吡嗪酰胺片近红外定量分析通用性模型的建立

Establishment of Universal NIR Model to Determine the Content of Pyrazinamide Tablets

目的建立近红外通用性模型,能对不同厂家吡嗪酰胺片的含量进行快速、无损地测定,有效监控其质量。方法采集9个浓度梯度的各3批自制样品及来源于20个不同厂家46批次的真实样品近红外漫反射光谱,并通过聚类分析方法确定校正集和预测集,考察不同预处理方法、谱段和光滑点数的影响,选择建立了最佳的吡嗪酰胺片的定量模型。结果 46个校正集样品经交叉验证建立校正模型,交叉验证均方根误差(RMSECV)为0.775,相关系数为99.4%;27个预测集真实样品的预测均方根误差(RMSEP)为0.962,预测值与真实值的相关系数为99.8%。预测值的平均回收率为99.9%(RSD为1.26%)。方法精密度RSD为0.84%(n=6),方法稳定性RSD为0.5%(n=5)。对6个厂家6批真实样品含量测定,相对误差均小于1.53%。结论所建立的定量模型能够对不同厂家不同规格的样品作出准确、快速的含量分析。

OBJECTIVE To found a universal near-infrared reflectance(NIR) model,to determine the content of pyrazinamide tablets from different manufacturers.METHODS Using cluster analysis method,diffuse reflectance spectra of 3 samples per concentration of 9 concentrations of simulated samples and 46 samples from 20 manufacturers were divided into calibration and validation groups.Then,the quantitative models were established using partial least squares(PLS) through selection of different wavelength ranges,preprocessing methods and smooth points.RESULTS The root mean square errors of cross validation(RMSECV) was 0.775,and determination coefficients is 99.4%.The root mean square errors of prediction(RMSEP) was 0.962.The correlation value between prediction and true of 27 samples in the validation groups is 99.8%,and the average recovery is 99.9%(RSD=1.26%).All the relative standard deviations of the true value and NIR prediction of 6 true samples from 6 manufacturers were no more than 1.53%.CONCLUSION The established NIR methods can be applied to accurate assay for the pyrazinamide tablets of different manufacturers.