川芎嗪衍生物TBN的HPLC含量测定方法VIP免费

QuantitativeHPLCAnalyticalMethodforTetramethylpyrazineDerivativeTBNStudentNameMAKSAUHANGStudentNo.2005055160MajorPharmacySupervisorProfessorWang,YuqiangDate(dd/mm/yyyy)25/05/2009暨南大学本科生毕业论文论文题目川芎嗪衍生物TBN的HPLC含量测定方法学院国际学院学系药学系专业药学姓名学号指导教师2008年5月25日StatementofOriginalityIherebydeclarethatthethesispresentedistheresultofresearchperformedbymepersonally,underguidancefrommysupervisor.Thisthesisdoesnotcontainanycontent(otherthanthosecitedwithreferences)thathasbeenpreviouslypublishedorwrittenbyothers,nordoesitcontainanymaterialpreviouslypresentedtoothereducationalinstitutionsfordegreeorcertificatepurposetothebestofmyknowledge.Ipromisethatallfactspresentedinthisthesisaretrueandcreditable.Signed:_________________Date：25-05-2009QuantitativeHPLCanalyticalmethodfortetramethylpyrazinederivativeTBNAbstract:Ahigh-performanceliquidchromatography(HPLC)methodforanewtetramethylpyrazinederivative,TBN,wasdeveloped.Analyticalperformanceparameterssuchaslinearity,precision,accuracy,specificity,limitofdetection(LOD)andlimitofquantification(LOQ)weredeterminedundertheguidelineofInternationalConferenceonHarmonizationQ2B[1].TBNwasanalyzedbyRP-HPLCwithC18columnusingmethanol-water(35:65)asmobilephase.Theflowrateis0.8ml/minandthedetectorwassetto295nm.Thelinearityofcalibrationcurveisgood(r2>0.999)andtheLODandLOQwere12.096ng/mland40.32ng/mlrespectively.Therelativestandarddeviation(RSD)ofprecisionandaccuracywere0.1245%and0.6895%,respectively,andthesamplerecoverywas99.08%(RSD:0.40%).ThismethodisreliableandeasyforTBNanalysis.KeyWords:tetramethylpyrazinederivative,TBN,HPLC川芎嗪衍生物TBN的HPLC含量测定方法摘要：目的：建立川芎嗪衍生物(TBN)高效液相含量测定方法。方法：选用C-18色谱柱；甲醇-水(35:65)；流速：0.8ml/min；检测波长为295nm。结果：TBN在12.42-310.5g/ml范围内线性关系良好(r2>0.999)；定量限和检测限分别为12.096ng/ml及40.32ng/ml；精密度及准确度RSD分别为0.1245%及0.6895%；加样回收率结果为99.08%(RSD:0.40%)。结论：本方法简便可靠，可作为TBN之定量分析方法。关键词：川芎嗪衍生物，TBN，高效液相Contents1.Introduction............................................................................................................................12.Materials................................................................................................................................22.1.Chemicals.....................................................................................................................22.2.Apparatus......................................................................................................................................33.ExperimentalMethod.............................................................................................................33.1.TBNstandardpreparation.........................................................................................................33.1.1.ColumnchromatographyforTBNpurification.................................................43.1.2.Semi-preparativecolumnchromatography......................................................................53.2.DevelopmentofHPLCmethodforTBN...............................................................................53.2.1.maxdetermination.......................................................................................................53.2.2.Optimizationof...