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大体积进样气质联用法测定浓缩果蔬汁中农药的残留量
引用本文:王建华, 张艺兵, 储晓刚, 王修林. 大体积进样气质联用法测定浓缩果蔬汁中农药的残留量[J]. 分析测试学报, 2006, 25(2): 29-34
作者姓名:王建华   张艺兵   储晓刚   王修林
作者单位:1. 山东出入境检验检疫局,山东,青岛,266002;中国海洋大学,化学化工学院,山东,青岛,266003
2. 山东出入境检验检疫局,山东,青岛,266002
3. 中国检验检疫科学研究院,食品安全研究所,北京,100025
4. 中国海洋大学,化学化工学院,山东,青岛,266003
基金项目:科技部食品安全专项基金
摘    要:建立了气相色谱-质谱同时检测果蔬汁中多类农药残留的方法。利用Agilent仪器的保留时间锁定功能(RTL)及相应的质谱农药库,建立了多类农药选择离子监测的分组时间窗,避免了仪器维护后农药保留时间烦琐的更新过程,保证了农药保留时间的重复性;探讨了具有溶剂排空模式的程序升温蒸发(PTV)对大体积进样的作用。通过对分流排空量、吹扫时间、PTV温度及其进样体积等PTV参数的优化,提高了检测灵敏度。通过同位素标汜农药作为内标,GC—MS的定量可靠性得到改善。

关 键 词:大体积进样  农药  水果汁  蔬菜汁  程序升温蒸发  气相色谱-质谱
文章编号:1004-4957(2006)02-0029-06
收稿时间:2005-03-19
修稿时间:2005-05-20

Determination of Pesticide Residues in Concentrated Fruit and Vegetable Juices by Gas Chromatography- Mass Spectrometry with Large-volume, Temperature-programmed Injection
WANG Jian-hua,ZHANG Yi-bing,CHU Xiao-gang,WANG Xiu-lin. Determination of Pesticide Residues in Concentrated Fruit and Vegetable Juices by Gas Chromatography- Mass Spectrometry with Large-volume, Temperature-programmed Injection[J]. Journal of Instrumental Analysis, 2006, 25(2): 29-34
Authors:WANG Jian-hua  ZHANG Yi-bing  CHU Xiao-gang  WANG Xiu-lin
Abstract:A GC-MS procedure in the selected ion monitoring mode was developed for the determination of multiple pesticide residues in concentrated fruit and vegetable juices.Retention time locking(RTL) pesticide database was used to simplify the editing of SIM ion groups and eliminate the tedious retention time updating process upon instrument maintenance.Large volume injection of samples with a temperature-programmed vaporizer(PTV) system was investigated.Split vent flow,purge time,PTV system temperature,and maximum sample volume were optimized.In comparison with conventional methods,the detection limits were improved by one order of magnitude.By use of stable isotopically labeled pesticides(surrogate) as internal standards,the reliability of quantification in GC-MS analysis could be improved.
Keywords:Large-volume injection   Pesticide   Fruit juice   Vegetable juice    Programmable temperature vaporizer   Gas chromatography- mass spectrometry
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