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直接串联质谱法同时测定干尿斑中的阿片类药物、可卡因及其代谢物。

Direct tandem mass spectrometry for the simultaneous assay of opioids, cocaine and metabolites in dried urine spots.

机构信息

Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, University of Santiago de Compostela, Santiago de Compostela, Spain.

出版信息

Anal Chim Acta. 2013 Jun 19;784:25-32. doi: 10.1016/j.aca.2013.04.061. Epub 2013 May 10.

Abstract

A micro-analytical method based on spotting urine samples (20μL) onto blood/urine spot collection cards followed by air-drying and extraction (dried urine spot, DUS) was developed and validated for the screening/confirmation assay of morphine, 6-methylacetylmorphine (6-MAM), codeine, cocaine and benzoylecgonine (BZE). Acetonitrile (3 mL) was found to be a useful solvent for target extraction from DUSs under an orbital-horizontal stirring at 180 rpm for 10 min. Determinations were performed by direct electrospray ionization tandem mass spectrometry (ESI-MS/MS) under positive electrospray ionization conditions, and by using multiple reaction monitoring (MRM) with one precursor ion/product ion transition for the identification and quantification (deuterated analogs of each target as internal standards) of each analyte. The limits of detection of the method were 0.26, 0.94, 1.5, 1.1, and 2.0 ng mL(-1), for cocaine, BZE, codeine, morphine and 6-MAM, respectively; whereas, relative standard deviations of intra- and inter-day precision were lower than 8 and 11%, respectively, and intra- and inter-day analytical recoveries ranged from 94±4 to 105±3%. The small volume of urine required (20 μL), combined with the simplicity of the analytical technique makes it a useful procedure for screening/quantifying drugs of abuse. The method was successfully applied to the analysis of urine from polydrug abusers.

摘要

建立并验证了一种基于将尿样(20μL)点样到血/尿斑采集卡上,风干后提取(干尿斑,DUS)的微分析方法,用于吗啡、6-单乙酰吗啡(6-MAM)、可待因、可卡因和苯甲酰爱康宁(BZE)的筛选/确证检测。研究发现,在 180rpm 轨道水平搅拌下,3mL 乙腈是从 DUS 中提取目标物的有效溶剂,提取时间为 10min。通过正电喷雾离子化串联质谱(ESI-MS/MS),采用多反应监测(MRM),以每个分析物的一个前体离子/产物离子跃迁对(每个目标物的氘代类似物作为内标)进行鉴定和定量。该方法的检测限分别为 0.26、0.94、1.5、1.1 和 2.0ng·mL-1,用于可卡因、BZE、可待因、吗啡和 6-MAM;而日内和日间精密度的相对标准偏差分别低于 8%和 11%,日内和日间分析回收率在 94%±4%至 105%±3%之间。该方法所需的尿液量少(20μL),与分析技术的简单性相结合,使其成为一种用于筛选/定量滥用药物的有用方法。该方法成功地应用于多药滥用者尿液的分析。

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