Screening of new abused drugs by Solid-Phase Microextraction

建立了固相微萃取（SPME）法测定人全血中有机磷农药的方法。将含有敌敌畏、杀虫硫磷、马拉硫磷、倍硫磷、异硫磷、乙硫磷、磷沙酮等8种农药的全血样本，在K_2CO_3存在下，于50℃下置于隔盖瓶中加热，SPME纤维在瓶中暴露30min。提取纤维后立即进行气相色谱- FPD （GC/FPD）分析。加样回收率为0.03 ~ 2.19%。除磷沙酮（200 ~ 800ng/0.5ml）外，其余农药在25 ~ 400ng/0.5ml全血范围内呈线性，检出限为0.2 ~ 25ng/0.5ml全血，磷沙酮（20ng/ 0.5ml）除外。综上所述，我们可以利用顶空SPME - GC/FPD提取和检测人全血中的有机磷农药。该方法具有简便、背景噪声、检出限和定量等优点，可在法医、临床、兽医和环境毒理学等领域的气相色谱分析前推荐使用。我们设计了一种液-液萃取法，用于全血中滥用药物的检出DOA筛选。采用二乙醚液液萃取法从基质中提取药物。检出限分别为10ng/ml（苯环利定）、90ng/ml（阿普唑仑）、140ng/ml（地西泮）、300ng/ml（硝西泮）、80ng/ml（三唑仑）、520ng/ml（安非他明）、400ng/ml（甲基苯丙胺）、300ng/ml（吗啡）、120ng/ml（可待因）、60ng/ml（戊巴比妥）、100ng/ml（巴比妥）、160ng/ml（苯巴比妥）、200ng/ml（阿米替林）、200ng/ml（丙咪嗪）、400ng/ml（去甲替林）。结果表明，该方法具有较高的灵敏度和准确性，可用于法医毒理学检测。

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.