Fatal intoxications by acenocoumarol, phenprocoumon and warfarin: method validation in blood using the total error approach.

Raphaël Denooz, Zoénabo Douamba, Corinne Charlier
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引用次数: 21

Abstract

A simple high-performance liquid chromatography (HPLC) method with ultraviolet (UV) detection has been developed and validated for simultaneous identification and quantification of three antivitamin K drugs (acenocoumarol, warfarin and phenprocoumon) in whole blood. The aim of this development was to propose an analytical technique adapted to the situations of forensic toxicology, i.e. intoxication with massive anticoagulant doses, when the usual coagulation tests could not be used. The blood sample, after spiked with prazepam as an internal standard (IS), was submitted to a liquid-liquid extraction (LLE) prior to HPLC analysis. A chromatographic separation was achieved on a C8 Symmetry column with a mobile phase consisting of an acetonitrile and phosphate buffer (pH 3.8) mixture in a gradient mode. Detection was carried out at a wavelength between 200 and 400 nm. This method has been validated with the concept of total error as decision criterion. Trueness ranged from 99.1% to 105.0% and precision was good with RSD between 1.3% and 6.7%. Consequently, this rapid and simple chromatographic technique is well adapted to focus intoxications with most important coumarinic drugs available on pharmaceutical market and is now routinely used in our laboratory for forensic "general unknown" screening.

阿塞诺古豆醇、苯丙酚和华法林致死性中毒:全误差法在血液中的方法验证。
建立了一种简便的紫外检测高效液相色谱(HPLC)方法,用于同时鉴定和定量全血中3种抗维生素K药物(阿塞诺香豆醇、华法林和phenprocoumon)。这一发展的目的是提出一种适用于法医毒理学情况的分析技术,即在常规凝血试验无法使用的情况下,使用大剂量抗凝剂进行中毒。血样中加入普拉西泮作为内标后,进行液液萃取(LLE),然后进行HPLC分析。在C8对称柱上进行色谱分离,流动相由乙腈和磷酸盐缓冲液(pH 3.8)组成,以梯度模式进行。检测波长在200至400纳米之间。以总误差为决策准则,对该方法进行了验证。准确度为99.1% ~ 105.0%,RSD为1.3% ~ 6.7%。因此,这种快速和简单的色谱技术很好地适用于药品市场上最重要的香豆素类药物的中毒,现在在我们的实验室常规用于法医“一般未知”筛选。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
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