NIR spectroscopy; Validation; Manufacturing process; Tablet assay; PAT
Abstract :
[en] The goal of this study was to apply the Process Analytical Technology FDA's initiative in pharmaceutical tablets manufacturing. Near Infrared Spectrophotometry (NIRS) was used as a non-destructive, very fast technique requiring no sample preparation. Direct compression powder blends containing Diltiazem HCl as a model drug were pressed into tablets for the calibration and the validation steps. First, a partial least squares model was built to calibrate the NIR spectrometer. Then, this model was validated and compared with a validated UV spectrophotometry reference method. For this comparison, the Bland and Altman's statistical method was applied. The manufacturing process was validated by producing three batches at three different concentration levels. The NIR analysis of these batches was performed during 3 days. This study shows that NIRS can be used to validate the whole manufacturing process and not only as an analytical method for tablets assay. NIRS is an interesting tool to show possible variations during the manufacturing process which could lead the finished product to fall outside of specifications.
Research Center/Unit :
C.I.R.M.
Disciplines :
Pharmacy, pharmacology & toxicology
Author, co-author :
Bodson, Cédric
Rozet, Eric ; Université de Liège - ULiège > Chimie analytique
Ziemons, Eric ; Université de Liège - ULiège > Chimie analytique
Evrard, Brigitte ; Université de Liège - ULiège > Département de pharmacie > Pharmacie galénique
E.T.S. Skibsted, Ph.D. Thesis, PAT and Beyond, 2005.
American Food Drug Administration (FDA). Guidance for Industry PAT-A Framework for Innovative Pharmaceutical Manufacturing and Quality Assurance (2004), FDA
Rodrigues L., Alves T., Cardoso J., and Menezes J. IDrugs 9 (2006) 44-48
Blanco M., Alcala M., Gonzalez J.M., and Torras E. J. Pharm. Sci. 95 (2006) 2137-2144
Ciurczak E.W., and Drennen J.K. In: Burns D.A., and Ciurczak E.W. (Eds). Handbook of Near-infrared Analysis (2001) 609-632
Chen Y., Thosar S.S., Forbess R.A., Kemper M.A., Rubinovitz R., and Shukla A.J. Drug Dev. Ind. Pharm. 27 (2001) 623-631
Kirsch J.D., and Drennen J.K. J. Pharm. Biomed. Anal. 19 (1999) 351-362
Laasonen M., Harmia-Pulkkinen T., Simard C., Rasanen M., and Vuorela H. Anal. Chem. 75 (2003) 754-760
Li T., Donner A.D., and Choi C. J. Pharm. Sci. 92 (2003) 1526-1530
Boulanger B., Dewé W., Chiap P., Crommen J., and Hubert Ph. J. Pharm. Biomed. Anal. 32 (2003) 753-765
Hubert Ph., Nguyen-Huu J.-J., Boulanger B., Chapuzet E., Chiap P., Cohen N., Compagnon P.-A., Dewé W., Feinberg M., Lallier M., Laurentie M., Mercier N., Muzard G., Nivet C., and Valat L. J. Pharm. Biomed. Anal. 36 (2004) 579-586
Bland J.M., and Altman D.G. Lancet 1 (1986) 307-310
Gottfries J., Depui H., Fransson M., Jongeneelen M., Josefson M., Langkilde F.W., and Witte D.T. J. Pharm. Biomed. Anal. 14 (1996) 1495-1503
Marini R.D., Servais A.-C., Rozet E., Chiap P., Boulanger B., Rudaz S., Crommen J., Hubert P., and Fillet M. J. Chromatogr. A 1120 (2006) 102-111
Rozet E., Morello R., Lecomte F., Martin G.B., Chiap P., Crommen J., Boos K.S., and Hubert P. J. Chromatogr. B 844 (2006) 251-260
Boulanger B., Dewe W., Gilbert A., Govaerts B., and Maumy-Bertrand M. Chemometr. Intell. Lab. Syst. 86 (2007) 198-207
International Conference on Harmonization (ICH) of Technical Requirements for registration of Pharmaceuticals for Human Use, Topic Q2 (R1): Validation of Analytical Procedures: Text and Methodology, Geneva, 2005.
Rozet E., Ceccato A., Hubert C., Ziemons E., Oprean R., Rudaz S., Boulanger B., and Hubert P. J. Chromatogr. A 1158 (2007) 111-125