[en] In the first two documents [Ph. Hubert, J.J. Nguyen-Huu, B. Boulanger, E. Chapuzet, P. Chiap, N. Cohen, P.A. Compagnon, W. Dewe, M. Feinberg. M. Lallier, M. Laurentie, N. Mercier, G. Muzard, C. Nivet, L. Valat, J. Pharm. Biomed. Anal. 36 (2004) 579-586; Ph. Hubert, J.J. Nguyen-Huu. B. Boulanger, E. Chapuzet, P. Chiap, N. Cohen, P.A. Compagnon, W. Dewe, M. Feinberg, M. Lallier, M. Laurentie, N. Mercier, G. Muzard. C. Nivet, L. Valat, E. Rozet, J. Pharm. Biomed. Anal., in press], a recent SFSTP Commission on the validation of analytical procedure has introduced a harmonized approach for the validation of analytical procedures. In order to complete this guide, the statistical methodology allowing to correctly conclude about the validity of a procedure is proposed in this third part of the guide. Indeed all the steps to obtain the decision tool namely the accuracy profile are described and illustrated step by step by a numerical example. This tool, based on the concept of total error (bias + standard deviation) build with a P-expectation tolerance interval, allows to easily take the right decision and simultaneously minimizing the risk of the future use of the analytical procedure. (C) 2007 Elsevier B.V. All rights reserved.
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
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., Valat L., and Rozet E. J. Pharm. Biomed. Anal. 45 (2007) 70-81
Chapuzet E., Mercier N., Bervioas-Martin S., Boulanger B., Chevalier P., Chiap P., Grandjean D., Hubert Ph., Lagorce P., Lallier M., Laparra M.C., Laurentie M., and Nivet J.C. STP Pharma Prat. 7 (1997) 169-194
Chapuzet E., Mercier N., Bervioas-Martin S., Boulanger B., Chevalier P., Chiap P., Grandjean D., Hubert Ph., Lagorce P., Lallier M., Laparra M.C., Laurentie M., and Nivet J.C. STP Pharma Prat. 8 (1997) 81-107
Hubert Ph., Chiap P., Crommen J., Boulanger B., Chapuzet E., Mercier N., Bervoas-Martin S., Chevalier P., Grandjean D., Lagorce P., Lallier M., Laparra M.C., Laurentie M., and Nivet J.C. Anal. Chim. Acta 391 (1999) 135-148
ISO 5725, Accuracy (trueness and precision) of measurement methods and results-Parts1-4, Part 6, ISO, Geneva, Switzerland, 1994.
ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories, ISO, Geneva, 2000.
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.
Guidance for Industry: Bioanalytical, Methods Validation for Human Studies, U.S. Department of Health and Human Services, Food and Drug Administration, Center for Drug Evaluation and Research (CDER), 2001.
Guidance for Industry: Analytical, Procedures and Methods Validation (Draft guidance), U.S. Department of Health and Human Services, Food and Drug Administration, Center for Drug Evaluation and Research (CDER), Center for Biologics Evaluation and Research (CBER), Août, 2000.
Shah V.P., Midha K.K., Dighe S., McGilveray I., Skelly J.P., Yacobi A., Layloff T., Viswanathan C.T., Cook C.E., McDowall R.D., and Pittman K.A. J. Pharm. Sci. 81 (1992) 309-312
Shah V.P., Midha K.K., Findlay J.W.A., Hill H.M., Hulse J.D., McGilveray I.J., McKay G., Miller K.J., Patnaik R.N., Powell M.L., Tonelli A., Viswanathan C.T., and Yacobi A. Pharm. Res. 17 (2000) 1551
Boulanger B., Dewé W., Chiap P., Crommen J., and Hubert Ph. J. Pharm. Biomed. Anal. 32 (2003) 753-765
Feinberg M., Boulanger B., Dewé W., and Hubert Ph. Anal. Bioanal. Chem. 380 (2004) 502-514
Rozet E., Hubert C., Ceccato A., Dewé W., Ziemons E., Moonen F., Michail K., Wintersteiger R., Streel B., Boulanger B., and Hubert Ph. J. Chromatogr. A 1158 (2007) 126-137
Rozet E., Ceccato A., Hubert C., Ziemons E., Oprean R., Rudaz S., Boulanger B., and Hubert Ph. J. Chromatogr. A 1158 (2007) 111-125
Huet S., Jolivet E., and Méssean A. La régression non linéaire (1992), Éditions INRA, Paris
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. STP Pharma Prat. 13 (2003) 101-138
Hoffman D., and Kringle R. J. Biopharm. Stat. 15 (2005) 283-293