[en] This paper is the first part of a summary report of a new commission of the Societe Francaise des Sciences et Techniques Pharmaceutiques (SFSTP). The main objective of this commission was the harmonization of approaches for the validation of quantitative analytical procedures. Indeed, the principle of the validation of theses procedures is today widely spread in all the domains of activities where measurements are made. Nevertheless. this simple question of acceptability or not of an analytical procedure for a given application, remains incompletely determined in several cases despite the various regulations relating to the good practices (GLP, GMP,...) and other documents of normative character (ISO, ICH. FDA,...). There are many official documents describing the criteria of validation to be tested, but they do not propose any experimental protocol and limit themselves most often to the general concepts. For those reasons, two previous SFSTP commissions elaborated validation guides to concretely help the industrial scientists in charge of drug development to apply those regulatory recommendations. If these two first guides widely contributed to the use and progress of analytical validations, they present, nevertheless, weaknesses regarding the conclusions of the performed statistical tests and the decisions to be made with respect to the acceptance limits defined by the use of an analytical procedure. The present paper proposes to review even the bases of the analytical validation for developing harmonized approach, by distinguishing notably the diagnosis rules and the decision rules. This latter rule is based on the use of the accuracy profile, uses the notion of total error and allows to simplify the approach of the validation of an analytical procedure while checking the associated risk to its usage. Thanks to this novel validation approach, it is possible to unambiguously demonstrate the fitness for purpose of a new method as stated in all regulatory documents. (C) 2004 Elsevier B.V. All rights reserved.
Ph. Hubert, J.J. Nguyen-Huu, B. Boulanger, E. Chapuzet, P. Chiap, N. Cohen, P.A. Compagnon, W. Dewé, M. Feinberg, M. Lallier, M. Laurentie, N. Mercie, G. Muzard, C. Nivet, and L. Valat STP Pharma. Pract. 13 2003 101 138
Commission of the European Communities, Working group of the committee of medical products, explanatory notes III/844/87-FR, final, August 1989.
Drugs Directorate Guidelines: Acceptable Methods, Authority of the Minister of National Health and Welfare, Health Protection Branch, Health and Welfare, Canada, 1992.
United States Pharmacopeia XXVI, General information <1225>, Validation of Compendial Methods, The United States Pharmacopeia Inc., Rockville, MD, USA, 2003, pp. 2439-2442.
Food and Drug Administration: International Conference on Harmonization, Definitions and terminology, Fed. Regist. 60 (1995) 11260-11262.
Food and Drug Administration: International Conference on Harmonization, Methodology, Fed. Regist. 62 (1997) 27463-27467.
Manager's Guide to VAM, Valid Analytical Measurement Programme, UK Department of Trade and Industry.
Eurachem Guide, The fitness for purpose of analytical methods, A Laboratory Guide to Method Validation and Related Topics, first ed., 1998, http://www.eurachem.ul.pt/guides.
Eurachem/Citac Guide, Quantifying Uncertainty in Analytical Measurement, second ed., Eurachem, 2000, http://www.eurachem.bam.de.
Food and Drug Administration, Guidance for Industry (draft), Analytical Procedures and Methods Validation, 2000, http://www.fda.gov/cder/guidance.
Food and Drug Administration, Guidance for Industry, Bioanalytical Methods Validation, 2001, http://www.fda.gov/cder/guidance.
ISO 3301, Statistical interpretation of data - comparison of two means in the case of paired observations, ISO, Geneva, Switzerland, 1975.
ISO 5725, Accuracy (trueness and precision) of measurement methods and results, Parts 1-4, 6, ISO, Geneva, Switzerland, 1994.
ISO/DIS 17025, General requirements for the competence of calibration and testing laboratories, ISO, Geneva, Switzerland, 1999.
ISO 11843-2, Capability of detection - part 2: methodology in the linear calibration case, ISO, Geneva, Switzerland, 2000.
ISO/DTS 21748 (2003), Guide to the use of repeatability, reproducibility and trueness estimates in measurement uncertainty estimation, ISO, Geneva, Switzerland, 2003.
SANCO Commission of the European communities Off. J. Eur. Commun. L221 2002 8 36
V.P. Shah, K.K. Midha, S. Dighe, I. McGilveray, J.P. Skelly, A. Yacobi, T. Layloff, C.T. Viswanathan, C.E. Cook, R.D. McDowall, and K.A. Pittman J. Pharm. Sci. 81 1992 309 312
Bio-International 2, Post conference satellite symposium, Update on Analytical Method Validation, H.H. Blume et K.K. Midha, Medpharm, Stuttgart, 1995, p. 319.
