色谱

色谱 ›› 2012, Vol. 30 ›› Issue (04): 419-422.

• 特别策划 • 上一篇    下一篇

离子色谱法检验尸体心血中草甘膦

王勇1, 吴波1, 连厚彬2, 施超欧3*   

  1. 1. 南京市公安局刑事科学技术研究所, 江苏 南京 210001; 2. 南京市公安局鼓楼分局, 江苏 南京 210036; 3. 华东理工大学分析测试中心, 上海 200237
  • 收稿日期:2011-12-19 修回日期:2012-02-26 出版日期:2012-04-28 发布日期:2012-04-28
  • 通讯作者: 施超欧,高级工程师,主要研究方向为离子色谱及液相色谱的应用研究

Determination of glyphosate in heart blood of corpse by ion chromatography

WANG Yong1, WU Bo1, LIAN Houbin2, SHI Chaoou3*   

  1. 1. Institute of Forensic Science and Technology of Nanjing Public Security Bureau, Nanjing 210001, China; 2. Gulou Substation of Nanjing Public Security Bureau, Nanjing 210036, China; 3. Analysis and Research Center, East China University of Science and Technology, Shanghai 200237, China
  • Received:2011-12-19 Revised:2012-02-26 Online:2012-04-28 Published:2012-04-28

PDF

296

被引次数

24

摘要： 建立了离子色谱检测人血中草甘膦的方法。血液样品使用乙腈沉淀蛋白质,离心后取上清液过Dionex OnGuard II RP 柱和Dionex OnGuard IIAg柱后,经IonPac AS-19阴离子色谱柱(25 mm×4 mm)分离,用KOH淋洗液自动发生器(EG)进行梯度淋洗,抑制器采用外加水模式,电导检测器检测。结果表明,草甘膦在10～100 mg/L范围内线性关系良好(相关系数r2=0.9999)。以信噪比(S/N)为3确定方法检出限为0.12 mg/L,以S/N=10确定方法定量限为0.39 mg/L;方法回收率为95.2%～109.1%,相对标准偏差(n=5)为1.2%～3.7%,检测实发案件中死者心血中草甘膦质量浓度为508 mg/L。该方法操作简便,结果准确,适用于血中草甘膦的定量检测,能快速为案件的侦破提供可靠的线索和依据,可满足公安工作的需要。

关键词: 草甘膦, 电导检测, 离子色谱法, 尸体, 心血

Abstract: A method for the determination of glyphosate in human blood by ion chromatography was established. The protein in heart blood from a corpse was precipitated with acetonitrile. The large molecules and Cl~in the supernatant were removed by a Dionex OnGuard II RP column and a Dionex OnGuard II Ag column, respectively. The filtrate was separated on an IonPac AS-19 column with KOH solution as eluent produced online by an eluent generator (EG). A suppressor with external water mode and a conductivity detector for the detection were used. The linear range of this method was 10~100 mg/L with a correlation coefficient (r2) of 0.999 9. The limits of detection (LOD, S/N=3) and quantification (LOQ, S/N=10) of glyphosate in blood were 0.12 mg/L and 0.39 mg/L, respectively. The recoveries ranged between 95.2%~109.1% with the relative standard deviations (RSDs, n=5) of 1.2%~3.7%. The glyphosate content in a heart blood sample from a corpse in an actual case was 508 mg/L detected by this method. This method is simple, sensitive, accurate, and can rapidly provided reliable clues and evidences for glyphosate poisoning cases. This method can meet the needs of public security work.

Key words: conductivity detection, corpse, glyphosate, heart blood, ion chromatography (IC)