Harmonization of strategies for the validation of quantitative analytical procedures

Abstract

In the first two documents [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. 36 (2004) 579-586; 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, 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 beta-expectation tolerance interval, allows to easily take the right decision and simultaneously minimizing the risk of the future use of the analytical procedure.

Thorough characterization of a Self-Emulsifying Drug Delivery System with Raman hyperspectral imaging: A case study

“…The validation samples mappings were then analyzed with the PLS model and the mean predicted concentration of each map was used to validate the model. This method has been validated using the "total error" approach in accordance with the validation requirements in the ICH Q2 R1 norm (Hubert et al, 2008(Hubert et al, , 2007a(Hubert et al, , 2007b(Hubert et al, , 2004.…”

Fighting Poor Quality Medicines: Development, Transfer and Validation of Generic HPLC Methods for Analyzing Two WHO Recommended Antimalarial Tablets

“…In this work, the transferred method was also validated using the accuracy profile as decision tool and for the simultaneous quantitation of the couples artemether/lumefantrine and artesunate/amodiaquine in fixed dose combination (FDC) tablets [17] [18]. We considered the validation criteria commonly used in analytical procedures set out in document Q2A of the International Conference on Harmonization (ICH) [19] namely: selectivity/ specificity, trueness, precision (repeatability and intermediate precision), accuracy, linearity, limit of detection (LOD) and limit of quantitation (LOQ).…”

Use of Accuracy Profile Procedure to Validate a Real-Time PCR Method to Quantify Bacteria in Feces

“…However, for E. faecium, the absolute bias is excluded from the acceptability limits but is constant throughout the range level. This type of accuracy profile was also described for analytical methods in chemistry and was analyzed in the usual manner using a correction factor (16,19). In fact, error is mainly linked to a systematic error which was assessed and determined on accuracy profile.…”

“…In addition, the goal of an analytical method is to fit-for-purpose, i.e., produce results that reflect the contents of samples with acceptable accuracy. This accuracy needs to assess trueness and precision simultaneously, i.e., to measure the total error that is used to determine the accuracy profile (13,14). Therefore, the accuracy profile is a possible decision-making graphical tool to decide whether an experimental procedure is valid, and its use has been widely discussed for physicochemical methods in previous published works (12,15,16).…”