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人死后全血、尿液及马尿液中β受体阻滞剂的固相萃取和衍生化方法

Solid-phase extraction and derivatisation methods for beta-blockers in human post mortem whole blood, urine and equine urine.

作者信息

Black S B, Stenhouse A M, Hansson R C

机构信息

Chemistry Centre (WA), East Perth, Australia.

出版信息

J Chromatogr B Biomed Appl. 1996 Oct 11;685(1):67-80. doi: 10.1016/0378-4347(96)00140-5.

DOI:10.1016/0378-4347(96)00140-5
PMID:8930755
Abstract

This paper details various rapid and sensitive methods for the extraction and derivatisation of propranolol, metoprolol, sotalol, atenolol, pindolol, timolol, oxprenolol, alprenolol and penbutolol in equine urine and in human post mortem whole blood and urine. Three solid-phase extraction methods are described involving the use of either XtrackT XRDAH515, Bond Elut Certify or Sep-Pak C18 cartridges. Two derivatisation methods are also described involving the formation of cyclised silyl or pentafluoropropionate derivatives with either chloromethyldimethylchlorosilane or pentafluoropropionic anhydride, respectively. Gas chromatographic-mass spectrometry analysis was carried out in select-ion monitoring mode. All these methods were evaluated using drug-free human post mortem blood, urine and equine urine fortified at various levels with the beta-blockers mentioned above. The application of some of these methods on a forensic case study is also presented. This work does not include samples from equine administration trials of beta-blockers.

摘要

本文详细介绍了多种快速灵敏的方法,用于从马尿、人死后全血及尿液中提取和衍生普萘洛尔、美托洛尔、索他洛尔、阿替洛尔、吲哚洛尔、噻吗洛尔、氧烯洛尔、阿普洛尔和喷布洛尔。文中描述了三种固相萃取方法,分别涉及使用XtrackT XRDAH515、Bond Elut Certify或Sep - Pak C18柱。还介绍了两种衍生方法,分别是与氯甲基二甲基氯硅烷或五氟丙酸酐形成环化硅烷基或五氟丙酸酯衍生物。采用选择离子监测模式进行气相色谱 - 质谱分析。所有这些方法均使用不含上述β受体阻滞剂的人死后血液、尿液以及添加了不同水平上述β受体阻滞剂的马尿进行评估。本文还介绍了其中一些方法在一个法医案例研究中的应用。这项工作不包括来自β受体阻滞剂马给药试验的样本。

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