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Screening of new abused drugs by Solid-Phase Microextraction

固相微萃取筛选新滥用药物

基本信息

批准号：
17590587
负责人：
HAMAJIMA Makoto
金额：
$ 2.36万
依托单位：
Fujita Health University
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (C)
财政年份：
2005
资助国家：
日本
起止时间：
2005 至 2007
项目状态：
已结题

项目摘要

In this report, we present a Solid-phase microextraction (SPME) method for determination of Organophosphate pesticides in human whole blood. The whole blood samples containing eight petsticides (dichlorvos, fenitnothion, malathion, fenthion, profenofos, isoxathion, ethion and phosalone) were heated at 50℃ in a septum-cappedvial in the presence of K_2CO_3, and an SPME fiber was exposed in the vial for 30 min. Immediately after withdrawal of the fiber, it was analyzed by gas chromatography with FPD (GC/FPD). Recoveries of the eight pesticides were 0.03-2.19%. The calibration curves for the pesticides showed linearity in the range of 25-400ng/0.5ml whole blood except for phosalone (200-800ng/0.5ml whole blood) with detection limits of 0.2-25ng/0.5ml whole blood except for phosalone (20ng/ 0.5ml whole blood).In conclusion, we have been able to extract and detect organophosphate pesticides in human whole bloods by use of the headspace SPME - GC/FPD. From the view points of simplicity, background noises, detection limit and quantitative, the present method can be recommended before analyses by GC in forenc, clinical, veterinary and environmental toxicology.We have devised a liquid-liquid extraction method for Triage DOA screening of the abused drugs in whole bloods. The drugs were extracted from the matrices by fluid-fluid extraction using diethyl ether. The dection limits were 10ng/ml(Phencyclidine), 90ng/ml (Alprazolam), 140ng/ml (Diazepam), 300ng/ml (Nitrazepam), 80ng/ml (triazolam), 520ng/ml (Amphetamine), 400ng/ml (Methamphetaniine), 300ng/ml (Morphine), 120ng/ml (Codeine), 60ng/ml (Pentobarbital), 100ng/ml (Barbital), 160ng/ml (Phenobarbital), 200ng/ml (Amitriptyline), 200ng/ml (Imipramine), 400ng/ml (Nortriptyline).In conclusion, our method is recommendable for the detection in forensic toxicology, because of its precision and sufficient sensitivity.

本文建立了固相微萃取（SPME）法测定全血中有机磷农药残留的方法。将含有敌敌畏、杀螟松、马拉硫磷、倍硫磷、丙溴磷、异恶硫磷、乙硫磷和伏杀隆等8种杀虫剂的全血样品在50℃、K_2CO_3存在下加热，将固相微萃取纤维在小瓶中暴露30 min，取出纤维后立即进行气相色谱-FPD（GC/FPD）分析。8种农药的回收率为0.03- 2.19%。除伏杀隆外，其它农药在25- 400 ng/0.5ml全血范围内线性关系良好（200- 800 ng/0.5 ml全血），除伏杀磷外，检测限为0.2- 25 ng/0.5 ml全血（20 ng/ 0.5ml全血）。总之，我们已经能够用顶空固相微萃取-气相色谱/火焰光度检测器（SPME-GC/FPD）提取和检测人全血中的有机磷农药。从方法简便、背景噪声、检出限和定量等方面考虑，本方法可推荐用于法医、临床、兽医和环境毒理学的GC分析前处理。使用乙醚通过液-液萃取从基质中萃取药物。检测限为10 ng/ml（苯环利定），90 ng/ml（阿普唑仑），140 ng/ml（地西泮），300 ng/ml（硝西泮），80 ng/ml（三唑仑），520 ng/ml（安非他明），400 ng/ml（甲基苯丙胺），300 ng/ml（吗啡）、120 ng/ml（可待因）、60 ng/ml（戊巴比妥），100 ng/ml（巴比妥），160 ng/ml（苯巴比妥），200 ng/ml（阿米替林），200 ng/ml结果表明，该方法具有较高的灵敏度和精密度，可用于法医毒理学检测。