法医学杂志

法医学杂志 ›› 2015, Vol. 31 ›› Issue (1): 41-43.DOI: 10.3969/j.issn.1004-5619.2015.01.010

• 技术与应用 • 上一篇    下一篇

SPE-GC/MS法分析鱼塘水中的5种农药

蔺大伟1，张  艳2，孙红雷1，李文海1，邵  凯1   

  1. （1． 泰安市公安局刑警支队刑事科学技术研究所，山东 泰安 271000； 2. 泰安市公安局泰山区分局刑事科学技术室，山东 泰安 271000）
  • 发布日期:2015-02-25 出版日期:2015-02-28
  • 作者简介:蔺大伟（1976—），男，山东菏泽人，工程师，主要从事毒物毒品分析研究；E-mail：lindawei1976@163.com

Determination of Five Pesticides in Fishpond by SPE-GC/MS

LIN DA-WEI1, ZHANG YAN2, SUN HONG-LEI1, LI WEN-HAI1, SHAO KAI1   

  1. （1. Institute of Criminal Science and Technology, Criminal Police Branch, Taian Public Security Bureau, Taian 271000, China; 2. Department of Criminal Science and Technology, Taishan Branch of Taian Public Security Bureau, Taian 271000, China）
  • Online:2015-02-25 Published:2015-02-28

被引次数

1

摘要： 目的 建立鱼类中毒案件中鱼塘水5种农药的固相萃取（solid phase extraction，SPE）结合气相色谱-质谱联用仪（GC/MS）的检测方法。 方法 比较Oasis HLB cartridge、Bond Elut C18和SampliQ C18 3种固相萃取柱提取、净化鱼塘水中5种农药的提取回收率，并考察洗脱剂种类、洗脱剂用量对提取回收率的影响。 结果 利用Bond Elut C18固相萃取柱，以3 mL苯作为洗脱剂，鱼塘水中5种农药质量浓度在1～50 μg/mL范围内有良好的线性关系，相关系数为0.996 2~0.999 6，测得的检出限为3.4～26 μg/L，提取回收率为61.49%~102.48%，相对标准偏差均≤3.01%。 结论 SPE-GC/MS法灵敏度高、准确度和精密度好，简单快速，溶剂消耗量少，适用于鱼塘水中5种农药的检测。

关键词: 法医毒理学, 农药, 气相色谱-质谱法, 固相萃取

Abstract: Objective To establish the solid phase extraction （SPE） with GC/MS technology for fish poisoning cases to determine five pesticides in fishpond. Methods By three solid phase extraction column including Oasis HLB cartridge, Bond Elut C18 and SampliQ C18, the recovery rate was compared to extract and purify five pesticides in fishpond. The effects of different kinds and dosages of eluents on extract rate were also reviewed. Results Using Bond Elut C18 as solid phase extraction column and 3 mL benzene as eluent, the linear range of mass concentration of five pesticides in fishpond was 1-50 μg/mL, and the correlation coefficient was 0.996 2-0.999 6. The limit of detection was 3.4-26 μg/L and the recovery was 61.49%-102.48%. The relative standard deviations was less than or equal to 3.01%. Conclusion With high sensitivity, good accuracy and precision, SPE-GC/MS has simple and quick operation and less solvent. It can be applied to determination of five pesticides in fishpond.

Key words: forensic toxicology, pesticides, gas chromatography-mass spectrometry, solid phase extraction

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