Original Paper

Preparation and characterization of amorphous, I and II forms of clopidogrel hydrogen sulfate

  1. Jie Lu1,*,
  2. Jing Wang1,
  3. S. Rohani2

Article first published online: 13 FEB 2012

DOI: 10.1002/crat.201200037

Issue

Crystal Research and Technology

Crystal Research and Technology

Volume 47, Issue 5, pages 505–510, May 2012

Additional Information

How to Cite

Lu, J., Wang, J. and Rohani, S. (2012), Preparation and characterization of amorphous, I and II forms of clopidogrel hydrogen sulfate. Cryst. Res. Technol., 47: 505–510. doi: 10.1002/crat.201200037

Author Information

  1. 1

    National Engineering Laboratory for Cereal Fermentation Technology, School of Chemical and Material Engineering, Jiangnan University; Wuxi 214122, P. R. China

  2. 2

    Department of Chemical and Biochemical Engineering, The University of Western Ontario; London, Ontario N6A 5B9, Canada

*National Engineering Laboratory for Cereal Fermentation Technology, School of Chemical and Material Engineering, Jiangnan University; Wuxi 214122, P. R. China

Publication History

  1. Issue published online: 4 MAY 2012
  2. Article first published online: 13 FEB 2012
  3. Manuscript Accepted: 30 JAN 2012
  4. Manuscript Received: 20 JAN 2012

Funded by

  • National Natural Science Foundation of China (Nos. 21176102 and 21176215)
  • Scientific Research Foundation for Returned Chinese Scholars (Yr 2011)
  • Fundamental Research Funds for the Central Universities (No. JUSRP30904)

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Keywords:

  • clopidogrel hydrogen sulphate;
  • polymorphs;
  • transformation;
  • characterization

Abstract

In this work the amorphous, I and II forms of clopidogrel hydrogen sulfate (CHS) were prepared and characterized by use of powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FTIR) and differential scanning calorimetry (DSC). The labile precipitate and oiling out during reactive crystallization were also firstly reported. Based on the solubility and thermochemical data, the amorphous form and I form is found to be monotropically related, while the I form and II form are enantiotropically related. In addition, both transformations from anhydrous form to I form and from I form to II form are greatly temperature-dependent, which gives us a window to prepare each pure form. These results will contribute a better understanding about the polymorphic nature and crystallization mechanism of clopidogrel hydrogen sulfate. (© 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim)

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