去甲斑蝥素片的制备工艺及其含量测定.docx

去甲斑蝥素片的制备工艺及其含量测定[摘要]目的建立一种去甲斑蝥素片的制备方法采用HPLC法检测去甲斑蝥素片的含量。方法以去甲斑蝥素为主药以淀粉、微晶纤维素（MCC）、乳糖为填充剂以羧甲基淀粉钠（CMS-Na）为崩解剂以聚乙烯吡咯烷酮-K30（PVP-K30）为黏合剂以硬脂酸镁为润滑剂制备去甲斑蝥素片。采用高效液相色谱法（HPLC）检测去甲斑蝥素片的含量；HPLC色谱条件为SpherigelODS-C18色谱柱；流动相：乙腈-pH3.1磷酸水溶液（10∶90）（V/V）；流速：1.0ml/min；柱温：25℃；检测波长：210nm；进样量：20μl。选定A（淀粉）、B（MCC）、C（CMS-Na）为考察因素采用U7（73）均匀设计通过溶出度指标优化去甲斑蝥素片的制备工艺。结果HPLC标准曲线方程：Y=925.374X-1778.8（r=0.9999）；线性范围：20～800μg/ml。日内精密度RSD：1.880%、0.172%、0.945%；日间精密度RSD：1.420%、1.126%、1.468%。低、中、高浓度的回收率分别为（98.77±1.24）%、（100.08±1.14）%、（99.59±0.58）%（n=5）。均匀设计回归方程为：K=-0.107-0.004A+0.017B-0.025C-0.0002B2+0.007C2（F=245.312P[关键词]去甲斑蝥素片；高效液相色谱；溶出度；均匀设计[中图分类号]R927[文献标识码]A[文章编号]1674-4721（2016）01（c）-0086-04[Abstract]ObjectiveToestablishapreparationmethodofNorcantharidintabletsandtodetectcontentofNorcantharidinTabletsbyusingHPLCmethod.MethodsNorcantharidintabletswerepreparedwithnorcantharidinasthemaindrugmicrocrystallinecellulose（MCC）andlactoseasthefillerssodiumcarboxymethylstarch（CMS-Na）asthedisintegratingagentpolyvinylpyrrolidoneK30（PVP-K30）asadhesive.ContentofNorcantharidintabletswasdetectedwiththemethodofHPLC；HPLCchromatographicconditionswere：SpherigelODSC18chromatographiccolumn；mobilephase：acetonitrile-pH3.1phosphoricacidaqueoussolution（10∶90）（V/V）；theflowrateof1.0ml/min；columntemperature25℃；detectionwavelengthof210nm；samplequantity20μl.ThefactorsA（starch）B（MCC）andC（CMS-Na）wereselectedU7（73）uniformdesignwasadoptedandpreparationofNorcantharidintabletswasoptimizedthroughthedissolutionindex.ResultsHPLCstandardcurveequation：Y=925.374X-1778.8（r=0.9999）；linearrange：20～800μg/ml.Theintra-dayprecisionRSDwere1.880%0.172%0.945%；inter-dayprecisionRSDwere1.420%1.126%and1.468%.Coefficientofrecoveryinlowmediumandhighconcentrationswereseparately（98.77±1.24）%（100.08±1.14）%（99.59±0.58）%（n=5）.UniformdesignregressionequationwasK=-0