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Development of a New Method Based on Chiral Ligand-Exchange Chromatography for the Enantioseparation of Propranolol

机译:手性配体交换色谱对映体拆分心得安的新方法的开发

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摘要

A new chromatographic procedure was proposed for the separation of propranolol (PRN) enantiomers based upon enantioselective chiral ligand-exchange chromatography. The separation was carried out on a short C8 column leading to considerably short separation time. L-alanine and Cu2+ were applied as chiral selector and central bivalent complexing ion, respectively. It was found that the kind of copper salt could influence the enantioseparation efficiency. The separation on the C8 stationary phase was more efficient than that on the C18 column. It was shown that the pH of mobile phase, organic modifier content of mobile phase, mole ratio of chiral ligand to bivalent ion and Cu (L-alanine) 2 concentration in the mobile phase were important in enantioseparation efficiency. Water/methanol (70:30) mixture containing L-alanine-Cu2+ (7:1) was found to be the best mobile phase condition for PRN enantioseparation. All effective parameters were optimized in order to improve the separation efficiency. The optimized HPLC method was utilized for analysis of propranolol enantiomers in spiked human blood plasma samples.
机译:提出了一种基于对映选择性手性配体交换色谱分离普萘洛尔(PRN)对映异构体的新色谱方法。分离在较短的C8色谱柱上进行,从而大大缩短了分离时间。 L-丙氨酸和Cu 2+ 分别用作手性选择剂和中心二价络合离子。发现铜盐的种类可以影响对映体分离效率。在C8固定相上的分离比在C18色谱柱上的分离更有效。结果表明,流动相的pH,流动相的有机改性剂含量,手性配体与二价离子的摩尔比和流动相中Cu(L-丙氨酸)2的浓度对对映体分离效率具有重要意义。发现含有L-丙氨酸-Cu 2 + (7:1)的水/甲醇(70:30)混合物是PRN对映体分离的最佳流动相条件。优化所有有效参数,以提高分离效率。优化的HPLC方法用于分析加标的人血浆样品中的普萘洛尔对映体。

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