination of bistrifluron,cyantraniliprole and SYP9080residues in fruits and vegetables.The analyteswere extracted from samples with acetonitrile,and purified by dispersion solid phase extraction using C18andprimary secondary amine(PSA)as solid phase adsorbent,then analyzed by LC-MS/MS.Bistrifluron andSYP9080were analyzed with negative ion multiple-reaction monitoring(MRM),cyantraniliprole was analyzedwith positive ion MRM.The matrix-induced weakening effect was observed in the analysis of cyantraniliproleand SYP9080in several samples including cucumber,apple and onion,and the weakening extent of thematrix-induced effect depended on the sample properties.But no matrix effect was found in the analysis ofbistrifluron in several samples.The interference of matrix was reduced by using the matrix-matched calibrationstandards curve in the analysis of cyantraniliprole and SYP9080.Bistrifluron could be quantified by anexternal standard of the matrix-matched calibration standards or the pure solvent calibration standards.Thelinear range was from0.2滋g/L to100滋g/L for bistrifluron,cyantraniliprole and SYP9080with the goodcorrelation coefficients(r逸0.9990).The recoveries of cucumber,grape,apple and scallion addedbistrifluron at0.005-2m^^kg were79.8%-99.9%,with relative standard deviations(RSD)of3.6%-9.8%.The limits of quantification(S/N=10)were0.210滋g/k g,0.160滋g/kg and0.004滋g/kg,andlimits of detection(S/N=3)were0.064滋g/kg,0.048滋g/kg and0.001滋g/kg for bistrifluron,cyantraniliprole and SYP9080,respectively.

关 键 词：液相色谱-串联质谱 水果和蔬菜 双三氟虫脲 四氯虫酰胺 氰虫酰胺 

分 类 号：TS255.7[轻工技术与工程—农产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]