文献类型：期刊文献

中文题名：固相萃取-液相色谱-电喷雾串联质谱法测定鲜枣中14种农药残留

英文题名：Determination of 14 Pesticide Residues in Fresh Jujube Using Liquid Chromatography Coupled with Electrospray Ionization Tandem Mass Spectrometry

作者：钟冬莲[1] 刘毅华[1] 沈丹玉[1] 莫润宏[1] 丁明[1] 汤富彬[1]

第一作者：钟冬莲

机构：[1]中国林科院亚热带林业研究所/国家林业局经济林产品质量检验检测中心(杭州)

年份：2015

卷号：34

期号：7

起止页码：731-737

中文期刊名：食品与生物技术学报

外文期刊名：Journal of Food Science and Biotechnology

收录：CSTPCD;;Scopus;北大核心:【北大核心2014】；CSCD:【CSCD2015_2016】；

基金：国家林业公益行业科研专项课题(201304705;201204414)

语种：中文

中文关键词：固相萃取;鲜枣;液相色谱-串联质谱法;农药残留

外文关键词：solid phase extraction,fresh jujube,Liquid chromatography tandem mass spectrometry(LC-MS/MS),pesticides residues

分类号：O657.63

摘要：选择强疏水性硅肢基质tC18柱为固相萃取净化柱,以电喷雾（ESI）为离子源,正离子多级 反应离子监测（MRM ＆模式,建立了固相萃取-液相色谱-串联质谱法（HPLC-MS/MS ＆测定鮮枣中 14种农药（包括有机磷杀虫剂、杀菌剂,有机杂环类杀虫剂和新型烟碱类杀虫剂＆残留的分析方 法.研究比较了不同提取溶剂的提取效果和不同固相萃取小柱的净化效果,同时优化了色谱分 离条件和质谱条件.14种农药在10-500 μg/L （或1-50μg/L）范围内线性相关,相关系数为 0.996 3-0.999 9,方法的定量限为0.10-9.50 μg/kg.14种农药在鮮枣中3个水平添加质量浓度 的的回收率在67.4%-116.8%,RSD为0.8%-14.8%之间.该方法操作简便,灵敏度、准确度和精 密度均符合农药多残留检测 ,适用于鮮枣中14种农药多残留的测.
This study developed a method to identify 14 pesticides residues(including organic phosphorus insecticides,fungicides,organic heterocyclic pesticides and novel nicotine insecticide) in fresh jujube by solid-phase extraction and liquid chromatography coupled with electrospray ionization tandem(HPLC-MS/MS),in which a strong hydrophobic silica bonded t C18 column was selected as the solid-phase extraction,electrospray ionization(ESI) was used as the ion source and positive ion multiple reaction monitoring(MRM) was set as the detection mode. The effects of different extraction solvents and solid-phase extraction columns were compared for the determination of 14 pesticides residues,and at the meanwhile the separation and detection conditions for the multiresidue analysis by chromatography and mass spectrometry were also optimized. A good linear relationship could be achieved for the detection of 14 pesticides in fresh jujube in the range of10~500 μg/L(or 1~50 μg/L),with the correlation coefficients of 0.996 3~0.999 9,the quantitation limits of 0.10~9.50 μg/kg,the recoveries of 67.4% ~116.8% for 14 pesticides of three different concentrations,and RSD of 0.8% ~14.8%. The optimized method,which is applicable to determine14 pesticide residues in fresh jujube,meets the requirements of the multiresidue analysis with simple operation,good sensitivity,and high accuracy.