辛伐他汀片近红外漫反射光谱定量分析模型的建立.docVIP

药物分析杂志ChinJPharmAnal2009,29(6) 3—989—辛伐他汀片近红外漫反射光谱定量分析模型的建立 陈贵斌,陶巧凤,洪利娅,胡昌勤1112 (11浙江省食品药品检验所,杭州310004;21中国药品生物制品检定所,北京100050) 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1199517～544613cm-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212%～1619%,交叉验证均方根误差(RMSECV)为01110,确定系数为019993;12个验证集市售样品的预测均方根误差(RMSEP)为01137,预测值与真实值的相关系数为019981。方法精密度RSD为1109%(n=6),方法稳定性RSD为0162%(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。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、样品的含量均匀度分析。 关键词:近红外漫反射光谱;定量分析;中图分类号:R917:(2009)06-0989-05 Developquantitativemodelsfordeterminationofsimvastatin 3tabletsusingnearinfrareddiffusereflectancespectroscopy CHENGui-bin,TAOQiao-feng,HONGLi-Ya,HUChang-qin (11ZhejiangInstituteforFoodandDrugControl,Hangzhou310004,China; 21NationalInstitutefortheControlofPharmaceuticalandBiologicalProducts,Beijing,100050,China)1112 Abstract　Objective:Todevelopanearinfrareddiffusereflectancespectroscopymethodforrapiddeterminationofsimvastatintablets.Methods:Usingclusteranalysismethod,diffusereflectancespectraof10samplesperconcentra2tionof8concentrationsofsimulatedsamplesand30samplesoffourspecificationsfrom7manufacturersweredivid2edintocalibrationandvalidationset.Thesecondderivativewasselectedasthepreprocessingmethodand1199517-544613cmwasselectedasthefrequencyrange.Thequantitativemodelswereestablishedbypartialleastsquares(PLS)algorithm.Results:92batchesofsimvastatintabletssamples,concentrationrangesof212%-1619%,wereusedascalibrationset.TherootmeansquareerrorsofcrossvalidationRMSECVwas01110,andde2terminationcoefficientsRwas0199931TherootmeansquareerrorofpredictionRMSEPof12batchessamplesinvalidationsetwas011371Thecorrelationvaluebetweenpredictionandtrueof12truesampleswas0199811AlltherelativedeviationsofthetruevalueandNIRpredictionof10truesamplesfrom8manufacturerswerenotmorethan210%.Andtheresultsofcontentuniformitytestof2samplesfrom2manufacturerswereaccordantwithHPLCre