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GC/MS 法测定尿液中的芬太尼、代谢物和类似物。

Determination of fentanyl, metabolite and analogs in urine by GC/MS.

机构信息

Antidoping Laboratory, FMSI, L.go G. Onesti 1, 00168, Rome, Italy.

出版信息

J Appl Toxicol. 2011 Oct;31(7):649-54. doi: 10.1002/jat.1613. Epub 2010 Dec 6.

DOI:10.1002/jat.1613
PMID:21132842
Abstract

A rapid and sensitive method for the simultaneous determination of alfentanyl, sufentanyl and fentanyl (and its major metabolite norfentanyl) in urine was developed and validated. The method involved a liquid-liquid extraction in alkaline conditions, derivatization with pentafluoropropionic anhydride to improve the sensitivity for norfentanyl and subsequent analysis in GC/MS. The LODs are 0.08 ng ml(-1) for all substances (0.04 ng ml(-1) for alfentanyl). Intra- and inter-day precision coefficient of variation was always below 15%; mean relative error (accuracy) was always below 15%. The method was linear for all analytes, with quadratic regression of calibration curves always higher than 0.99. The method was applied to real samples of subjects who had received therapeutic doses of fentanyl, showing its suitability for the determination of low levels of these substances. The method was also applied to a subject whose death was attributed to fentanyl overdose.

摘要

建立并验证了一种尿液中阿芬太尼、舒芬太尼和芬太尼(及其主要代谢物去甲芬太尼)的同时快速灵敏检测方法。该方法涉及在碱性条件下进行液-液萃取,用五氟丙酰酐衍生化以提高去甲芬太尼的灵敏度,随后进行 GC/MS 分析。所有物质的检测限(LOD)均为 0.08ng/ml(阿芬太尼为 0.04ng/ml)。日内和日间精密度变异系数始终低于 15%;平均相对误差(准确度)始终低于 15%。该方法对所有分析物均呈线性,二次回归校准曲线始终高于 0.99。该方法已应用于接受芬太尼治疗剂量的受试者的实际样本,表明其适用于检测这些物质的低水平。该方法还应用于一位死因归咎于芬太尼过量的受试者。

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