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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Simultaneous determination of optical and chemical purities of a drug with two chiral centers by liquid chromatography-circular dichroism detection on a non-chiral stationary phase
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Simultaneous determination of optical and chemical purities of a drug with two chiral centers by liquid chromatography-circular dichroism detection on a non-chiral stationary phase

机译：通过非手性固定相的液相色谱-圆二色性检测同时测定具有两个手性中心的药物的光学和化学纯度

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The need for a rapid and cheap chromatographic technique for the simultaneous determination of diastereoisomeric and chemical purities of a drug has led to develop a non-enantioselective HPLC method on a porous graphitic carbon (PGC) sorbent and by using circular dichroism (CD) detection. Among a lot of non-chiral chromatographic supports tested, PGC was the only one allowing the separation of all benzoxathiepin diastereoisomers. After optimization of the chromatographic conditions, a mobile phase composed of chloroform, acetonitrile and methanol was suitable to elute the diastereoisomers with their related chemical impurities in less than 20 min by gradient mode. CD detection was found to be compatible with elution gradient and both the UV, CD and g anisotropy factor signals were recorded without disturbance. The determination of chemical purity was achieved with UV detection (254 nm) whereas the diastereoisomeric purity was determined using CD detection (258 nm) by plotting the anisotropy factors (R,S-S,R and R,R-SS) versus the enantiomeric excess of each couple of enantiomers. A mathematic model was developed in order to express the diastereoisomeric excess versus the enantiomeric excess of each couple of enantiomers. Hence, the HPLC-UV/CD method was convenient to give access simultaneously to the optical and chemical purities of a chiral drug. (C) 2008 Published by Elsevier B.V.
机译：同时需要一种快速廉价的色谱技术来同时测定药物的非对映异构体和化学纯度的方法，已导致开发一种在多孔石墨碳（PGC）吸附剂上并使用圆二色性（CD）检测的非对映选择性HPLC方法。在许多经过测试的非手性色谱载体中，PGC是唯一可以分离所有苯并氧杂噻吩非对映异构体的载体。优化色谱条件后，由氯仿，乙腈和甲醇组成的流动相适用于通过梯度模式在不到20分钟的时间内洗脱非对映异构体及其相关化学杂质。发现CD检测与洗脱梯度兼容，并且记录了UV，CD和g各向异性因子信号而没有干扰。化学纯度的确定是通过UV检测（254 nm）实现的，而非对映异构体纯度是通过CD检测（258 nm）通过绘制各向异性因子（R，SS，R和R，R-SS）对每对对映体。为了表达每对对映异构体的非对映异构过量相对于对映异构过量，建立了数学模型。因此，HPLC-UV / CD方法可方便地同时获得手性药物的光学和化学纯度。 （C）2008由Elsevier B.V.发布

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