Validation Of Models Of Multivariate Calibration: An Application In The Determination Of Polymorphic Purity Of Carbamazepine By Near Infrared Spectroscopy [validação De Modelos De Calibração Multivariada: Uma Aplicação Na Determinação De Pureza Polimórfica De Carbamazepina Por Espectroscopia No Infravermelho Próximo]

Abstract

The application of analytical procedures based on multivariate calibration models has been limited in several areas due to requirements of validation and certification of the model. Procedures for validation are presented based on the determination of figures of merit, such as precision (mean, repeatability, intermediate), accuracy, sensitivity, analytical sensitivity, selectivity, signal-to-noise ratio and confidence intervals for PLS models. An example is discussed of a model for polymorphic purity control of carbamazepine by NIR diffuse reflectance spectroscopy. The results show that multivariate calibration models can be validated to fulfill the requirements imposed by industry and standardization agencies.27610041011Barros Neto, B., Pimentel, M.F., Araújo, M.C.U., (2002) Quim. Nova, 25, p. 856http://www.analytik-news.de/Presse/2002/178.htmlCharne, R., De Luna, F.C.A., Charnet, E.M.R., Bovino, H., (1999) Análise de Modelos de Regressão Linear: Com Aplicações, , Ed. da UNICAMP: CampinasMiller, J.N., Miller, J.C., (2000) Statistics and Chemometrics for Analytical Chemistry, 4a Ed., , Prentice Hall: United KingdomChui, Q.S.H., Zucchini, R.R., Lichtig, J., (2001) Quim. Nova, 24, p. 374Barros Neto, B., Scarminio, I.S., Bruns, R.E., (2001) Como Fazer Experimentos: Pesquisa e Desenvolvimento Na Ciência e Na Industria, 2a Ed., , Ed. da UNICAMP: CampinasBrereton, R.G., (2000) Analyst, 125, p. 2125Jong, S., (1993) Chemom. Intell. Lab. Syst., 18, p. 251Lorber, A., Faber, K., Kowalski, B.R., (1997) Anal. Chem., 69, p. 1620Faber, N.M., (1998) Anal. Chem., 70, p. 5108Ferré, J., Brown, S.D., Rius, F.X., (2000) J. Chemom., 15, p. 537Goicoechea, H.C., Olivier, A.C., (2001) Chemom. Intell. Lab. Syst., 56, p. 73Faber, N.M., (1998) J. Chemom., 12, p. 405Curie, L.A., (1999) Anal. Chim. Acta., 391, p. 105(1997) International Conference on Harmonization, ICH Harmonised Tripartite Guideline - Validation of Analytical Procedures: Metodology, 62, p. 27463. , Fed. Regist(1995) International Conference on Harmonization, ICH Harmonised Tripartite Guideline - Text on Validation of Analytical Procedures, 60, p. 11260. , Fed. RegistStandards Practices for Infrared Multivariate Quantitative Analysis, , ASTM E 1655-00Moffat, A.C., Trafford, A.D., Jee, R.D., Graham, P., (2000) Analyst, 125, p. 1341Laasonen, M., Pulkkinen, T.H., Simard, C., Rasanen, M., Vuorela, H., (2003) Anal. Chem., 75, p. 754De La Pena, A.M., Mansilla, A.E., Valenzuela, M.I.A., Goicoechea, H.C., Olivieri, A.C., (2002) Anal. Chim. Acta, 463, p. 75Fernandez, J.A., Jin, L., Wahl, F., Faber, N.M., Massart, D.L., (2003) Chemom. Intell. Lab. Sys., 65, p. 281Voet, H.V.D., (1999) J. Chemom., 13, p. 195Borka, L., Lönmo, A., Winsnes, R., (1992) Pharm. Acta Helv., 8, p. 231Rustichelli, C., Gamberini, G., Ferioli, V., Gamberini, M.C., Ficarra, R., Tommasini, S., (2000) J. Pharm. Biomed. Anal., 23, p. 4