Determination of Amide Herbicides and Their Metabolites by GC－MS in Aquatic Products

PENG Zhong-xiao; ZHANG Hua-wei; LI Jia-wei; GONG Xiang-hong; ZHANG Xiu-zhen; XU Ying-jiang; WANG Dan; LIU Yong-chun

doi:10.19969/j.fxcsxb.21070202

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Determination of Amide Herbicides and Their Metabolites by GC－MS in Aquatic Products

Experimental Techniques and Methods | 更新时间：2022-07-01

- Determination of Amide Herbicides and Their Metabolites by GC－MS in Aquatic Products
- Journal of Instrumental Analysis Vol. 41, Issue 3, Pages: 403-408(2022)
- 作者机构：
  
  1.上海海洋大学食品学院，上海 201306
  2.山东省海洋资源与环境研究院，山东烟台 264006
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.21070202
  CLC：
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彭中校,张华威,李佳蔚等.水产品中酰胺类除草剂及其代谢物的气相色谱－质谱法测定[J].分析测试学报,2022,41(03):403-408.

PENG Zhong-xiao,ZHANG Hua-wei,LI Jia-wei,et al.Determination of Amide Herbicides and Their Metabolites by GC－MS in Aquatic Products[J].Journal of Instrumental Analysis,2022,41(03):403-408.
彭中校,张华威,李佳蔚等.水产品中酰胺类除草剂及其代谢物的气相色谱－质谱法测定[J].分析测试学报,2022,41(03):403-408. DOI： 10.19969/j.fxcsxb.21070202.

PENG Zhong-xiao,ZHANG Hua-wei,LI Jia-wei,et al.Determination of Amide Herbicides and Their Metabolites by GC－MS in Aquatic Products[J].Journal of Instrumental Analysis,2022,41(03):403-408. DOI： 10.19969/j.fxcsxb.21070202.

摘要

建立了同时测定水产品中5种酰胺类除草剂（乙草胺、甲草胺、异丙甲草胺、丁草胺、丙草胺）及其代谢物2-甲基-6-乙基苯胺（MEA）、2， 6-二乙基苯胺（DEA）的气相色谱－质谱联用（GC－MS）分析方法。样品经二氯甲烷－乙酸乙酯（3∶2，体积比）混合溶剂提取，正己烷洗脱后进行GC－MS检测。在优化检测条件下，MEA、DEA、异丙甲草胺在1.0～25 μg/L质量浓度范围内，其余4种目标物在2.0～50 μg/L质量浓度范围内与其响应值线性关系良好，相关系数（,r,2,）均不低于0.998 8。在低、中、高3个加标水平下，四角蛤蜊的回收率为69.7%～111%，相对标准偏差（RSD）为0.40%～7.6%；许氏平鮋和三疣梭子蟹的回收率分别为65.3%～118%、61.4%～113%，RSD分别为1.7%～9.3%、0.90%～7.1%。MEA、DEA、异丙甲草胺的检出限和定量下限分别为0.5、1.5 μg/kg，其余4种农药的检出限、定量下限分别为1.0、3.0 μg/kg。用该方法检测山东省沿海海域的四角蛤蜊、大菱鲆、中国对虾和半滑舌鳎样品，在一份四角蛤蜊样品中检出代谢物MEA，检出率为2.5%。该方法灵敏度、精密度均满足农药残留检测要求，适用于水产品中5种酰胺类除草剂及其代谢物的残留检测。

Abstract

A method was established for the simultaneous determination of 5 amide herbicides，i.e. acetochlor，alachlor，metolachlor，butachlor and pretilachlor，as well as their metabolites including 2-ethyl-6-methylaniline（MEA） and 2， 6-diethylaniline and（DEA） in aquatic products by gas chromatography－mass spectrometry（GC－MS）．Based on previous studies，the pretreatment conditions and chromatographic conditions were optimized in this paper．The appropriate characteristic ions were selected to achieve the chromatographic separation and determination for five amide herbicides and their metabolites in aquatic products．In the sample pretreatment，the mixing parameters for the extractant were optimized，the appropriate eluent and elution volume were selected，and the heating program for the chromatographic column was optimized to make the separation effect better．Specific method and process were as following：the sample was firstly extracted with dichloromethane－ethyl acetate（3∶2，by volume），then concentrated with nitrogen blowing，purified by HLB solid phase extraction，eluted with 3 mL ,n,-hexane，and finally quantified by GC－MS detection．Results showed that，after optimizing the detection conditions，there were good linear response values in the mass concentration range of 1.0－25 μg/L for MEA，DEA and metolachlor，and 2.0－50 μg/L for the other four herbicides．Meanwhile，the correlation coefficients（,r,2,） were greater than 0.998 8．The spiked recoveries for ,Mactraveneriformis ,at low，medium and high levels,ranged from 69.7% to 111%，with the relative standard deviations（RSDs） of 0.40%－7.6%．The recoveries for ,Sebastes schlegelii, ranged from 65.3% to 118%，with the RSDs of 1.7%－9.3%．The recoveries for ,Portunustrituberculatus, ranged from 61.4% to 113%，with the RSDs of 0.90%－7.1%．The limits of detection（LODs） and limits of quantification（LOQs） for MEA，DEA and metolachlor were 0.5 μg/kg and 1.5 μg/kg，respectively．The LODs and LOQs for the remaining four herbicides were 1.0 μg/kg and 3.0 μg/kg，respectively．This method was used to detect ,Mactraveneriformis,，,Scophthalmus maximus,，,Fenneropenaeuschinensis, and ,Cynoglossussemilaevis, samples in the coastal waters of Shandong Province．The metabolite MEA was detected in one of the ,Mactraveneriformis, samples with a detection rate of 2.5%．The sensitivity and precision of this method could meet the requirements for pesticide residue detection，and was suitable for the detection on 5 kinds of amide herbicides and their metabolites in aquatic products．

关键词

气相色谱－质谱酰胺类除草剂水产品农药残留

Keywords

gas chromatography－mass spectrometry（GC－MS）amide herbicidesaquatic productspesticide residues

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