尿中MDMA和MDA的酰基衍生化-电子俘获检测气相色谱分析法

Analysis of MDMA and MDA in urine by acyl derivatization and gas chromatography with electron-capture detection

研究了致幻性安非它明类药物MDMA和MDA的三氟乙酰、二氯乙酰、一氯二氟乙酰、五氟丙酰、七氟丁酰、五氟苯甲酰和二硝基苯甲酰衍生化的反应条件,发现所研究的各种衍生化反应均可用少量酸酐或酰氯在环己烷中室温下几分钟内完成。在此基础上建立了尿中MDMA和MDA的用微量环己烷提取的、各种衍生化的、电子俘获检测的气相色谱分析方法。方法操作简便快速,多数方法的检出限低于10μg/L,检测MDMA最灵敏的方法是七氟丁酰衍生化方法,检出限为4.1μg/L,检测MDA最灵敏的方法是五氟苯甲酰衍生化方法,检出限为2.5μg/L。对其中几种灵敏度较高的方法进行了线性关系和回收率的考查。

In this paper the reaction conditions for trifluoroacetylation, dichloroacetylation, monochlorodifluoroacetylation, pentafluoropropanoylation, heptafluorobutyrylation, pentafluorobenzoylation, and 3,5-dinitrobenzoylation of MDMA and MDA of hallucinatory amphetamine drugs were investigated. It was found that all of the acylation reaction studied could be accomplished at room temperature in a period of several minutes using small amount of acid anhydride or acyl chloride as derivatization reagent and cyclobexane as reaction solvent. On the base of this studies the methods for analysis of MDMA and MDA in urine by cyclohexane extraction and various acyl derivatization and gas chromatography with electron-capture detection were developed. This methods were rapid and simple. The limits of detection （LOD） of most of the methods were below 10 μg/L. The most sensitive one for MDMA was the heptafluorobutyrylation method and the LOD of which was 4.1 μg/L. That for MDA was the pentafluorobenzoylation method and the LOD of which was 2.5μg/L. Several more sensitive methods were selected to examine the linearity and recovery. The results were satisfactory.