柱前荧光标记高效液相色谱法对血浆中l-麻黄碱和d-伪麻黄碱的定量分析

l-麻黄碱和d-伪麻黄碱是生药麻黄中早为人知而至今仍被广泛用于临床的一对手性异构生物碱。由于二者为生药麻黄中的主要成分但药理活性不同,为便于临床监控及有效用药,高分辨高灵敏度的检测方法的开发迫在眉睫。本文以易于得到的dansylchloride为柱前荧光标识试剂,在确定了最佳衍生化及分离条件的基础上,建立了理想的色谱分析系统(线性检测范围1～800ng·ml^-1)。同时运用此方法,完成了对静注l-麻黄碱和d-伪麻黄碱后豚鼠血浆内该对手性异构体水平的考查,并且定量检测了服用中成药小青龙合剂后人血浆中的该对手性异构体。

QUANTITATIVE ANALYSIS OF(l)-EPHEDRINE AND(d)- PSEUDOEPHEDRINE IN PLASMA BY HIGH-PERFORMANCELIOUD CHKOMATOGRAPHY WITH FLUORESCENCE DETECTION

Quantitative analysis of(l)-ephedrine(l-Ep)and(d)-pseudoephedrine(d-Ps )in plasma by high-performance liquid chromatography(HPLC)is described.The newly developed method is based on a precolumn derivatization with 5-dimethyl- aminonaphthalene-1-sulfonyl chloride(DNSCI )in acetonitrile. The diastereomers formed were separated on a reversed phase column by HPLC with fluorescence detection employing 0.6%phosphate buffer(pH 6.5)-methanof(3:8,v/v)as mobile phase.The detection limit of each Ephedra alkaloid stereoisomer was 0.5 ng at a signal- to-noise ratio of 3 :1 ,the linear response to each stereoisomer being 1～800 ng· ml^-1.The plasma level profile of l-Ep and d-ps in guinea pig was investigated by this method. The determination of l- Ep and d-Ps in plasma of a volunteer after oral administration of Xiao Qinglong Heji was also performed.