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一种用于测定尿液中苯丙胺及相关药物的便捷衍生化方法。

A convenient derivatization method for the determination of amphetamine and related drugs in urine.

作者信息

Jonsson J, Kronstrand R, Hatanpää M

机构信息

Department of Forensic Chemistry, University Hospital, Linköping, Sweden.

出版信息

J Forensic Sci. 1996 Jan;41(1):148-51.

PMID:8934716
Abstract

The most commonly abused CNS stimulant in Sweden is amphetamine followed by phenmetrazine. Methamphetamine and phentermine are rarely seen but still of interest. This paper describes a rapid and sensitive method for the analysis of amphetamine, methamphetamine, phentermine, and phenmetrazine in urine using gas chromatography with nitrogen sensitive detection (GC-NPD). The method also qualitatively determines ephedrine and norephedrine. The derivatization was carried out at room temperature with methyl chloroformate to form the corresponding carbamates. Other chloroformate analogues were also tested. Because methyl chloroformate is relatively stable in the presence of water the extraction and derivatization were combined in one step. A concentration step was not necessary to achieve sufficient sensitivity. The recovery was more than 83% for all analytes. The LOQ was 0.05, 0.03, 0.07 and 0.01 (microgram/mL urine) for amphetamine, methamphetamine, phentermine and phenmetrazine respectively. The cut-off was set at 0.2 microgram/mL. The within-day and between-day relative standard deviation (RSD) for amphetamine were 2.2% (n = 9) and 4.7% (n = 5) respectively. There was a good quantitative correlation (r2 = 0.995) between GC-NPD using chloroformate derivatives and gas chromatography-mass spectrometry (GC-MS) using trifluoroacetic anhydride (TFA) as derivatizing agent for the determination of amphetamine in authentic samples.

摘要

在瑞典,最常被滥用的中枢神经系统兴奋剂是苯丙胺,其次是苯甲曲秦。甲基苯丙胺和芬特明很少见,但仍值得关注。本文描述了一种使用带氮敏感检测的气相色谱法(GC-NPD)分析尿液中苯丙胺、甲基苯丙胺、芬特明和苯甲曲秦的快速灵敏方法。该方法还能定性测定麻黄碱和去甲麻黄碱。衍生化反应在室温下用氯甲酸甲酯进行,以形成相应的氨基甲酸酯。还测试了其他氯甲酸酯类似物。由于氯甲酸甲酯在有水存在的情况下相对稳定,萃取和衍生化可一步完成。无需浓缩步骤即可获得足够的灵敏度。所有分析物的回收率均超过83%。苯丙胺、甲基苯丙胺、芬特明和苯甲曲秦的定量限分别为0.05、0.03、0.07和0.01(微克/毫升尿液)。临界值设定为0.2微克/毫升。苯丙胺日内和日间相对标准偏差(RSD)分别为2.2%(n = 9)和4.7%(n = 5)。在实际样品中,使用氯甲酸酯衍生物的GC-NPD法与使用三氟乙酸酐(TFA)作为衍生剂的气相色谱-质谱联用(GC-MS)法测定苯丙胺之间存在良好的定量相关性(r2 = 0.995)。

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