| 固相萃取净化-液相色谱串联质谱确证茶叶中的6种乙撑双二硫代氨基甲酸盐类农药残留 |
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| 引用本文： | 祝伟霞,杨冀州,刘亚风,魏蔚.固相萃取净化-液相色谱串联质谱确证茶叶中的6种乙撑双二硫代氨基甲酸盐类农药残留[J].分析测试学报,2010,29(11). |
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| 作者姓名： | 祝伟霞 杨冀州 刘亚风 魏蔚 |
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| 作者单位： | 河南出入境检验检疫局; |
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| 基金项目： | 国家质检总局行业标准制修订计划资助项目 |
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| 摘 要： | 建立了液相色谱串联质谱法测定茶叶中代森锌、代森锰、代森锰锌、代森钠、代森联、甲基代森锌等6种乙撑双二硫代氨基甲酸盐类农药的确证方法。方法选用碱性乙二胺四乙酸二钠作为提取液,并将难溶盐转化为水溶性钠盐,甲酯化试剂碘甲烷进行衍生化反应,采用亲水-亲脂平衡固相萃取柱(Oasis HLB)净化甲酯化产物,甲醇洗脱,6.5min内衍生物在Sunfire C18色谱柱中完成分离,电喷雾正离子多反应监测模式下监测。茶叶中甲基代森锌的定量下限为20μg/kg,在5～200μg/kg范围内呈良好的线性关系;其它代森盐类化合物的定量下限均为10μg/kg,在2～200μg/kg范围内呈良好的线性关系;在绿茶、红茶和乌龙茶叶中添加不同水平待测物时,平均回收率为79%～99%,相对标准偏差为4.7%～14.6%。经验证该方法可简单、快速、准确地检测多种茶叶中的代森与甲基代森类农药残留。
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| 关 键 词： | 茶叶 代森类农药 二硫代氨基甲酸盐 残留 液相色谱串联质谱 |
Determination of 6 Ethylenebis Dithiocarbamates Residues in Tea by Liquid Chromatography Tandem Mass Spectrometry with Solid-phase Extraction Purification |
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| ZHU Wei-xia,YANG Ji-zhou,LIU Ya-feng,WEI Wei.Determination of 6 Ethylenebis Dithiocarbamates Residues in Tea by Liquid Chromatography Tandem Mass Spectrometry with Solid-phase Extraction Purification[J].Journal of Instrumental Analysis,2010,29(11). |
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| Authors: | ZHU Wei-xia YANG Ji-zhou LIU Ya-feng WEI Wei |
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| Institution: | ZHU Wei-xia,YANG Ji-zhou,LIU Ya-feng,WEI Wei(Henan Entry-Exit Inspection and Quarantine Bureau,Zhengzhou 450003,China) |
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| Abstract: | A new confirmative liquid chromatography-tandem mass spectrometric(LC-MS/MS) method was developed for the determination of six dithiocarbamate salts,including zineb,maneb,mancozeb,nabam,metiram and propineb in tea sample.The 6 analytes were extracted with an alkaline EDTA-Na2 solution.The extracts were transformed into water-soluble sodium salt compounds and derived with organic solvent methyl iodide(CH3I).The cleanup procedures were performed on a hydrophilic-lipophilic solid-phase extraction column(Oasis ... |
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| Keywords: | tea ethylenebis dithiocarbamates residues LC-MS/MS |
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