柱前衍生化RP-HPLC分离巴氯芬的对映异构体
RP-HPLC separation of Baclofen enantiomer by pre-column derivatization
作者:张春艳;袁牧;黄碧云;季红;朱柳;
Author:
收稿日期: 年卷(期)页码:2008,(03):-342-343
期刊名称:华西药学杂志
Journal Name:WEST CHINA JOURNAL OF PHARMACEUTICAL SCIENCES
关键字:吡喃葡萄糖基异硫氰酸酯(GITC);巴氯芬;反相高效液相色谱法;对映体拆分
Key words:
基金项目:广东省科技基金项目(2006B35501003);;
广州市属高校科技计划项目(20041019)
中文摘要
目的建立巴氯芬对映异构体的拆分方法。方法采用柱前衍生化RP-HPLC法,以2,3,4,6-乙酰基-β-D-吡喃葡萄糖基异硫氰酸酯为柱前手性衍生化试剂,考察衍生化时间、试剂用量、流动相组成及其pH等因素对手性分离的影响。结果采用ZORBAX-C8(150 mm×4.6 mm,5μm)色谱柱,在流动相为甲醇-0.05 mol.L-1磷酸二氢钾溶液(40:60,pH6.0)、紫外检测波长为254 nm、流速为1.5 m.lmin-1、柱温35℃的色谱条件下,巴氯芬对映体衍生物获得了基线分离,分离度为1.93,并确认了R(+)-衍生物的色谱峰。结论所建方法简便、快速,为巴氯芬的光学异构体的测定提供了参考。
参考文献
[1]Amikishieva AV.Testosterone and behavior:involvement of thehormone in psychotropic effects of baclofen[J].Bull Exp BiolMed,2007,143(2):259-63.
[2]Amikishieva AV,Semendvaeva SN.Effects of baclofen on anxie-ty,sexual motivation,and olfactory perception in male mice in dif-ferent psychoemotional states[J].Neurosci Behav Physiol,2007,37(9):929-937.
[3]Sivilotti L,Nistri A.GABA receptor mechanisms in the centralnervous system[J].Progr Neurobiol,1991,36(1):35-92.
[4]Goda R,Murayama N,Fujimaki Y,et al.Simple and sensitiveliquid chromatography-tandem mass spectrometry method for de-termination of theS(+)-andR(-)-enantiomers of baclofenin human plasma and cerebrospinal fluid[J].J Chromatogr B,2004,801(2):257-264.
[5]Zhu Z,Neirinck L.Chiral separation and determination ofR-(-)-andS-(+)-baclofen in human plasma by high-per-formance liquid chromatography[J].J Chromatogr B,2003,785(2):277-283.
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