摘要
基于气相色谱-三重四极杆质谱(GC-MS/MS)建立了快速测定植物源性产品中草枯醚和氟除草醚残留量的方法。蔬菜、水果、谷物、油料、茶叶、调味料和药用植物等样品经乙酸乙酯提取,离心后上清液经分散固相萃取净化,经TG-5SILMS毛细管色谱柱(30 m×0.25 mm×0.25,μm)分离,采用GC-MS/MS分析,在多反应监测(MRM)模式下检测,基质匹配外标法定量。对样品前处理条件特别是净化试剂的选择和含量进行了优化,确定了最优化的实验条件。在优化实验条件下,目标化合物在2.5~250μg/L范围内的线性关系良好,相关系数均大于0.99,方法定量限为0.005 mg/kg。空白样品在低、中、高3个添加水平下的平均回收率为89.5%~116.8%,相对标准偏差(RSD,n=6)为2.3%~9.2%,方法的准确度和精密度符合农药残留测定要求。该方法具有操作简单、快速、灵敏、准确的特点,能满足植物源性产品中草枯醚和氟除草醚的检测要求。
A rapid determination method was developed for chlornitrofen and fluoronitrofen residues in plant-derived products by gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS).Chlornitrofen and fluoronitrofen residues in vegetables,fruits,grains,oilseeds,tea,spices and medicinal plants were extracted with ethyl acetate,and purified by dispersive solid phase extraction after centrifugation.After centrifugation and filtration,the target compounds were analyzed in the multiple reaction monitoring mode by GC-MS/MS,and quantified by matrix matching external standard method.The sample pretreatment conditions,especially the selection of purification reagents and content were optimized,and the optimal experimental conditions were determined.The results showed that the calibration curves were linear in the range of 2.5-250μg/L with correlation coefficients higher than 0.99.Recovery tests were conducted by adding mixed standards to blank samples at three concentration levels.The recoveries were in the range of 89.5%-116.8%with relative standard deviations(RSDs,n=6)of 2.3%-9.2%.The quantitation limits of chlornitrofen and fluoronitrofen were 0.005 mg/kg.The accuracy and precision of this method met the requirements of pesticide residue determination.The method is simple,rapid,and sensitive;can meets the requirements for the detection of chlornitrofen and fluoronitrofen residues in plant-derived products.
作者
荣杰峰
修凡超
陈富泓
许美珠
翁城武
徐敦明
RONG Jiefeng;XIU Fanchao;CHEN Fuhong;XU Meizhu;WENG Chengwu;XU Dunming(Quanzhou Customs Comprehensive Technology Service Center,Quanzhou 362000;Xiamen Customs Technology Center,Xiamen 361000)
出处
《分析科学学报》
CAS
CSCD
北大核心
2023年第2期139-145,共7页
Journal of Analytical Science
基金
云南重大科技专项计划(202102AE090042)。
关键词
草枯醚
氟除草醚
植物源性产品
气相色谱-三重四极杆质谱法
Chlornitrofen
Fluoronitrofen
Plant-derived products
Gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS)
