改进的PMP柱前衍生化方法用于单糖的组成分析(3)

1458高等学校化学学报　　　　　　　　　　　　　　　　Vol.27　行多糖的单糖组成分析.同时还对螺旋藻多糖SPPA21,SPPB21及SPPC21水解样品进行了衍生化分析,并采用112节中的方法求出各单糖间的摩尔比.3种多糖的单糖组成摩尔比与文献[4,5]中报道的结果一致.

3　结　　论

本文建立的糖类物质衍生化方法具有广阔应用前景,还可以用于碱性β消除反应解离O2寡糖链,对结构糖生物学研究有重要意义.

参　考　文　献

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[2]　XUJin(徐　瑾),ZHANGLing2Yi(张凌怡),LITong(李　彤)etal..ChineseJournalofChromatography(色　谱)[J],2003,

(4):363—366

[3]　MADing2Yuan(马定远),CHENJun(陈　君),LIPing(李　萍)etal..ChineseJournalofAnalyticalChemistry(分析化学)[J],

2002,30(6):702—705

[4]　WANGZhong2Fu(王仲孚),PENGZhi2Ying(彭志英),HUANGLin2Juan(黄琳娟)etal..ActaPharmaceuticaSinica(药学学报)

[J],2001,36(2):112—115

[5]　WANGZhong2Fu(王仲孚),PENGZhi2Ying(彭志英),HUANGLin2Juan(黄琳娟)etal..ChineseJournalDrugs(中国海洋

药物)[J],2001,(3):17—19

AnImprovedPMPDerig

ion

Xue2Fu13,HUANGLin2Juan,BAIQuan,JIAJing2Fen211

(1.LifeScienceCollege,KeyLaboratoryofMinistryofEducationforWestern

ChinaResourceBiologyandBiotechnology;

2.InstituteofModernSeparationScience,NorthwestUniversity,Xi′an710069,China)

Abstract　Animprovedcarbohydratederivatizationmethodemploying12phenyl232methyl252pyrazolone(PMP)wasdevelopedinthisstudy.Liquidammoniawasusedinsteadofsodiumhydroxideaqueoussolutiontoprovidethebasemediumforthederivatizationreaction.DerivatizationreactionandHPLCseparationconditionswereoptimized,includingreactiontime,reactiontemperatureandPMPconsumption.Thederivativesoffivereduc2ingmonosaccharideswerewellseparatedbyHPLC.Becauseweemployedammoniainsteadofsodiumhydro2xide,theexcessivevolatileammoniacanberemovedbyvacummdrying,thesederivativescouldbedirectlyanalyzedbyMALDI2TOF2MSwithoutdesaltingprocedure,possessingpotentialapplicationformonosaccharideandoligosaccharideseparationandsubsequentMSanalysis.ThismethodnotonlyincreasedtheMSdetectionsensitivity,butalsodecreasedsamplewastesduringpurification.Wesuccessfullyappliedthismethodtomo2nosaccharidecompositionanalysisofpolysaccharidesSPPA21,SPPB21andSPPC21purifiedfromSpirulinaPlatensis.

Keywords　HPLC;12Phenyl232methyl252pyrazolone;Derivatization;Saccharide

(Ed.:A,G)

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