Rapid determination of ambrisentan enantiomers by enantioselective liquid chromatography using cellulose-based chiral stationary phase in reverse phase mode.
Rapid determination of ambrisentan enantiomers by enantioselective liquid chromatography using cellulose-based chiral stationary phase in reverse phase mode.
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DOI：
10.1002/jssc.201101062
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发表时间：
2012-04
影响因子：
3.1
通讯作者：
Michal Douša;Petr Gibala
中科院分区：
文献类型：
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作者：
Michal Douša;Petr Gibala
建立了一种灵敏、特异、快速的高效液相色谱（HPLC）测定双布里森坦对映体的方法。在反相系统中测试了六个手性柱。用20 mM甲酸钠（pH 3.0）与乙腈（55:45;v/v）的混合物对Chiralcel oz3r（3-氯-4-甲基苯基氨基甲酸酯纤维素）进行了拆分，拆分率大于2.5。根据国际协调会议（ICH）指南进行HPLC方法的验证，包括线性、检出限、定量限、精密度、准确度和选择性。该方法色谱分离速度快（小于6 min），适用于对映纯活性药物成分(S)- ambristan中(R)- ambristan的常规测定。
A sensitive, specific, and rapid high-performance liquid chromatography (HPLC) method for the determination of ambrisentan enantiomers has been developed and validated. Six chiral columns were tested in a reversed-phase system. Excellent enantioseparation with the resolution more than 2.5 was achieved on Chiralcel OZ-3R (cellulose 3-chloro-4-methylphenylcarbamate) using mixture of 20 mM sodium formate (pH 3.0) with acetonitrile (55:45; v/v). Validation of the HPLC method including linearity, limit of detection, limit of quantification, precision, accuracy, and selectivity was performed according to the International Conference on Harmonisation (ICH) guidelines. The method has an advantage of a very quick chromatographic separation (less than 6 min) and therefore is highly suitable for routine determination of (R)-ambrisentan in enantiopure active pharmaceutical ingredient (S)-ambrisentan.