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建立并应用 GC-MS 方法监测长期接触杀虫剂氯菊酯

Development and application of GC-MS method for monitoring of long-term exposure to the pesticide cypermethrin.

机构信息

Center of Toxicology Science & Research, Medical School, University of Crete, Heraklion, Crete, 71409, Greece.

出版信息

Drug Test Anal. 2014 Jun;6 Suppl 1:9-16. doi: 10.1002/dta.1601.

Abstract

Cypermethrin (CPMN) is a synthetic pyrethroid used as an insecticide in large-scale commercial agricultural applications as well as for domestic purposes. In the present study a gas chromatography-mass spectrometry (GC-MS) based method was developed and validated for the quantitation of CPMN metabolites, 3-phenoxybenzoic acid (3-PBA) and cis- and trans- 3-(2,2-dichlorovinyl)-2,2-dimethyl-1-cyclopropane (cis- and trans- Cl2 CA). The developed method was applied for the monitoring of CPMN metabolites in hair of laboratory animals (rabbits) intentionally exposed per os to CPMN at 40 (low dose) and 80 (high dose) mg/kg weight/day for 16 weeks. The analytical method comprises three main steps: isolation of analytes from hair, analytes derivatization, and subsequent instrumental analysis by GC-MS. The limits of detection ensured by the method are 4.0, 3.9 and 1.0 pg/mg hair for cis-Cl2 CA, trans-Cl2 CA and 3-PBA, respectively. The instrument responce is linear (r(2)  > 0.99) in the investigated concentrations range from 25 to 1000 pg/mg. With and between-run precision as well as accuracy were estimated and found satisfactory. Analytes were efficiently isolated by solid-liquid extraction from hair with recoveries greater than 84.8% for cis-Cl2 CA, 87.2% for trans-Cl2 CA and 96.4% for 3-PBA. Rabbit's hair showed increasing levels for all metabolites (metabolites accumulation in a time and dose dependent manner) over time and in a dose-dependent manner. The developed experimental procedure could be used for biomonitoring of population exposure to CPMN.

摘要

氯菊酯(CPMN)是一种合成拟除虫菊酯,被广泛用于大规模商业农业应用以及家庭用途的杀虫剂。本研究建立并验证了一种基于气相色谱-质谱(GC-MS)的方法,用于定量检测 CPMN 代谢物 3-苯氧基苯甲酸(3-PBA)和顺式及反式 3-(2,2-二氯乙烯基)-2,2-二甲基-1-环丙烷(顺式和反式 Cl2 CA)。该方法应用于监测经口摄入 40(低剂量)和 80(高剂量)mg/kg/天的 CPMN 后 16 周的实验室动物(兔子)毛发中的 CPMN 代谢物。分析方法包括三个主要步骤:从毛发中分离分析物、分析物衍生化以及随后通过 GC-MS 进行仪器分析。该方法的检测限分别为 cis-Cl2 CA、trans-Cl2 CA 和 3-PBA 的 4.0、3.9 和 1.0 pg/mg 毛发。仪器响应在 25 至 1000 pg/mg 的研究浓度范围内呈线性(r(2)  > 0.99)。批内和批间精密度和准确度均令人满意。顺式-Cl2 CA 的回收率大于 84.8%,反式-Cl2 CA 的回收率大于 87.2%,3-PBA 的回收率大于 96.4%,分析物通过固相萃取从毛发中有效分离。随着时间的推移和剂量的增加,所有代谢物的水平均升高(代谢物呈时间和剂量依赖性积累)。所建立的实验程序可用于监测人群接触 CPMN 的情况。

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