info:eu-repo/semantics/bachelorThesis
Desarrollo y validación del método analítico por espectrometria nir y calibracion multivariable para la cuantificación de captopril en tabletas 25mg”
Fecha
2011Autor
Saldaña Calderón, Luis Alberto
Institución
Resumen
The present study was conducted to develop and validate the analytical method by NIR spectrometry and Multivariable Calibration for quantification of Captopril 25 mg tablets. The developed method makes use of NIR spectroscopy (Near Infrared) associated with the Multivariable calibration technique based on PLS-1 (Partial Least Squares). In the construction of the model, synthetic tablets were prepared from a Doptimized experimental design with captopril concentration range from 80% -120% larger than the tablets produced by Induquímica Laboratory. NIR spectra were recorded in the range of 4000-10000 cm-1 with a Perkin Elmer NIR spectrometer with Fourier transform, with diffuse reflectance accessory for solids and Teflon as a blank. The reference method for the determination of captopril concentrations in the samples was based on the HPLC technology (high performance liquid chromatography). The new method NIR-PLS-1 developed is fast, accurate and it doesn’t consume reagents harmful to the environment. Its main and remarkable advantage is not to need the solubilization of samples which makes the control the content of captopril in all tablets possible, without destroying them, as it happens in an analysis by HPLC. This method was developed and validated based on some figures of merit of ASTM E1655 05 and American Pharmacopoeia USP 32, what allow it to be certified later by Induquímica Laboratory, which has shown interest to implement it in the process quality control. The method showed good performance and results comparable to the HPLC reference method according to USP, being the standard error of calibration and validation 0.57 mg and 0.68 mg, respectively. The linearity test showed a coefficient of determination r2 of 0.9753, all values obtained by the reference method were within their limits of estimation and the significance of the bias test yielded a value of 0.4166 tcalculado, what indicates that the method provides the same results as the reference method. The method showed good accuracy, as it was assessed according to the repeatability of the system, repeatability of the method and intermediate precision, yielding a CV of 0.52%, 3.48% and 3.83% respectively, results conforming to their specifications. These validation parameters allow the analytical method developed for NIR spectroscopy and multivariate calibration as validated for the quantification of Captopril 25mg Tablets