离子色谱法检验尸体心血中草甘膦

Determination of glyphosate in heart blood of corpse by ion chromatography

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 On-GuardⅡRP柱和Dio nex OnGuardⅡAg柱后,经Io nPac AS-19阴离子色谱柱(25 m m×4 m m)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10～100m g/L范围内线性关系良好(相关系数r2=0.999 9)。以信噪比(S/N)为3确定方法检出限为0.12 m g/L,以S/N=10确定方法定量限为0.39 m g/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。

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.