Development and analytical validation of a multivariate calibration method for determination of amoxicillin in suspension formulations by near infrared spectroscopy

Abstract

This paper proposes a new method for determination of amoxicillin in pharmaceutical suspension formulations, based on transflectance near infrared (NIR) measurements and partial least squares (PLS) multivariate calibration. A complete methodology was implemented for developing the proposed method, including an experimental design, data preprocessing by using multiple scatter correction (MSC) and outlier detection based on high values of leverage, and X and Y residuals. The best PLS model was obtained with seven latent variables in the range from 40.0 to 65.0mgmL−1 of amoxicillin, providing a root mean square error of prediction (RMSEP) of 1.6mgmL−1. The method was validated in accordance with Brazilian and international guidelines, through the estimate of figures of merit, such as linearity, precision, accuracy, robustness, selectivity, analytical sensitivity, limits of detection and quantitation, and bias. The results for determinations in four commercial pharmaceutical formulations were in agreement with the official high performance liquid chromatographic (HPLC) method at the 99% confidence level. A pseudo-univariate calibration curve was also obtained based on the net analyte signal (NAS). The proposed chemometric method presented the advantages of rapidity, simplicity, low cost, and no use of solvents, compared to the principal alternative methods based on HPLC.