Diastereomeric and enantiomeric high-performance liquid chromatographic separation of synthetic anisodamine.

Diastereomeric and enantiomeric high-performance liquid chromatographic separation of synthetic anisodamine.
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DOI:
10.1016/j.jpba.2006.09.006
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发表时间:
2007-02
影响因子:
3.4
通讯作者:
Li-min Yang;Yifan Xie;Hong-Zhuan Chen;Yang Lu
Li-min Yang;Yifan Xie;Hong-Zhuan Chen;Yang Lu
中科院分区:
医学3区
文献类型:
--
作者:
Li-min Yang;Yifan Xie;Hong-Zhuan Chen;Yang Lu

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为了研究临床上广泛使用的胆碱受体拮抗剂山莨菪碱(654-2)的对映体药代动力学和生物转化,采用ZORBAX Eclipse XDB-C18色谱柱,将其拆分为两个外消旋体(I和II)。采用HPLC法,使用CHIRALPAK AD-H作为手性固定相(CSP),乙腈-2-丙醇-DEA 97:3:0.1(v/v/v)作为移动的相,对654-2、I和II进行非对映体和/或对映体分离。通过对移动的相修饰剂、修饰剂浓度和柱温的考察,优化了方法。同时分离654-2的两对映体的HPLC方法已得到验证。
In order to investigate the enantiomeric pharmacokinetics and biotransformation of synthetic anisodamine (654-2), a cholinoceptor antagonist widely used in clinic in China, it has been preparatively separated into two racemates (I and II) by using ZORBAX Eclipse XDB-C18 column. The diastereo- and/or enantioseparations of 654-2, I and II were carried out by HPLC using CHIRALPAK AD-H as chiral stationary phase (CSP) and acetonitrile–2-propanol–DEA 97:3:0.1 (v/v/v) as mobile phase. The methods were optimized by studying mobile phase modifiers, concentration of modifier and column temperature. The HPLC method for the simultaneous separation of two pairs of enantiomers of 654-2 has been validated.