尿中3,4-亚甲二氧基甲基苯丙胺的五氟苯甲酰衍生化—氮磷检测气相色谱分析法

The determination of 3,4-methylenedioxymethamphetamine in urine by pentafluorobenzoyl derivatization and gas chromatography with nitrogen-phosphorus detection

本文建立了尿中3,4亚甲二氧基甲基苯丙胺(MDMA)的五氟苯甲酰衍生化-氮磷检测气相色谱分析方法,1ml检尿碱化、加氯化钠饱和、用0.2ml环己烷提取,提取液加4μl五氟苯甲酰氯于室温反应10min,过量试剂用0.1mol/L氢氧化钠溶液涡洗除去,有机相供进样分析。尿中MDMA的检测限为4.0ng/ml,较非衍生化、乙酰化、三氟乙酰化、五氟丙酰化和七氟丁酰衍生化等分析法灵敏。

In this paper the determination method of 3, 4-methylenedioxymethamp- hetamine（MDMA） in urine by pentafluorobenzoyl derivatization and gas chromatography with nitrogen-phosphorus detection was developed. One ml urine samples were alkalined and saturated with sodium chloride then extracted with 0.2ml cyclohexane . The extracts were added to 4μl of pentafluorobenzoyl chloride to carry out derivatization reaction at room temperature for 10min . After reaction the excess derivatization reagents were destroyed by washing with 0. 1mol/L sodium hydroxide solution and the organic phases were devated to gas chromatography. The limit of detection of MDMA in urine was 4.0ng/ml. The present method is more sensitive than acetyl, trifluoroacetyl, pentafluompmpanoyl, heptafluorobutanoyl derivatization methods and underivatization method.