川芎嗪衍生物TBN的HPLC含量测定方法

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(r20.999)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(r20.999)；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.OptimizationofHPLCconditionsforTBN...........................................................63.3.ValidationofHPLCmethod...................................................................................................73.3.1.Specificity.....................................................................................................................73.3.2.Linearity........................................................................................................................73.3.3.Precision........................................................................................................................73.3.4.LimitofQuantificationandLimitofDetection....................................................83.3.5.Range.............................................................................................................................83.3.6.Accuracy........................................................................................................................83.3.7.Stability..........................................................................................................................83.3.8.Recovery........................................................................................................................83.3.9.ContentAssay...............................................................................................................94.ResultsandDiscussion........................................................................................................95.Conclusion.........................................................................................................................19Acknowledgement....................................................................................................................20References.............................................................................................................