液相色谱-串联质谱法测定果蔬中4种新型卵菌纲杀菌剂残留  

Determination of New Type of 4 Bactericids Used for Control of Oomycete Diseases Residues in Fruits and Vegetables by Liquid Chromatography/Tandem Mass Spectrometry

作　　者：崔淑华[1,2] 许美玲 钱家亮 段浩 刘金峰 林黎明 王开运[1] 

机构地区：[1]山东农业大学植物保护学院,泰安271018 [2]临沂出入境检验检疫局检验检疫技术中心,临沂276034 [3]山东省检验检疫局科学技术研究院,青岛266555

出　　处：《分析化学》2011年第12期1836-1840,共5页Chinese Journal of Analytical Chemistry

基　　金：国家质检公益性行业科研专项(No.200910145-2)资助

摘　　要：建立了蔬菜和水果中噻唑菌胺、苯噻菌胺、氟啶酰菌胺和双炔酰菌胺4种新型卵菌纲杀菌剂的分散固相萃取-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ODSC18-N两种基质分散净化剂净化,采用液相色谱-三重四级杆串联质谱(LC/MS/MS)检测。实验通过空白基质溶液稀释标准建立校正的标准曲线,以消除基质效应。结果表明,噻唑菌胺和氟啶酰菌胺在1～100μg/L,苯噻菌胺和双炔酰菌胺在0.5～50μg/L线性范围内具有良好的线性关系,相关系数为0.9994～0.9999;4种卵菌纲杀菌剂添加回收率在80.9%～101.3%之间;相对标准偏差(RSD)均小于6.3%。定量限在0.53～1.3μg/kg之间,检出限为0.16～0.40μg/kg。A method was developed for the determination of ethaboxam,benthivalicarb-isopropyl,fluopicolide and mandipropamid in fruits and vegetables.The analytes were extracted from the samples by acetonitrile,and purified by dispersion solid phase extraction using ODS C18-N and PSA as solidphase,and then analyzed by LC/MS/MS with multiple reaction monitoring（MRM）.The interference of matrix was reduced by the matrix-matched calibration standards curve.The linear range was from 1 μ /L to 100 μ /L for ethaboxam,fluopicolide,from 0.5 μ/L to 50 μ g/L for benthivalicarb-isopropyl,mandipropamid（r≥0.9994）.The fortified recoveries were from 80.9% to 101.3% with relative standard deviations（RSD） lass than 6.3%.The limits of quantification were 0.53 μ g/kg to 1.3 μ g/kg and the limit of detection were 0.16 to 0.40 μ g/kg.

关 键 词：液相色谱串联质谱 果蔬 QuEChERS方法 噻唑菌胺 苯噻菌胺 氟啶酰菌胺 双炔酰菌胺 

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