色谱

色谱

• 研究论文 • 上一篇    下一篇

反相柱色谱法分离纯化洛沙坦原料中的杂质

聂晶1,2,文毅2,余琼卫2,相秉仁1,冯钰锜2

  

  1. 1.Center for Instrumental Analysis, China Pharmaceutical University, Nanjing 210009, China; 2.Department of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072, China
  • 收稿日期:2004-12-03 修回日期:1900-01-01 出版日期:2006-01-30 发布日期:1987-09-25
  • 通讯作者: 冯钰琦

Isolation and Purification of the Process Impurity in Losartan by Reversed-Phase Column Chromatography

NIE Jing1,2, WEN Yi2, YU Qiongwei2, XIANG Bingren1, FENG Yuqi2   

  1. 1.Center for Instrumental Analysis, China Pharmaceutical University, Nanjing 210009, China; 2.Department of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072, China
  • Received:2004-12-03 Revised:1900-01-01 Online:2006-01-30 Published:1987-09-25

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摘要：

采用反相柱色谱法对洛沙坦原料中的洛沙坦同分异构体杂质(含量约4%)进行了分离制备。收集每份流出液并进行高效液相色谱(HPLC)检测,合并含有目标化合物的流出液。对杂质粗品进行重结晶,所得产物的纯度大于99%(经HPLC检测)；质谱分析结果表明,该杂质的相对分子质量与洛沙坦的相同,质谱裂解规律与洛沙坦一致；并通过核磁共振对该化合物进行了结构确证。与常规制备色谱相比,该方法分离步骤简单,分离效率高,上样量大,收率高。

关键词: 纯化, 反相柱色谱, 核磁共振 , 洛沙坦, 同分异构体, 质谱

Abstract:

A process impurity (~ 4%, w/w) was isolated from losartan crude by low-pressure reversed-phase column chromatography. At first the elution portions containing the target compound were collected. After evaporation and recrystallization, the purity of the target compound was found to be over 99% based on high performance liquid chromatography with ultraviolet absorption. The electrospray ionization-mass spectrometry result showed that it was an isomeric compound of losartan, which had same fragmentation pattern with its parent compound. And at last the compound was further characterized by nuclear magnetic resonance. This research demonstrates that the low-pressure reversed-phase column chromatography can raise separation efficiency and recovery comparing with other conventional column chromatography, and the technique can be applied as an effective means for the enrichment and extraction of impurities in pharmaceutical separation.

Key words: isomeric compound, losartan, mass spectrometry, nuclear magnetic resonance spectroscopy , purification, reversed-phase column chromatography