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Application of solid-phase microextraction/high-performance liquid chromatography mass spectrometry to forensic toxicology

固相微萃取/高效液相色谱质谱法在法医毒理学中的应用

基本信息

批准号：
10470122
负责人：
KUMAZAWA Takeshi
金额：
$ 6.46万
依托单位：
Showa University
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (B).
财政年份：
1998
资助国家：
日本
起止时间：
1998 至 2000
项目状态：
已结题

项目摘要

In forensic toxicology, the extraction, identification and quantification of a chemical (s) are essential in the case of victims whose case of death is considered due to or related to intoxication by drugs and poisons. The main interest in these fields is focused on methodologies, with regard to how rapidly, accurately and sensitively chemicals can be detected. In the present study, we established a procedure for the determination of stimulants, opioids, phenothiazines, butyrophenones, benzodiazepines, organophosphate pesticides, carbamate pesticides and naturally occurring poisons in human samples by solid-phase microextraction (SPME)-high performance liquid chromatography (HPLC)/mass spectrometry (MS).SPME was achieved with polydimethylsiloxane (PDMS) for stimulants or organophosphate pesticides, carbowax/divinylbenzene (DVB) for opioids, polyacrylate for phenothiazines or butyrophenones and PDMS/DVB for benzodiazepines, carbamate pesticides or amanitins from human whole blood, serum and urine samples. HPLC/MS with electrospray ionization (ESI) as interface and ionization mode was used for detection of all drugs and poisons, except for atmospheric pressure chemical ionization for detection of organophosphate pesticides. In the analysis of phenothiazines, butyrophenones and benzodiazepines, HPLC/tandem MS (MS/MS) showed much higher sensitivity than HPLC/MS.In addition to the spiked human body fluids, the method was applied to urine samples containing methamphetamine and amphetamine in a medico-legal case, and to samples of whole blood and urine after oral administration of phenothiazines by a male volunteer, these drugs could be isolated from human samples by SPME and sensitively quantified by HPLC/MS or HPLC/MS/MS.The present SPME-HPLC/MS method can be recommended for use in therapeutic monitoring, clinical toxicology and forensic toxicology.

在法医毒理学中，如果受害者的死亡被认为是由于药物和毒药中毒或与之有关，则必须提取、鉴定和确定化学品的数量。这些领域的主要兴趣集中在如何快速、准确和灵敏地检测化学品的方法上。建立了固相微萃取-高效液相色谱-质谱联用（SPME-HPLC-MS）检测人体样品中兴奋剂、阿片类、吩噻嗪类、丁酰苯酮类、苯二氮卓类、有机磷类、氨基甲酸酯类及天然毒物的方法。聚乙二醇/二乙烯基苯（DVB）用于阿片类药物，聚丙烯酸酯用于吩噻嗪或丁酰苯，PDMS/DVB用于苯并二氮杂卓类药物、氨基甲酸酯杀虫剂或鹅膏蕈碱。采用电喷雾离子化（ESI）为接口和离子化模式的高效液相色谱/质谱（HPLC/MS）对所有药物和毒物进行检测，但有机磷农药的检测采用常压化学离子化。在吩噻嗪、丁酰苯和苯二氮卓类药物的分析中，HPLC/串联MS（MS/MS）显示出比HPLC/MS高得多的灵敏度。除了加标的人体体液外，该方法还应用于法医案例中含有甲基苯丙胺和苯丙胺的尿液样品，以及男性志愿者口服吩噻嗪后的全血和尿液样品，该方法可用于临床毒理学、药物监测和法医毒理学研究。