法医学杂志

法医学杂志 ›› 2018, Vol. 34 ›› Issue (4): 379-383.DOI: 10.12116/j.issn.1004-5619.2018.04.007

• 论著 • 上一篇    下一篇

GC-MS/MS法检测生物样品中硫丹含量

张  帆1，乔君元2，禹明筠1，贾  娟1，曹  洁1，张  潮1，崔海燕1，贠克明1，尉志文1   

  1. 1. 山西医科大学法医学院，山西 太原 030024； 2. 太原市公安局，山西 太原 030024
  • 发布日期:2018-08-25 出版日期:2018-08-28
  • 通讯作者: 尉志文，男，博士，硕士研究生导师，主要从事法医毒物学研究；E-mail：weizhiwen2000@163.com
  • 作者简介:张帆（1993—），男，硕士研究生，主要从事法医毒物学研究；E-mail：dennis112233@163.com
  • 基金资助:
    国家重点研发计划资助项目（2017YFC0803504，2017YFC0800704）；国家科技基础专项资助项目（SQ2015FYJ010051）；山西省科技攻关资助项目（20130313020-2）；山西省回国留学人员科研资助项目（2014-032）

Determination of Endosulfan Concentrations in Biological Samples by GC-MS/MS

ZHANG Fan1, QIAO Jun-yuan2, YU Ming-jun1, JIA Juan1, CAO Jie1, ZHANG Chao1, CUI Hai-yan1, YUN Ke-ming1, WEI Zhi-wen1   

  1. 1. School of Forensic Medicine, Shanxi Medical University, Taiyuan 030024, China; 2. Taiyuan Public Security Bureau, Taiyuan 030024, China
  • Online:2018-08-25 Published:2018-08-28

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摘要： 目的 建立生物样品中硫丹（α硫丹和β硫丹）的气相色谱-串联质谱（GC-MS/MS）检测方法，观察硫丹在水生动物体内的分布，为相关案件的法医学鉴定提供实验依据。 方法 血液和肌肉样品采用乙腈沉淀蛋白，GC-MS/MS法检测，多反应监测模式扫描，以保留时间和离子比例定性，外标工作曲线法定量。 结果 血液样品中α硫丹和β硫丹在0.062 5~10 μg/mL范围内线性关系良好，相关系数（r）均大于0.99，检出限分别为1 ng/mL和2 ng/mL，定量限分别为4 ng/mL和8 ng/mL。肌肉样品中α硫丹和β硫丹在0.062 5~10 μg/g范围内线性关系良好，相关系数（r）均大于0.98，检出限分别为1 ng/g和4 ng/g，定量限分别为4 ng/g和16 ng/g。血液和肌肉样品中α硫丹和β硫丹的准确度为90.76%~108.91%，日内精密度（RSD）为2.35%~8.71%，日间精密度（RSD）为5.44%~10.29%。中毒案件中，在鱼和螃蟹体内各部位均检出硫丹，且不同部位间含量差异均具有统计学意义。 结论 本研究建立的硫丹GC-MS/MS检测方法快捷、准确、灵敏，适用于微量生物检材中硫丹的检测。硫丹在鱼和螃蟹体内分布不均匀，为硫丹相关法医学鉴定案件中毒物分析检材的采集和分析提供了依据。

关键词: 法医毒理学, 硫丹, 中毒, 气相色谱-质谱法, 生物样品

Abstract: Objective To establish an analytical method of the endosulfan concentrations （α-endosulfan and β-endosulfan） in biological samples by GC-MS/MS. To observe the distribution of endosulfan in aquatic animals and provide experimental evidence for forensic identification of relevant cases. Methods Acetonitrile was added to the blood and muscle samples for precipitating the protein. The endosulfan concentrations were determined by GC-MS/MS in multiple reaction monitoring mode. Qualitative analysis was performed according to the retention time and ion rate, and quantitative analysis was performed by external standard working curve method. Results In blood samples, the calibration curves of α-endosulfan and β-endosulfan ranging from 0.062 5 to 10 μg/mL had good linear relationship, the correlation coefficients （r） of which were >0.99. The limits of detection （LOD） were 1 ng/mL and 2 ng/mL and the limits of quantification （LOQ） were 4 ng/mL and 8 ng/mL, respectively. In muscle samples, the calibration curves of α-endosulfan and β-endosulfan ranging from 0.062 5 to 10 μg/g, the r of which were >0.98. The LOD were 1 ng/g and 4 ng/g and the LOQ were 4 ng/g and 16 ng/g, respectively. The accuracy of α-endosulfan and β-endosulfan was 90.76%-108.91% both in blood and muscle samples, the interday and intraday precision were 2.35%-8.71% and 5.44%-10.29%, respectively. In poisoning cases, endosulfan were detected in all parts of fish and crab and the content difference was statistically significant. Conclusion The endosulfan detection method based on GC-MS/MS established in the present study is rapid, sensitive and accurate, which can be applied to the endosulfan detection in traces biological samples. The distribution of endosulfan in fish and crab was different, which can provide evidence to the sample collection and analysis for toxicological analysis in relevant forensic identification.

Key words: forensic toxicology, endosulfan, poisoning, gas chromatography-mass spectrometry, biological samples