摘要
目的:采用近红外漫反射光谱分析技术和化学计量学的方法对小规格的辛伐他汀片进行快速无损的含量测定和含量均匀度检查。方法:采集8个浓度梯度的各10批自制样品及来源于7个不同厂家30批次4个规格的市售样品的近红外漫反射光谱,并通过聚类分析方法确定校正集和验证集,光谱预处理方法为二阶导数,谱段范围为11995.7～5446·3cm-1,回归方法采用偏最小二乘法。结果:92个校正集样品经交叉验证建立校正模型,浓度范围为2.2%～16.9%,交叉验证均方根误差(RMSECV)为0.110,确定系数为0.9993;12个验证集市售样品的预测均方根误差(RMSEP)为0.137,预测值与真实值的相关系数为0.9981。方法精密度RSD为1.09%(n=6),方法稳定性RSD为0.62%(n=5)。对8个厂家10批4个规格市售样品含量测定,相对偏差均小于2%。对2个厂家的2批样品的含量均匀度检查结果与HPLC法结果无明显差异。结论:建立的定量模型能对不同企业生产的小规格的辛伐他汀片作出准确、快速、无损的定量分析,可用于药品的现场快速分析和某一厂家样品的含量均匀度分析。
Objective：To develop a simvastatin tablets. Methods： Using tion of 8 concentrations of simulated near infrared diffuse reflectance spectroscopy method for rapid determination of cluster analysis method,diffuse reflectance spectra of 10 samples per concentrasamples 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^-1 was 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. l l0,and de- termination 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.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2009年第6期989-993,共5页
Chinese Journal of Pharmaceutical Analysis
基金
浙江省分析测试项目(2007F70006)
关键词
近红外漫反射光谱
定量分析
含量均匀度检查
辛伐他汀
near - infrared diffuse reflectance spectroscopy
quantitative analysis
content uniformity
simvastatin
