分析与检测

QuEChERS-气相色谱分析厦门海域鱼体中有机氯类农药残留特征及风险评价

  • 毕思远 ,
  • 曹建涛 ,
  • 李保玲 ,
  • 朱志强 ,
  • 曹涛 ,
  • 李森
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  • 1 (哈尔滨体育学院,黑龙江 哈尔滨,150008)
    2 (济南市农产品质量检测中心,山东 济南,250000)
    3 (广东省检迅检测科技有限公司,广东 东莞,523843)
    4 (深圳市汇知科技有限公司,广东 深圳,518000)
博士,副研究员(朱志强教授为通讯作者,E-mail:alix_bi0129@foxmail.com)。

收稿日期: 2019-02-19

  网络出版日期: 2019-11-15

基金资助

国家博士后基金面上项目二等资助(2017M611382)

Determination and risk assessment of organochlorine pesticides in marine fishfrom Xiamen sea area by QuEChERS combined with gas chromatography

  • BI Siyuan ,
  • CAO Jiantao ,
  • LI Baoling ,
  • ZHU Zhiqiang ,
  • CAO Tao ,
  • LI Sen
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  • 1 (Harbin Sport University, Harbin 150008, China)
    2 (Test Center for Agri-products Quality of Jinan, Jinan 250000, China)
    3 (Guangdong Quick Test Technologies Co. Ltd., Dongguan 523843, China)
    4 (Shenzhen Huizhi Technologies Co.Ltd., Shenzhen 518000, China)

Received date: 2019-02-19

  Online published: 2019-11-15

摘要

以厦门海域10种鱼类作为研究对象,利用QuEChERS-气相色谱分析鱼肉中有机氯农药(organochlorine pesticides, OCPs)的残留水平和特征,并探讨其可能的健康风险。样品经V(正己烷)∶V(丙酮)=1∶1提取,经400 mg PSA,150 mg C18和900 mg无水MgSO4净化,采用气相色谱定性和定量分析,结合气相色谱-质谱法确认。各OCPs在1~50 μg/L质量浓度范围内线性相关系数均大于0.998 8,回收率为83.2%~103.5%,精密度为4.8%~12.1%,检出限0.01~0.09 μg/kg;10种鱼类均有OCPs检出,含量在5.532~22.174 μg/kg之间,带鱼和鳓鱼的OCPs含量最高,分别为22.174 μg/kg和19.910 μg/kg;P’P’-DDD、P’P’-DDE和β-HCH是最主要的OCPs污染物;各异构体的含量水平和组成特征表明该水域的OCPs大部分来自早期农药使用残留,但疑似有三氯杀螨醇引入的DDT污染;估计每日膳食摄入量(estimated daily intake, EDI)均远低于国标规定值。QuEChERS可以应用于大批量水产品中OCPs的检测分析,厦门海域的水环境近期受OCPs污染较小,食用该水域的鱼类产生OCPs危害的风险较低。

本文引用格式

毕思远 , 曹建涛 , 李保玲 , 朱志强 , 曹涛 , 李森 . QuEChERS-气相色谱分析厦门海域鱼体中有机氯类农药残留特征及风险评价[J]. 食品与发酵工业, 2019 , 45(21) : 229 -235 . DOI: 10.13995/j.cnki.11-1802/ts.020240

Abstract

With 10 fish species in Xiamen area as the research objects, the residue dose and characteristics of organochlorine pesticides (OCPs) in fish were analyzed by QuEChERS-gas chromatography, and their possible health risks were discussed. Fish muscles were extracted with hexane and acetone (1∶1) homogenate and purified with 400 mg PSA, 150 mg C18 and 900 mg magnesium sulfate, followed by GC-ECD and GC-MS analysis. The results showed that the calibration curves were linear in the range of 1-50 ìg/L for each OCP, with correlation coefficients all above 0.998 8, the average recoveries of 83.2%-103.5%, the RSDs of 4.8-12.1%, and the detection limits of 0.01-0.09 μg/kg. Meanwhile, OCPs were detected in all 10 fish species, with the concentrations ranging from 5.532 μg/kg to 22.174 μg/kg. The concentrations of OCPs in Trichiurus lepturus and Ilisha elongata Bennett were the highest, reaching 22.174 μg/kg and 19.910 μg/kg, respectively. P′P′-DDD, P′P′-DDE and â-HCH were the main pollutants. The contents and composition of the isomers indicated that most of the OCPs in Xiamen area were come from early pesticide residues, but there was a suspected contamination of DDT caused by the degradation of dicofol. However, the EDI was far lower than daily food intake from the national standard. Therefore, QuEChERS can be applied to the detection of OCPs in marine fish, and the water environment in Xiamen sea area has been less polluted by OCPs recently, indicating low risk of OCPs by fish consumption.

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