Potential of synchrotron X-ray powder diffractometry for detection and quantification of small amounts of crystalline drug substances in pharmaceutical tablets

The purpose of this study was to develop a sensitive system for detection of crystalline drug substances in intact pharmaceutical tablets by X-ray powder diffractometry (XRPD), using synchrotron X-rays. Fenoprofen calcium dihydrate was used as a model compound. The wavelength and path length of X-ra...

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Bibliographic Details
Published in:Journal of pharmaceutical and biomedical analysis 2011-09, Vol.56 (2), p.448-453
Main Authors: Yamada, Hiroyuki, Masuda, Katsuhiko, Ishige, Takayuki, Fujii, Kotaro, Uekusa, Hidehiro, Miura, Keiko, Yonemochi, Etsuo, Terada, Katsuhide
Format: Article
Language:English
Subjects:
Analysis
Analytical, structural and metabolic biochemistry
Anti-Inflammatory Agents, Non-Steroidal - chemistry
Biological and medical sciences
calcium
Chemistry, Pharmaceutical
Crystalline
Crystallization
Crystallography, X-Ray
detection limit
Drug Compounding
drugs
Fenoprofen - chemistry
Fundamental and applied biological sciences. Psychology
General pharmacology
Medical sciences
Pharmacology. Drug treatments
Powder Diffraction
Reproducibility of Results
Sensitive detection
Sensitivity and Specificity
Synchrotron radiation
Synchrotrons
Tablet
Tablets
Technology, Pharmaceutical - methods
Titanium - chemistry
wavelengths
X-radiation
X-ray powder diffractometry
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Summary:The purpose of this study was to develop a sensitive system for detection of crystalline drug substances in intact pharmaceutical tablets by X-ray powder diffractometry (XRPD), using synchrotron X-rays. Fenoprofen calcium dihydrate was used as a model compound. The wavelength and path length of X-rays from synchrotron radiation were optimized in order to maximize the potential of the synchrotron radiation. The optimum wavelength and path length for the measurement of fenoprofen calcium dihydrate were found to be 0.69817 Å and 6.0 mm, respectively, based on theoretical calculations. Under the optimized conditions, a limit of quantification of 0.05% (RSD = 9.4%, n = 3) and a limit of detection of 0.02% (RSD = 17.3%, n = 3), results which are approximately 10 2 times as sensitive as those obtained using conventional XRPD instruments, were achieved. The technique was also applied to fenoprofen calcium dihydrate detection in intact film-coated tablets, which contained Ti in the coating film, and a limit of detection of 0.02% was again attained.
ISSN:0731-7085
1873-264X
DOI:10.1016/j.jpba.2011.05.038