Transferência de calibração de misturas de pós para comprimidos intactos: um novo uso em análise farmacêutica para uma ferramenta quimiométrica conhecida

Abstract

The use of chemometrics and near-infrared (NIR) spectroscopy in pharmaceutical analysis has increased in recent years and is slowly gaining access to the rigorous pharmacopeic methods. However, quantitative multivariate modeling requires a large number of samples, with wide range of active pharmaceutical ingredient concentration. Although the use of multivariate calibration reduces the cost of analysis, comparing to univariate methods, the cost of producing different samples of tablets outer of productions specifications may be high. In the other way, samples of powder mixtures can be produced in small scale reaching a low cost of sampling. Due to this, the calibration transfer, which is a chemometric tool used to correct models constructed from samples measured in different instruments, from powder mixtures to intact tablets allows a reduced cost modeling and the possibility of using the same model in different steps of the productions quality control.This work developed a partial least squares (PLS) model to quantify nevirapine and studied the calibration transfer from powder-mixture model to intact tablet spectra using direct standardization methods (PDS piecewise direct standardization and DWPDS double window piecewise direct standardization). The working range was 83.0 to 113.9% of nevirapine target value. RMSEP (root mean square error of prediction) of tablets was reduced from 2.0 to 1.7 %. The calibration transfer between different physical forms is an original idea that was effective from powders mixtures to tablets, opening perspectives to determinations in other matrices, since the sample can be obtained in different forms.