首页> 中文期刊>分析化学 >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

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

     

摘要

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 μg/L to 100 μg/L for ethaboxam, fluopicolide, from 0. 5 μg/L to 50 μg/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 μg/kg to 1. 3 μg/kg and the limit of detection were 0. 16 to 0. 40 μg/kg.%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l~100 μg/L,苯噻菌胺和双炔酰菌胺在0.5~50 μg/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0.53~1.3 μg/kg之间,检出限为0.16~0.40 μg/kg.

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