手性色谱柱测定维格列汀中间体对映异构体
CSTR:
作者:
作者单位:

作者简介:

通讯作者:

中图分类号:

基金项目:

国家“重大新药创制”科技重大专项(2014ZX09507001)


Determination of the vildagliptin intermediate
Author:
Affiliation:

Fund Project:

  • 摘要
  • |
  • 图/表
  • |
  • 访问统计
  • |
  • 参考文献
  • |
  • 相似文献
  • |
  • 引证文献
  • |
  • 资源附件
  • |
  • 文章评论
    摘要:

    为建立维格列汀中间体对映异构体含量的测定方法,采用正相高效液相色谱法,色谱柱为ChiralpakAD-H型手性色谱柱(250 mm×4.6 mm,5 μm),流动相为正己烷-乙醇-甲醇(三者体积比为65∶25∶10),流速为0.8 mL/min,进样体积为10 μL,检测波长为210 nm,柱温为35 ℃。实验得知:维格列汀中间体与其对映异构体的分离度良好,空白溶剂不干扰对映异构体的含量测定;检测限为27 ng/mL,定量限为81 ng/mL;重复性试验中,供试品所含对映异构体含量的RSD值均小于2.0%;稳定性试验中,12 h内对映异构体峰面积及含量的RSD值均小于2.0%;耐用性试验中,维格列汀中间体与其对映异构体峰可实现完全分离,并且不同参数下对映异构体含量的RSD值小于2.0%。结果表明,此方法专属性强,灵敏度高,重复性、耐用性良好,可用于维格列汀中间体对映异构体含量的测定。

    Abstract:

    In order to establish a NP-HPLC method for the determination of enantiomer in vildagliptin intermediate, the determination is carried out on the column of ChiralpakAD-H(250 mm×4.6 mm, 5 μm), with the mobile phase of n-hexane, ethanol and methanol(volume ratio of 65∶25∶10)at flow rate of 0.8 mL/min. The sample volume is 10 μL, the wavelength is 210 nm and the column temperature is 35 ℃. The result shows that the vildagliptin intermediate and its enantiomer could be well separated and detected effectively; blank solvent doesn't interfere with the enantiomer assaying; the detection limit is 27 ng/mL and the quantification limit is 81 ng/mL; in repetitive test, the RSD of enantiomer assaying of samples are no more than 2.0%; in stability test, the RSD are no more than 2.0% in 12 h; the vildagliptin intermediate and its enantiomer could be well separated in the test of durability with all RSDs below 2.0%. The method is simple, reliable, accurate and durable, and can be used for determination of enantiomer in vildagliptin intermediate.

    参考文献
    相似文献
    引证文献
引用本文

栗伟娜,胡 佳,翟梦宇,高子彬.手性色谱柱测定维格列汀中间体对映异构体[J].河北科技大学学报,2017,38(3):249-254

复制
分享
相关视频

文章指标
  • 点击次数:
  • 下载次数:
  • HTML阅读次数:
  • 引用次数:
历史
  • 收稿日期:2017-01-22
  • 最后修改日期:2017-03-22
  • 录用日期:
  • 在线发布日期: 2017-06-28
  • 出版日期:
文章二维码