辛伐他汀片近红外漫反射光谱定量分析模型的建立___

Abstract Objective:To develop a near infrared diffuse reflectance spectroscopy method for rapid determination of simvastatin tablets.Methods:Using cluster analysis method,diffuse reflectance spectra of 10 samples per concentration of 8 concentrations of simulated samples and 30 samples of four specifications from 7 manufacturers were divided into calibration and validation set.The second derivative was selected as the preprocessing method and 11995.7-5446.3 cm^-1was selected as the frequency range.The quantitative models were established by partial least squares (PLS) algorithm.Results:92 batches of simvastatin tablets samples,concentration ranges of 2.2%-16.9%,were used as calibration set.The root mean square errors of cross validation RMSECV was 0.110,and determination coefficients R² was 0.9993.The root mean square error of prediction RMSEP of 12 batches samples in validation set was 0.137.The correlation value between prediction and true of 12 true samples was 0.9981.All the relative deviations of the true value and NIR prediction of 10 true samples from 8 manufacturers were not more than 2.0%.And the results of content uniformity test of 2 samples from 2 manufacturers were accordant with HPLC results.Conclusion:The established NIR methods can be applied not only to accurately and fast assay the various specifications simvastatin tablets of different manufacturers,but also can be used to test the content uniformity of a manufacturer's sample in process control.