Quantitative Determination of Hydrate Content of Theophylline Powder by Chemometric X-ray Powder Diffraction Analysis
The purpose of this study was to establish a calibration model to predict the hydrate content in powder materials consisting of anhydrate (theophylline anhydrate (THA)) and theophylline monohydrate (THM) by using various kinds of X-ray powder diffraction (XRPD) analytical methods. XRPD profiles were measured five times each for 11 standard samples containing of THA and THM. THM content in the standard samples was evaluated based on XRPD profiles by the diffraction peak height and area methods, and the Wakelin’s and principal component regression (PCR) methods, respectively. Since THA and THM were cube- and rod-shaped particles, the standard samples consisted of THA and THM showed crystal orientation due to THM crystal shape. THA showed reproducible XRPD profiles, but THM showed fluctuating intensities in some specific peaks in the profiles. The linear calibration models were evaluated based on calibration XRPD datasets of the standard materials by various methods. In the result based on validation XRPD datasets, the order of the mean bias and the mean accuracy were peak height > peak area > Wakelin’s > PCR, indicating that PCR was the best method to correct sample crystal orientation. The effectiveness of the PCR method in construction of calibration models was discussed by a scientific approach based on regression vectors.
- Haleblian JK, McCrone W. Pharmaceutical applications of polymorphism. J Pharm Sci. 1969;58:911. CrossRef
- ICH harmonized guideline. Q6A Specifications, test procedures and acceptance criteria for new drug substances and new drug products, chemical substance; 1999.
- Byrn S, Pfeiffer R, Ganey M, Hoiberg C, Poochikian G. Pharmaceutical solids: a strategic approach to regulatory considerations. Pharm Res. 1995;12:945. CrossRef
- Yoshino H, Hagiwara Y, Kobayashi S, Samejima M. Estimation of polymorphic transition degree of pharmaceutical raw materials. Chem Pharm Bull. 1984;32:1523.
- Artursson T, Hagman A, Bjőuml S, Trygg J, Wold S, Jacobsson JP. Study of preprocessing methods for the determination of crystalline phases in binary mixtures of drug substances by X-ray powder diffraction and multivariate calibration. Appl Spectrosc. 2000;54:1222–30. CrossRef
- Zevin LS, Kimmel G. Quantitative X-ray diffractometry. New York: Springer; 1995.
- Okumura T, Nakazono M, Otsuka M, Takayama K. An accurate quantitative analysis of polymorphs based on artificial neural networks. Colloids Surf B. 2006;49:153. CrossRef
- Okumura K, Otsuka M. A novel standard sample powder preparation method for quantitative analysis of polymorphs. J Pharm Sci. 2005;94:1013. CrossRef
- Paulson W Ed. Regulatory leeway sought for process analytical technology. The Gold Sheet, Vol. 36. Elsevier, Chevy Chase; 2002.
- Process Analytical Technology (PAT) Initiative, U. S. Food and Drug Administration Center for Drug Evaluation and Research Home Page, http://www.fda.gov/cder/OPS/PAT.htm/.
- Florence AJ, Johnston A, Price SL, Nowell H, Kennedy AR, Shankland N. An automated parallel crystallisation search for predicted crystal structures and packing motifs of carbamazepine. J Pharm Sci. 2006;95:1918. CrossRef
- Palabiyik IM, Dinç E, Onur F. Simultaneous spectrophotometric determination of pseudoephedrine hydrochloride and ibuprofen in a pharmaceutical preparation using ratio spectra derivative spectrophotometry and multivariate calibration techniques. J Pharm Biomed Anal. 2004;34:473. CrossRef
- Kramer R. Chemometric techniques for quantitative analysis. New York: Marcel Dekker; 1998. p. 51–99. CrossRef
- Hasegawa T. Quantitative analytical techniques of spectra. Tokyo: Kodansha Scientific; 2005.
- Otsuka M, Fukui Y, Otsuka K, Kim HJ, Ozaki Y. Determination of cephalexin crystallinity and investigation of formation of its amorphous solid by chemoinformetrical near infrared spectroscopy. J Near Infrared Spectrosc. 2006;14:9. CrossRef
- Ramirez JL, Bellamy MK, Romanach RJ. A novel method for analyzing thick tablets by near infrared spectroscopy. Pharm Sci Tech. 2001;2:1–10. article 11 (http://www.pharmscitech.com).
- Tantry JS, Tank J, Suryanarayanan R. Processing-induced phase transitions of theophylline - implications on the dissolution of theophylline tablets. J Pharm Sci. 2007;96:1434–44. CrossRef
- Otsuka M, Kaneniwa N, Kawakami K, Umezawa O. Effect of surface characteristic of theophylline anhydrate powder on hygroscopic stability. JPharm Pharmcol. 1990;42:606–10.
- Shefter E, Higuchi T. Dissolution behavior of crystalline solvated and nosovated forms of some pharmaceuticals. J Pharm Sci. 1963;52:781–91. CrossRef
- Walkelin JH, Virgi HS, Crystal E. Development and Comparison of Two X-ray Methods for Determinating the Crystallinity of Cotton Cellulose. J Appl Phys. 1981;30:1674.
- Martents H, Næs T. Multivariate calibration. New York: Wiley; 1989.
- Quantitative Determination of Hydrate Content of Theophylline Powder by Chemometric X-ray Powder Diffraction Analysis
Volume 11, Issue 1 , pp 204-211
- Cover Date
- Online ISSN
- Springer US
- Additional Links
- hydrate form
- principal component regression analysis
- theophylline monohydrate and monohydrate
- X-ray powder diffraction analysis
- Wakelin’s method
- Industry Sectors