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加速溶剂萃取-气相色谱-负化学源质谱法测定茶叶中有机氯和拟除虫菊酯类农药残留量
引用本文:胡贝贞,沈国军,邵铁锋,谢丽萍.加速溶剂萃取-气相色谱-负化学源质谱法测定茶叶中有机氯和拟除虫菊酯类农药残留量[J].分析试验室,2009,28(1).
作者姓名:胡贝贞  沈国军  邵铁锋  谢丽萍
作者单位:绍兴出人境检验检疫局,绍兴,312000
摘    要:建立了茶叶中13种有机氯和10种拟除虫菊酯农药残留量的气相色谱-负化学离子源.质谱(GC-NCl-MS)分析方法.茶叶样品用V(丙酮):V(CH2Cl2)=1:1混合液作提取剂经加速溶剂萃取,提取液经凝胶色谱净化除去大部分的色素、脂类和蜡质,再经活性炭-氨基(Carb-NH2)复合小柱和Florisil小柱净化后,用GC-NCl-MS的选择离子监测方式(SIM)进行定性和定量分析.添加50μg/kg 浓度水平时,农药回收率在45.6%~112.4%之间,相对标准偏差在0.57%~10.1%之间;方法的检出限(3倍信噪比)在0.05~10.0μg/kg之间.方法适用于出口茶叶农残检测实际工作.

关 键 词:加速溶剂萃取  茶叶  负化学离子源  有机氯  拟除虫菊酯

Determination of organochlorine and pyrethroid pesticide residues in tea by accelerated solvent extraction and gas chromatography-negative chemical ionization-mass spectrometry
HU Bei-zhen,SHEN Guo-jun,SHAO Tie-feng,XIE Li-ping.Determination of organochlorine and pyrethroid pesticide residues in tea by accelerated solvent extraction and gas chromatography-negative chemical ionization-mass spectrometry[J].Chinese Journal of Analysis Laboratory,2009,28(1).
Authors:HU Bei-zhen  SHEN Guo-jun  SHAO Tie-feng  XIE Li-ping
Institution:Shaoxing Entry-Exit Inspection and Quarantine Bureau;Shaoxing 312000
Abstract:A gas chromatography-negative chemical ionization mass spectrometric (GC-NCI-MS) method has been de- veloped for analyzing 23 kinds of organochlorine and pyrethroid pesticides in tea.The target analytes were extracted with acetone/dichloromethane (V/V,1:1) through accelerated solvent extraction (ASE),purified by gel permeation chromatography (GPC) to eliminate the great mass of coextracts such as pigments,fat and waxiness,and then further cleaned by Carb-NH_2 and florisil solid-phase extraction (SPE) cartri...
Keywords:Accelerated solvent extraction  Tea  Negative chemical ionization  Organochlorine  Pyrethroid  
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