Guillot J G, Lefebvre M, Weber J P
Centre de Toxicologie du Québec, Sainte-Foy, Canada.
J Anal Toxicol. 1997 Mar-Apr;21(2):127-33. doi: 10.1093/jat/21.2.127.
We present an analytical method for the determination of heroin, free 6-acetylmorphine (6-AM), and free morphine in blood, urine, and vitreous humor. This method is used in postmortem cases where heroin is the suspected cause of death. The analytical protocol includes the following steps: liquid-liquid extraction at pH 9.5, propionylation at room temperature of 6-AM, and morphine by propionic anhydride using 4-dimethylaminopyridine as catalyst. Neither heroin nor diethylnalorphine (internal standard) is transformed during this derivatization. The reaction products are analyzed using full-scan (250-405 amu) ion trap gas chromatography-mass spectrometry. This method provides a baseline separation and distinctive mass spectrum of each compound of interest. Reproducibility and an evaluation of analysis parameters are also presented.
我们提出了一种用于测定血液、尿液和玻璃体液中 heroin、游离 6 - 乙酰吗啡(6 - AM)和游离吗啡的分析方法。该方法用于怀疑 heroin 为死因的死后案例。分析方案包括以下步骤:在 pH 9.5 条件下进行液 - 液萃取,在室温下使用 4 - 二甲基氨基吡啶作为催化剂,通过丙酸酐对 6 - AM 和吗啡进行丙酰化。在此衍生化过程中,heroin 和二乙 nalorphine(内标)均不发生转化。使用全扫描(250 - 405 amu)离子阱气相色谱 - 质谱联用仪对反应产物进行分析。该方法能对每种目标化合物进行基线分离并给出独特的质谱图。还介绍了重现性以及分析参数的评估。