盐酸雷诺希芬的电子电离质谱和快原子轰击电离(-)质谱研究

:2003207214;:2003209212:(1977),(),,,,E2mail:[e-mail]25220045JournalofChineseMassSpectrometrySocietyVol.25No.2May2004(-)1,2,2,2,2(1.,510632;2.,610061):,EI2MSFAB(-)2MSFAB(-)2MS,möz510[M+HCl+H]-möz509[M+HCl]-möz473[M]möz472[M-H];EIMS,möz473[M]+möz474[M+H]+,möz473[M]+C28H27NO4S,:;;(EIMS);(-)(FAB(-)2MS):O657163;R948:A:100422997(2004)022107203StudyonRealoxifenHydrochloridebyElectronIonizationMassSpectrometryandFast-atomBombardmentMassSpectrometryHANHai1,LIZhang2wan2,ZHANGQiang2,ZHENGHu2,WENLing2ling2(1.DepartmentofPharmacy,JinanUniversity,Guangzhou510632,China;2.DepartmentofPharmacy,SichuanUniversity,Chengdu610061,China)Abstract:Realoxifenhydrochlorideisanewsynthesiscompound,usedforthepreventionandtreatmentofosteoporosisandotherdiseasecausedbyosteoporosis.Forfurtherstudyonit,massspectrometrytechniques,suchaselectronionizationmassspectrometry(EIMS)andfast-atombombardmentmassspectrometry(FAB(-)2MS)canprovidevaluableinformationandwasusedfortheelucidationsofitsstructureandfragmentationpathway.Theresultsshowsthemolecularionpeakmöz510[M+HCl+H]-,möz509[M+HCl]-,möz473[M]-andmöz472[M-H]-weredetectedbyFAB(-)2MS;möz473[M]+andmöz474[M+1]+detectedbyEIMS.Andthemolecularformulaofrealoxifenhy2drochloridecouldbecertifiedasC28H27NO4S.Furthermore,thefragmentationpathwayofraloxifenhydrochlorideisalsoexplained.Keywords:massspectrometry;studyonrealoxifenhydrochloride;electronionizationmassspectrometry(EIMS);fast2atombombardmentmassspectrometry(FAB(-)MS),,[1](Realoxifenhydrochloride)Lilly,199712(FDA),19981,,,[62222(42)[b]232]2[42[22(12)][2,3],:C28H27NO4SHCl,509.5Da,,,,,Lilly,[2,3],42,42,,[1]1111VGAutospec3000:VGEIMS200(110-5Pa),70eV,3secödec,möz501000amu;FAB(-)2MS(Glycerol),5secödec,möz501000amu,1LA,25kV,112[2],11Fig.1Geometricstructureofrealoxifenhydrochloride2EI2MSFAB(-)2MS,HClM211FAB(-)-MSFAB(-)2MS,möz510[M+HCl+H]-,möz509[M+HCl]-,möz473[M]-möz472[M2H]-,509Da,,473,[M]-möz473,möz388[M-85]-,möz361[M-112]-(Glycerol,m=92),möz564,möz587möz495möz403möz311möz219möz127FAB(-)2MSFAB(-)2MS11FAB(-)MSTable1FAB(-)-MSassignmentsforraloxifenhydrochloridemözPresentingformö%Relativeabundance587[HCl+6Glycerol-H]-0.63564[M+Glycerol-H]-7.83510[M+HCl+H]-3.14509[M+HCl]-2.59495[HCl+5Glycerol-H]-;[M+Na-H]-5.71473[M]-24.05472[M-H]-39.73403[HCl+4Glycerol-H]-10.49388[M-85]-2.10361[M-112]-7.61311[HCl+3Glycerol-H]-21.91219[HCl+2Glycerol-H]-79.34127[HCl+Glycerol-H]-100.00212EIMSEIMSmöz473[M]+möz474[M+H]+,C28H27NO4SEIMS,CHO(29)möz316möz287,;7677möz269möz270möz211möz212,;CO(28)möz184möz241,;12811298möz345möz362möz375,;möz121,;möz83möz84möz85,EIMS,EIMS2801252Fig.2Fragmentationpathwayofrealoxifenhydrochloride,EI2MSFAB(-)2MS,EI2MSFAB(-)2MS,GCöMS,3(EIMS)(-)(FAB(-)2MS),,EI2MSFAB(-)2MS2:[1],.[J].,2001,22(6):275.[2],,,.[J].,2000,10(4):258.[3],.[J].,2002,18(1):1.[4].()[H].:,1989.[5].[M].:,2000.(128)ofGCöMS,butalsomakesacontributiontolastdevelopmentofeconomyinsocietyandpeoplehealth.4CONCLUSIONMATinporksamplesweredetermined.TheexperimentsuggestedthatMATcanbeanalyzedqualitativelyandquantitativelybyGCöMS.Itwasasuccessfulmethodologicaltry.REFERENCES:[1]ChuanhuanLUO,RongSHU.CorrespondenceofChinaPharmacologyAssociation[M].1997,14:2224.[2]WestWS,HancockD,MouleC,etal.RecentAdv.DopingAnal(8)Proc[C].ManfredDonikeWorkshop,CologneWorkshopDopeAnal,18th,2000:109118.[3]GrazelaV,RuxandraM,MiaL,etal.RecentAdv.DopingAnal(8)Proc.ManfredDonikeWorkshop,CologneWorkshopDopeAnal,18th,2000:215220.[4]ZhaoQing,HaoXiao2jiang,ChenYao2Zu,etal.AntitumorDiterpenoidsFromHedyChiumyunna2nenseandTheirPhotosensitizedOxidation[J].ZhiWuXueBao,1999,41(5):528530.9012:(-)