摘要
研究了致幻性安非他明类药物3,4-亚甲二氧基甲基安非他明(MDMA)和3,4-亚甲二氧基安非他明(MDA)的乙酰化、三氟乙酰化、五氟丙酰化、七氟丁酰化、二氯乙酰化、一氯二氟乙酰化、五氟苯甲酰化、五氟苯磺酰化和二硝基苯甲酰化的衍生化反应条件,发现除了乙酰化之外所研究的各种衍生化反应均可用5μL酸酐或酰氯在环己烷中于20℃10 m in内完成。乙酰化可用20μL乙酸酐在60℃30 m in内完成。在此基础上建立了尿中MDMA和MDA的各种衍生化的氮磷检测气相色谱(GC/NPD)分析方法。方法操作简便快速,绝大多数方法的检出限低于10μg/L,其中二氯乙酰化、一氯二氟乙酰化、五氟苯甲酰化、五氟苯磺酰化和二硝基苯甲酰化的GC/NPD分析方法未见文献报道。对一些灵敏的方法进行了线性关系和回收率的考察,结果满意。
In this paper the reaction conditions of acetylation, trifluoroacetylation, dichloroacetylation, monochlorodifluoroacetylation, pentafluoropropanoylation, heptafluorobutyrylation, pentafluorobenzoylation, pentafluorobenzensulfonylation, and 3,5-dinitrobenzoylation of MDMA and MDA of hallucinotory amphetamines drug were investigated. It was found that all of the acylation reactions but acetylation could be accomplished in cyclohexane at room temperature in 10 rain, using 5 μL of acid anhydride or acyl chloride as derivatization reagent. Acetylation needed 20μL of anhydride at 60 ℃ to react 30 rain. Methods for analysis of MDMA and MDA in urine by cyclohexane extraction and various acyl derivatization and gas chromatography with nitrogen -phosphorous detection were developed based on these investigations. These methods were rapid and simple. The limit of detection for most methods was below 10 μg/L. Among the methods studied in this paper the methods using dichloroacetylation, monochlorodifluoroacetylation, pentafluoro-benzoylation, pentafluorobenzensulfonylation, and 3,5-dinitrobenzoylation have not been found in the literature. Several more sensitive methods were selected to examine the linearity and recovery. The result was satisfactory.
出处
《分析测试学报》
CAS
CSCD
北大核心
2007年第4期500-502,507,共4页
Journal of Instrumental Analysis
基金
公安部科研基金资助项目(20049323101)
关键词
尿
致幻性安非它明类药物
酰基衍生化
气相色谱
氮磷检测器
Urine
Hallucinatory amphetamines drug
Acyl derivatization
Gas chromatography
Ni-trogen - phosphorous detection
