Towards a full integration of optimization and validation phases: An Analytical-Quality-by-Design approach

[en] When using an analytical method, defining an Analytical Target Profile (ATP) focused on quantitative performance represents a key input, and this will drive the method development process. In this context, two case studies were selected in order to demonstrate the potential of a Quality-by-Design (QbD) strategy when applied to two specific phases of the method lifecycle: the pre-validation study and the validation step. The first case study focused on the improvement of a Liquid Chromatography (LC) coupled to Mass Spectrometry (MS) stability-indicating method by the means of the QbD concept. The Design of Experiments (DoE) conducted during the optimization step (i.e. determination of the qualitative Design Space (DS)) was performed a posteriori. Additional experiments were performed in order to simultaneously conduct the pre-validation study to assist in defining the DoE to be conducted during the formal validation step. This predicted protocol was compared to the one used during the formal validation. A second case study based on the LC/MS-MS determination of glucosamine and galactosamine in human plasma was considered in order to illustrate an innovative strategy allowing the QbD methodology to be incorporated during the validation phase. An operational space, defined by the qualitative DS, was considered during the validation process rather than a specific set of working conditions as conventionally performed. Results of all the validation parameters conventionally studied were compared to those obtained with this innovative approach for glucosamine and galactosamine. Using this strategy, qualitative and quantitative information were obtained. Consequently, an analyst using this approach would be able to select with great confidence several working conditions within the operational space rather than a given condition for the routine use of the method. This innovative strategy combines both a learning process and a thorough assessment of the risk involved.

Research center :

Centre Interfacultaire de Recherche du Médicament - CIRM

Disciplines :

Pharmacy, pharmacology & toxicology

Author, co-author :

Hubert, Cédric ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique

Houari, Sabah ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique

Rozet, Eric ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique

Lebrun, Pierre ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique

Hubert, Philippe ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique

Language :

English

Title :

Towards a full integration of optimization and validation phases: An Analytical-Quality-by-Design approach

Publication date :

2015

Journal title :

Journal of Chromatography. A

ISSN :

0021-9673

eISSN :

1873-3778

Publisher :

Elsevier Science, Amsterdam, Netherlands

Peer reviewed :

Peer Reviewed verified by ORBi

Available on ORBi :

since 13 April 2015

Statistics

Number of views

182 (20 by ULiège)

Number of downloads

726 (10 by ULiège)

