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 chromatogra phy with nitrogenphosphorus detection was developed. One ml urine samples we re alkalined and saturated with sodium chloride then extracted with 02ml cyclohe x ane .The extracts were added to 4μl of pentafluorobenzoyl chloride to carry out derivatization reaction at room temperature for 10min . After reaction the exce ss derivatization reagents were destroyed by washing with 01mol/L sodium hydr ox ide solution and the organic phases were devated to gas chromatography . The lim it of detection of MDMA in urine was 40ng/ml.The present method is more sensit i ve than acetyl, trifluoroacetyl, pentafluoropropanoyl ,heptafluorobutanoyl deriv atization methods and underivatization method.