色谱

色谱 ›› 2013, Vol. 31 ›› Issue (12): 1167-1175.DOI: 10.3724/SP.J.1123.2013.05051

• 研究论文 • 上一篇    下一篇

基于QuEChERS提取方法优化的液相色谱-串联质谱法测定蔬菜中51种氨基甲酸酯类农药残留

王连珠1, 周昱2, 黄小燕1, 王瑞龙1, 林子旭1, 陈泳1, 王登飞1, 林德娟3, 徐敦明2   

  1. 1. 漳州出入境检验检疫局, 福建 漳州 363100;
    2. 厦门出入境检验检疫局, 福建 厦门 361012;
    3. 漳州师范学院, 福建 漳州 363000
  • 收稿日期:2013-05-30 修回日期:2013-07-25 出版日期:2013-12-28 发布日期:2013-12-05
  • 通讯作者: 王连珠
  • 基金资助:

    福建省自然科学基金项目（2011J01386）

Determination of 51 carbamate pesticide residues in vegetables by liquid chromatography-tandem mass spectrometry based on optimization of QuEChERS sample preparation method

WANG Lianzhu1, ZHOU Yu2, HUANG Xiaoyan1, WANG Ruilong1, LIN Zixu1, CHEN Yong1, WANG Dengfei1, LIN Dejuan3, XU Dunming2   

  1. 1. Zhangzhou Entry-Exit Inspection and Quarantine Bureau, Zhangzhou 363100, China;
    2. Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361012, China;
    3. Zhangzhou Normal University, Zhangzhou 363000, China
  • Received:2013-05-30 Revised:2013-07-25 Online:2013-12-28 Published:2013-12-05

PDF

352

被引次数

114

摘要：

采用气相色谱-质谱（GC-MS）全扫描结合NIST谱库检索方法分析6种蔬菜（番茄、青刀豆、大葱、青花菜、姜、胡萝卜）提取液中的基质干扰物，以蒸发残渣重量法探讨乙二胺N-丙基硅烷（PSA）、十八烷基硅烷（C18）及两者组合对6种蔬菜提取液基质干扰物的净化效果及吸附机理，考察了原创QuEChERS方法及AOAC 2007.01方法对蔬菜中51种氨基甲酸酯类农药提取的适用性，并建立了液相色谱-串联质谱法测定蔬菜中51种氨基甲酸酯类农药残留的方法。结果表明，C18与PSA组合进行分散固相萃取的净化效果最好；AOAC 2007.01方法适用于二氧威以外的50种农药残留的提取，而原创QuEChERS方法对二氧威残留的提取可获得满意结果。经电喷雾正离子电离及多反应监测模式来测定目标化合物，采用基质匹配标准溶液曲线法进行定量。结果表明：51种农药在6种基质中3个添加水平（10、20、100 μg/kg）的回收率为58.4%~126%，相对标准偏差为3.3%~26%；以信噪比（S/N）≥10计，久效威及杀螟丹的定量限（LOQ）为50 μg/kg，其他49种农药的LOQ为0.2~10 μg/kg。本文方法有效、灵敏，适用于不同蔬菜基质中51种氨基甲酸酯类农药残留的测定。

关键词: QuEChERS, 氨基甲酸酯类农药, 气相色谱-质谱, 蔬菜, 液相色谱-串联质谱, 蒸发残渣

Abstract:

The raw extracts of six vegetables (tomato, green bean, shallot, broccoli, ginger and carrot) were analyzed using gas chromatography-mass spectrometry (GC-MS) in full scan mode combined with NIST library search to confirm main matrix compounds. The effects of cleanup and adsorption mechanisms of primary secondary amine (PSA), octadecylsilane (C18) and PSA+C18 on co-extractives were studied by the weight of evaporation residue for extracts before and after cleanup. The suitability of the two versions of QuEChERS method for sample preparation was evaluated for the extraction of 51 carbamate pesticides in the six vegetables. One of the QuEChERS methods was the original un-buffered method published in 2003, and the other was AOAC Official Method 2007.01 using acetate buffer. As a result, the best effects were obtained from using the combination of C18 and PSA for extract cleanup in vegetables. The acetate-buffered version was suitable for the determination of all pesticides except dioxacarb. Un-buffered QuEChERS method gave satisfactory results for determining dioxacarb. Based on these results, the suitable QuEChERS sample preparation method and liquid chromatography-positive electrospray ionization-tandem mass spectrometry under the optimized conditions were applied to determine the 51 carbamate pesticide residues in six vegetables. The analytes were quantified by matrix-matched standard solution. The recoveries at three levels of 10, 20 and 100 μg/kg spiked in six vegetables ranged from 58.4% to 126% with the relative standard deviations of 3.3%-26%. The limits of quantification (LOQ, S/N≥10) were 0.2-10 μg/kg except that the LOQs of cartap and thiofanox were 50 μg/kg. The method is highly efficient, sensitive and suitable for monitoring the 51 carbamate pesticide residues in vegetables.

Key words: carbamate pesticide, evaporation residue, gas chromatography-mass spectrometry (GC-MS), liquid chromatography-tandem mass spectrometry (LC-MS/MS), QuEChERS, vegetable

中图分类号: