Aplicação de metodos quimiometricos de calibração de segunda ordem e transferencia de calibração na determinação simultanea de misturas de farmacos utilizando espectroscopia de fluorescencia molecular em fase solida / Aplication of chemometric methods of second order calibration and transfer of calibration for simultaneous determination of pharmaceutical mixture using solid-phase molecular fluorescence

AUTOR(ES)

Julio Cesar Laurentino Alves

DATA DE PUBLICAÇÃO

2009

RESUMO

In this work it was developed a methodology for determination of acetylsalicylic acid (ASA), paracetamol and caffeine in pharmaceutical formulations using solidphase molecular fluorescence and second order calibration methods. This methodology is usefull even in the presence of unknown interferences and with spectral overlap of the components in the mixture. Parallel Factor Analysis (PARAFAC) and Unfolded Partial Least Squares (UPLS) were used for second order calibration models development. Errors below to 5% were obtained for all compounds using an external validation set. Advantages not included in the reference methods such as low cost, no need of sample preparation, simple and fast analysis and no generation of waste, make this method very attractive, allowing to the simultaneous determination of compounds with good reproducibility and accuracy. Also, to propose a solution for the problem observed during the models development, due to change of sample matrix, the transfer of calibration was used. In this study it was used the method of Piecewise Direct Standardization applied to UPLS models constructed from samples of pharmaceutical mixtures of acetilsalicilic acid (ASA), paracetamol and caffeine with starch/cellulose 1:1 as excipient and samples with lactose as excipient, for accomplishment of the calibration transfer procedures. The transfer of calibration through Piecewise Direct Standardization method (PDS) applied to the UPLS calibration models provided excellent prediction results for pharmaceutical mixture in diferent excipient with relative errors less than 5%. From the values of RMSEP obtained for the results of the models of reference and the models of calibration transference, it was evaluated through a F test, that there is no difference, with 99% of significance level, in the results obtained by two models

ASSUNTO(S)

espectroscopia de fluorescencia formulação farmaceutica fluorescence spectroscopy pharmaceutical formulation

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