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首页> 外文期刊>Separation Science Plus >Microchemical enantioseparation of betaxolol and orciprenaline by reversed phase HPLC
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Microchemical enantioseparation of betaxolol and orciprenaline by reversed phase HPLC

机译：微量化学enantioseparation倍他洛尔和反相高效液相色谱法测定奥西那林

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摘要

Enantioseparation of (RS)-orciprenaline and (RS)-betaxolol was achieved by synthesizing their diastereomeric derivatives with chiral derivatizing reagents prepared on a cyanuric chloride platform. There were three dichloro-triazine derivatives with amino acid amides as chiral auxiliaries and three monochloro-triazine derivatives with methoxy as achiral moiety and amino acid amides as chiral auxiliaries in cyanuric chloride. A total of 12 pairs of diastereomeric derivatives were synthesized under microwave irradiation and were separated using reversed phase high-performance liquid chromatography by applying different mobile phases on a C(18)column in gradient eluting mode with ultraviolet detection at 230 nm. Resolutions were compared and interpreted on the basis of structure of chiral auxiliaries. Besides, diastereomeric derivatives were separated by open column chromatography and the samples so obtained were used for confirmation of their elution order and configuration by(1)H-NMR spectroscopy. In addition, lowest energy optimized structures of diastereomeric derivatives were developed using the density functional theory based Gaussian software that were interpreted to supplement the absolute configurations. The method validation was carried out for detection limit, linearity, accuracy, and precision. Limits of detection were 0.005 and 0.007 mu g/mL.
机译：奥西那林和Enantioseparation (RS)(RS)倍他洛尔是通过合成的非对映的衍生品与手性三聚氰酰derivatizing试剂的准备氯的平台。dichloro-triazine与氨基酸衍生品酰胺作为手性助剂和三个monochloro-triazine衍生品与甲氧基非手性的一部分,作为手性氨基酸酰胺三聚氰酰氯的助剂。对非对映的衍生品合成微波辐射下使用反相高效分离通过应用不同的液相色谱法移动阶段C(18)列在梯度淋洗模式与紫外检测,享年230岁nm。结构的手性助剂的基础。此外,非对映的衍生品通过开放的柱层析法和分离所以获得用于确认样品他们的洗脱顺序和配置(1)核磁共振光谱学。优化结构的非对映的衍生品开发使用密度功能理论基于高斯软件被解释为补充的绝对吗配置。的检出限、线性、准确性,精度。0.007μg / mL。

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