More statistics

Scopus citations^®

Scopus citations^®
without self-citations

OpenCitations

Bibliography

ICH, Q8(R2), Pharmaceutical development, 2009.
ICH, Q2(R1), Validation of analytical procedures, 1996.
ICH, Q9, Quality risk management, 2006.
ICH, Q10, Pharmaceutical quality system, 2008.
U.S. Pharmacopeial Convention, chapters 1224, 1225, 1226, USP panel expert.
U.S. Pharmacopeial Convention, chapters 1032, 1033, 1034, USP panel expert.
U.S. Pharmacopeial Convention, chapter 1210, USP panel expert.
Peterson J.J. A Bayesian approach to the ICH Q8 definition of design space. J. Biopharm. Stat. 2008, 18:959.
Peterson J.J., Yahyah M. A Bayesian design space approach to robustness and system suitability for pharmaceutical assays and other processes. Stat. Biopharm. Res. 2009, 1:441.
Nethercote P., Ermer J. Quality by design for analytical methods: implications for method validation and transfer. Pharm. Tech. 2012, 36(10):52.
Orlandini S., Pinzauti S., Furlanetto S. Application of quality by design to the development of analytical separation methods. Anal. Bioanal. Chem. 2013, 405:443.
Debrus B., Guillarme D., Rudaz S. Improved quality-by-design compliant methodology for method development in reversed-phase liquid chromatography. J. Pharm. Biomed. Anal. 2013, 84:215.
Rozet E., Lebrun P., Hubert P., Debrus B., Boulanger B. Design spaces for analytical methods. Trends Anal. Chem. 2013, 42:157.
Hubert C., Lebrun P., Houari S., Ziemons E., Rozet E., Hubert Ph. Improvement of a stability-indicating method by quality-by-design versus quality-by-testing: a case of a learning process. J. Pharm. Biomed. Anal. 2014, 88:401.
Borman P., Nethercote P., Chatfield M., Thompson D., Truman K. The application of quality by design to analytical methods. Pharm. Technol. 2007, 31:142.
Katz P., Campbell C. FDA 2011 process validation guidance: process validation revisited. J. GXP Compliance 2012, 16:18.
Pohl M., Schweitzer M., Hansen G., Hanna-Brown M., Borman P., Smith K., Larew J., Nethercote P. Implications and opportunities of applying QbD principles to analytical measurements. Pharm. Technol. Eur. 2010, 22:29.
Burdick R.K., LeBlond D.J., Sandell D., Yang H., Pappa H. Statistical methods for validation of procedure accuracy and precision. Pharm. Forum 2013, 39.
Borman P., Chatfield M., Damjanov I., Jackson P. Design and analysis of method equivalence studies. Anal. Chem. 2009, 81:9849.
Dewé W. Review of statistical methodologies used to compare (bio)assays. J. Chromatogr. B 2009, 877:2208.
Skelley A.M., Mathies R.A. Rapid on-column analysis of glucosamine and its mutarotation by microchip capillary electrophoresis. J. Chromatogr. A 2006, 1132:304.
Hubert C., Houari S., Lecomte F., Houbart V., De Bleye C., Fillet M., Piel G., Rozet E., Hubert Ph. Development and validation of a sensitive solid phase extraction/hydrophilic interaction liquid chromatography/mass spectrometry method for the accurate determination of glucosamine in dog plasma. J. Chromatogr. A 2010, 1217:3275.
Lebrun P., Govaerts B., Debrus B., Ceccato A., Caliaro G., Hubert P., Boulanger B. Development of a new predictive modelling technique to find with confidence equivalence zone and design space of chromatographic analytical methods. Chemometr. Intell. Lab. Syst. 2008, 91:4.
Debrus B., Lebrun P., Ceccato A., Caliaro G., Rozet E., Nistor I., Oprean R., Rupérez F.J., Barbas C., Boulanger B., Hubert P. Application of new methodologies based on design of experiments, independent component analysis and design space for robust optimization in liquid chromatography. Anal. Chim. Acta 2011, 691:33.
Lebrun P., Boulanger B., Debrus B., Lambert Ph., Hubert Ph. A Bayesian design space for analytical methods based on multivariate models and predictions. J. Biopharm. Stat. 2012, (accepted July 2012, http://hdl.handle.net/2268/128222).
Hemstrom P., Irgum K. Hydrophilic interaction chromatography. J. Sep. Sci. 2006, 29:1784.
Borman P., Chatfield M., Damjanov I., Jackson P. Method ruggedness studies incorporating a risk based approach: a tutorial. Anal. Chim. Acta 2011, 703:101.
Hsieh Y. Potential of HILIC-MS in quantitative bioanalysis of drugs and drug metabolites. J. Sep. Sci. 2008, 31:1481.
Gama M.R., da Costa Silva R.G., Collins C.H., Bottoli C.B.G. Hydrophilic interaction chromatography. Trends Anal. Chem. 2012, 37:48.
Chambers E., Wagrowski-Diehl D.M., Lu Z., Mazzeo J.R. Systematic and comprehensive strategy for reducing matrix effects in LC/MS/MS analysis. J. Chromatogr. B 2007, 852:22.
Mess J.-N., COté C., Bergeron A., Furtado M., Garofolo F. Selection of HILIC columns to handle matrix effect due to phospholipids. Bioanalysis 2009, 1:57.
Tan B., Negahban A., McDonald T., Zhang Y., Holliman C. Utilization of hydrophilic-interaction LC to minimize matrix effects caused by phospholipids. Bioanalysis 2012, 4:2049.
U.S. Department of Health and Human Services, Food and Drug Administration (FDA), Center for Drug Evaluation and Research (CDER), Center for Veterinary Medicine (CVM), Guidance for industry: Bioanalytical Method Validation (Rockville, MD, May 2001).
Rozet E., Ceccato A., Hubert C., Ziemons E., Oprean R., Rudaz S., Boulanger B., Hubert Ph. Analysis of recent pharmaceutical regulatory documents on analytical method validation. J. Chromatogr. A 2007, 1158:111.
Rozet E., Wascotte V., Lecouturier N., Preat V., Dewé W., Boulanger B., Hubert Ph. Improvement of the decision efficiency of the accuracy profile by means of a desirability function for analytical methods validation. Application to a diacetyl-monoxime colorimetric assay used for the determination of urea in transdermal iontophoretic extracts. Anal. Chim. Acta 2007, 591:239.
U.S. Department of Health and Human Services, Food and Drug Administration (FDA), Center for Drug Evaluation and Research (CDER), Center for Biologics Evaluation and Research (CBER), Guidance for Industry Analytical Procedures and Methods Validation for Drugs and Biologics (Rockville, MD, February 2014).