J. Caporal-Gautier, J.M. Nivet, P. Algranti, M. Guilloteau, M. Histe, M. Lallier, J.J. Nguyen-Huu, and R. Russoto STP Pharma. Pract. 2 1992 205 226
E. Chapuzet, N. Mercier, S. Bervoas-Martin, B. Boulanger, P. Chevalier, P. Chiap, D. Grandjean, Ph. Hubert, P. Lagorce, M. Lallier, M.C. Laparra, M. Laurentie, and J.C. Nivet STP Pharma. Pract. 7 1997 169 194
Ph. Hubert, P. Chiap, J. Crommen, B. Boulanger, E. Chapuzet, N. Mercier, S. Bervoas-Martin, P. Chevalier, D. Grandjean, P. Lagorce, M. Lallier, M.C. Laparra, M. Laurentie, and J.C. Nivet Anal. Chim. Acta 391 1999 135 148
A.C. Causey, H.M. Hills, and L.J. Phillips J. Pharm. Biomed. Anal. 8 1990 625 628
G.P. Carr, and J.C. Wahlich J. Pharm. Biomed. Anal. 8 1990 613 618
P.A.D. Edwardson, G. Bhaskar, and J.E. Fairbrother J. Pharm. Biomed. Anal. 8 1990 929 933
A.R. Buick, M.V. Doig, S.C. Jeal, G.S. Land, and R.D. McDowall J. Pharm. Biomed. Anal. 8 1990 629 637
H.T. Karnes, and C. March J. Pharm. Biomed. Anal. 9 1991 911 918
J.R. Lang, and S. Bolton J. Pharm. Biomed. Anal. 9 1991 357 361
J.R. Lang, and S. Bolton J. Pharm. Biomed. Anal. 9 1991 435 442
C. Hartmann, D.L. Massart, and R.D. McDowall J. Pharm. Biomed. Anal. 12 1994 1337 1343
D. Dadgar, P.E. Burnett, M.G. Choc, K. Gallicano, and J.W. Hooper J. Pharm. Biomed. Anal. 13 1995 89 97
J. Vessman J. Pharm. Biomed. Anal. 14 1996 867 869
S. Braggio, R.J. Barnaby, P. Grossi, and M. Cugola J. Pharm. Biomed. Anal. 14 1996 375 388
C. Hartmann, J. Smeyers-Verbeke, D.L. Massart, and R.D. McDowall J. Pharm. Biomed. Anal. 17 1996 193 218
P. Chiap, Ph. Hubert, B. Boulanger, and J. Crommen Anal. Chim. Acta 391 1999 227 238
L.A. Curie Anal. Chim. Acta 391 1999 127 134
M. Feinberg, and N. Raguènès Anal. Chim. Acta 391 1999 239 252
B. Boulanger, Ph. Hubert, P. Chiap, W. Dewé, Objectives of pre-study validation and decision rules, AAPS APQ Open forum, Washington, 2000.
B. Boulanger, Ph. Hubert, P. Chiap, W. Dewé, and J. Crommen Statistical analysis of the validation results GMP 2000
Ph. Hubert, P. Chiap, W. Dewé, B. Boulanger, J. Crommen, The usefulness of accuracy profile in LC method validation, HPLC 2001, Maastrich, 2001.
W.A. Findlay, W.C. Smith, J.W. Lee, G.D. Nordblom, I. Das, B.S. DeSilva, M.N. Khan, and R.R. Bowsher J. Pharm. Biomed. Anal. 21 2000 1249 1273
J. Ermer J. Pharm. Biomed. Anal. 24 2001 755 767
Y. Vander Heyden, A. Nijhuis, J. Smeyers-Verbeke, B.G.M. Vandeginste, and D.L. Massart J. Pharm. Biomed. Anal. 24 2001 723 753
B. Boulanger, W. Dewé, P. Chiap, J. Crommen, and Ph. Hubert J. Pharm. Biomed. Anal. 32 2003 753 765
J.O. De Beer, P. Baten, C. Nsengyumva, and J. Smeyers-Verbeke J. Pharm. Biomed. Anal. 32 2003 767 811
Ph. Hubert, J.J. Nguyen-Huu, B. Boulanger, E. Chapuzet, P. Chiap, N. Cohen, P.A. Compagnon, W. Dewé, M. Feinberg, M. Lallier, M. Laurentie, N. Mercier, G. Muzard, C. Nivet, L. Valat., J. Pharm. Biomed. Anal. (submitted for publication).
S. Pinzauti, P. Gratteri, S. Furlanetto, P. Mura, E. Dreassi, and R. Phan-Tan-Luu J. Pharm. Biomed. Anal. 14 1996 881 889
S. Furlanetto, S. Pinzauti, P. Gratteri, E. La Porta, and G. Calzeroni J. Pharm. Biomed. Anal. 15 1997 1585 1594
Y. Vander Heyden, F. Questier, and L. Massart J. Pharm. Biomed. Anal. 18 1998 43 56
Y. Vander Heyden, F. Questier, and D.L. Massart J. Pharm. Biomed. Anal. 18 1998 153 168
Food and Drug Administration, Process Analytical Technology (PAT) Initiative, 2002, http:// www.fda.gov/cder/OPS/PAT.html.
