Hostname: page-component-78c5997874-94fs2 Total loading time: 0 Render date: 2024-11-05T21:17:40.386Z Has data issue: false hasContentIssue false
  • English
  • Français

Determination of the Relative Amounts of α-carbamazepine and β-carbamazepine in a Mixture by Powder X-Ray Diffractometry

Published online by Cambridge University Press:  10 January 2013

Raj Suryanarayanan
Raj Suryanarayanan
Affiliation:
Department of Pharmaceutics, College of Pharmacy, University of Minnesota, Minneapolis, Minnesota, U.S.A.
Get access Rights & Permissions [Opens in a new window]

Abstract

A powder X-ray diffraction technique has been developed to quantify the relative amounts of α-carbamazepine (A) and β-carbamazepine (B) when they occur as a mixture. The theoretical basis of this technique was developed in 1948 by Alexander and Klug (Anal. Chem., 20:886-889). The powder X-ray diffraction patterns of A and B revealed that the line with d-spacing of 10.1 Å was unique to A. The ratio of the integrated intensity of the 10.1 Å line in a mixture of A and B, to the intensity of the 10.1 Å line in a sample consisting of only A, was calculated as a function of weight fraction of A in the mixture. These ratios were also experimentally determined, and there was a good agreement between the theoretical and experimental intensity ratios. The particle size of the samples, the sample preparation technique and the experimental conditions were controlled so as to eliminate the major sources of error in powder X-ray diffractometry. In order to minimize preferred orientation of the particles, a sample holder was specially fabricated.

Type
Research Article
Information
Powder Diffraction , Volume 5 , Issue 3 , September 1990 , pp. 155 - 159
Copyright
Copyright © Cambridge University Press 1990

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Alexander, L. & Klug, H.P. (1948). Anal. Chem. 20, 886–889.Google Scholar
Blom, S. (1962). Lancet 1, 839–840.CrossRefGoogle Scholar
Brindley, G.W. (1961). In The X-Ray Identification and Crystal Structure of Clay Minerals, 2nd ed., ed. Brown, G., 492. London: Mineralogical Society.Google Scholar
Chao, R.S. & Vail, K.C. (1987). Pharm. Res. 4, 429–432.Google Scholar
Cullity, B.D. (1978). Elements of X-Ray Diffraction, 2nd ed., 101–102, 414, 417–418. Reading, MA: Addison-Wesley.Google Scholar
Himes, V.L., Mighell, A.D. & De Camp, W.H. (1981). Acta Crystallogr. B37, 2242–2245.CrossRefGoogle Scholar
Jongmans, J.W.M. (1964). Epilepsia 5, 74–82.CrossRefGoogle Scholar
Kala, H., Haack, U., Pollandt, P. & Brezesinski, G. (1986). Acta Pharm. Technol. 32, 72–77,Google Scholar
as given in Chem. Abstracts (1986) 105, 120610g.Google Scholar
Kala, H., Haack, U., Wenzel, U., Zessin, G. & Pollandt, P. (1987). Pharmazie 42, 524–527.Google Scholar
Kaneniwa, N., Yamaguchi, T., Watari, N. & Otsuka, M. (1984). Yakugaku Zasshi (J. Pharm.) 104, 184–190.CrossRefGoogle Scholar
Klug, H.P. & Alexander, L.E. (1974). X-Ray Diffraction Procedures for Polycrystalline and Amorphous Materials. 2nd ed., 94–95, 294, 360–364, 368–369, 486, 531–536, 540–541. New York: J. Wiley & Sons.Google Scholar
Krahn, F.U. & Mielck, J.B. (1987). Pharm. Acta Helv. 62, 247–254.Google Scholar
Krahn, F.U. & Mielck, J.B. (1989). Int. J. Pharm. 53, 25–34.Google Scholar
Kuhnert-Brandstatter, M. (1971). Thermomicroscopy in the Analysis of Pharmaceuticals, 227. Braunschweig: Pergamon.Google Scholar
Laine, E., Tuominen, V., Ilvessalo, P. & Kahela, P. (1984). Int. J. Pharm. 20, 307–314.Google Scholar
Lefebvre, C., Guyot-Hermann, A.M., Draguet-Brughmans, M., Bouche, R. & Guyot, J.C. (1986). Drug Dev. Ind. Pharm. 12, 1913–1927.Google Scholar
Lowes, M.M.J., Caira, M.R., Lotter, A.P. & Van Der Watt, J.G. (1987). J. Pharm. Sci. 76, 744–752.CrossRefGoogle Scholar
Morris, M.C., McMurdie, H.F., Evans, E.H., Paretzkin, B., de Groot, J.H., Hubbard, C.R. & Carmel, S.J. (1975). Standard X-Ray Diffraction Patterns. Monog. 25 (16), 1–5. Springfield, VA: National Technical Information Service.Google Scholar
Pohlmann, H., Gulde, C., Jahn, R. & Pfeifer, S. (1975). Pharmazie 60, 709–711.Google Scholar
Powder Diffraction File (1989). PDF 33-1565, β-Carbamazepine. Swarthmore, PA: International Centre for Diffraction Data.Google Scholar
Powder Diffraction File (1989). PDF 33-1566, α-Carbamazepine. Swarthmore, PA: International Centre for Diffraction Data.Google Scholar
Reboul, J.P., Cristau, B., Soyfer, J.C. & Astier, J.P. (1981). Acta Crystallogr. B37, 1844–1848.Google Scholar
Suryanarayanan, R. (1989). Pharm. Res. 6, 1017–1024.Google Scholar
Umeda, T., Ohnishi, N., Yokoyama, T., Kuroda, K., Kuroda, T., Tatsumi, E. & Matsuda, Y. (1984). Yakugaku Zasshi (J. Pharm.) 104, 786–792.CrossRefGoogle Scholar
Yang, S.S. & Guillory, J.K. (1972). J. Pharm. Sci. 61, 26–40.Google Scholar