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采用气相色谱-质谱联用技术同时检测毛发、血浆、唾液和尿液中的可卡因、海洛因及其代谢物。

Simultaneous assay of cocaine, heroin and metabolites in hair, plasma, saliva and urine by gas chromatography-mass spectrometry.

作者信息

Wang W L, Darwin W D, Cone E J

机构信息

Addiction Research Center, National Institute on Drug Abuse, Baltimore, MD 21224.

出版信息

J Chromatogr B Biomed Appl. 1994 Oct 14;660(2):279-90. doi: 10.1016/0378-4347(94)00309-2.

Abstract

As part of an ongoing research program on the development of drug detection methodology, we developed an assay for the simultaneous measurement of cocaine, heroin and metabolites in plasma, saliva, urine and hair by solid-phase extraction (SPE) and gas chromatography-mass spectrometry (GC-MS). The analytes that could be measured by this assay were the following: anhydroecgonine methyl ester; ecgonine methyl ester;. ecgonine ethyl ester; cocaine; cocaethylene; benzoylecgonine; cocaethylene; norcocaethylene; benzoylnorecgonine; codeine; morphine; norcodeine; 6-acetylmorphine; normorphine; and heroin. Liquid specimens were diluted, filtered and then extracted by SPE. Additional handling steps were necessary for the analysis of hair samples. An initial wash procedure was utilized to remove surface contaminants. Washed hair samples were extracted with methanol overnight at 40 degrees C. Both wash and extract fractions were collected, evaporated and purified by SPE. All extracts were evaporated, derivatized with N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) with 1% trimethylchlorosilane (TMCS) and analyzed by GC-MS. The limit of detection (LOD) for cocaine, heroin and metabolites in biological specimens was approximately 1 ng/ml with the exception of norcodeine, normorphine and benzoylnorecgonine (LOD = 5 ng/ml). The LOD for cocaine, heroin and metabolites in hair was approximately 0.1 ng/mg of hair with the exception of norcodeine (LOD = 0.3 ng/mg) and normorphine and benzoylnorecgonine (LOD = 0.5 ng/mg). Coefficients of variation ranged from 3 to 26.5% in the hair assay. This assay has been successfully utilized in research on the disposition of cocaine, heroin and metabolites in hair, plasma, saliva and urine and in treatment studies.

摘要

作为一项正在进行的药物检测方法开发研究项目的一部分,我们开发了一种通过固相萃取(SPE)和气相色谱 - 质谱联用(GC - MS)同时测定血浆、唾液、尿液和毛发中可卡因、海洛因及其代谢物的分析方法。该分析方法可测定的分析物如下:脱水芽子碱甲酯;芽子碱甲酯;芽子碱乙酯;可卡因;可口乙酮;苯甲酰芽子碱;可口乙酮;去甲可口乙酮;苯甲酰去甲芽子碱;可待因;吗啡;去甲可待因;6 - 乙酰吗啡;去甲吗啡;以及海洛因。液体样本经稀释、过滤后通过SPE进行萃取。毛发样本的分析需要额外的处理步骤。首先采用清洗程序去除表面污染物。清洗后的毛发样本在40摄氏度下用甲醇萃取过夜。收集清洗液和萃取液,蒸发后通过SPE进行纯化。所有提取物经蒸发后,用含1%三甲基氯硅烷(TMCS)的N,O - 双(三甲基硅基)三氟乙酰胺(BSTFA)进行衍生化,然后通过GC - MS进行分析。生物样本中可卡因、海洛因及其代谢物的检测限约为1 ng/ml,但去甲可待因、去甲吗啡和苯甲酰去甲芽子碱除外(检测限 = 5 ng/ml)。毛发中可卡因、海洛因及其代谢物的检测限约为0.1 ng/mg毛发,但去甲可待因除外(检测限 = 0.3 ng/mg),去甲吗啡和苯甲酰去甲芽子碱的检测限为0.5 ng/mg。毛发分析中的变异系数范围为3%至26.5%。该分析方法已成功应用于可卡因、海洛因及其代谢物在毛发、血浆、唾液和尿液中的代谢研究以及治疗研究。

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