mmol/l KOH (2):0~20 min,3mmol/l KOH;20.1~28min,200mmol/L KOH;28.1~ 33min,3mmol/L KOH :8!L/min; :30 ;.:, ( 1); : ; : / (Pd/H) ; :0.4!L (P

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1 (FENXIHUAXUE) ChineseJournalofAnalyticalChemistry DOI: /SP.J * (, ) ICS , 2mol/L min,, 50%, 84% ~104%,CapilaryCarborPacPA20,,10, 99.9%; 2.5~75!g/L ; ; 1 [1~3] [1,2] [4,5] [6], [7] [1,2,8], 6 [9~11] 10 - (CapilaryIC-PAD),CapilaryCarborPacPA20,, ICS-5000,OnGuardRP ( Dionex ); ( ); ( ); ( );0.22!m 10 : (Sigma ); (99.7%, J.T.Baker ); (, ); (Milipore, 18.2 MΩcm); ( ) 2.2 :CapilaryCarboPacPA20 (150mm 0.4mm);CapilaryCarboPacPA20G (35mm 0.4mm) : CapilaryEGC-KOH Cartridge KOH ; (1):0~15 min,8 mmol/l KOH;15.1~23 min,200 mmol/l KOH;23.1~28 min, ; * jil.li@thermofisher.com

2 mmol/l KOH (2):0~20 min,3mmol/l KOH;20.1~28min,200mmol/L KOH;28.1~ 33min,3mmol/L KOH :8!L/min; :30 ;.:, ( 1); : ; : / (Pd/H) ; :0.4!L (Pd/H ) Table1 Quadruple waveform forcarbohydratedetection (Pd/H Ref.Electrode) 1000 mg/l Waveformtime(s) Potential(V) Integration 5 mg/l, On mg/l, 10 mg/l Of 2,5,10,20,100, " " g ml, mL 4mol/L 1mL,, min, 5mL ; 0.5mL 10mL, 0.22!m OnGuardRP, 3mL, 3 [12] 3.1-1% CapilaryCarboPacPA20, CarboPac, (CapilaryEG), 200 mmol/l,, ph/ Ag/AgCl - / ph/ag/agcl 6 / CapilaryCarboPacPA20 CarboPac,,,, 10, (Fuc) (Rha) (Ara) (GlcN) (Gal) (Glc) 2 (Xyl) (Man)

3 9 : (Fru) (Rib) 1a b 1 1(a) 2(b) Fig.1 Chromatogramsofsamplesusingseparationmethod1 (a)andmethod2 (b) Fuc:fucose;Rha:rhamnose;Ara:arabinose;GlcN:glucosamine;Gal:galactose;GLC:glucose;Xyl: xylose;man:mannose;fru:fructose;rib:ribose. OH ",OH ", ;,OH " ph, pk a 12~14 ph, [13] 25, pk a=12.43,l pk a=12.04, 10mmol/L, ph<12 pk a, 2~10mmol/L, ; 8 mmol/l 8 mmol/l 1 pk a,oh ",, 3mmol/L, 3 mmol/l 2, 200mmol/L KOH 8min 3.3 H 2SO 4 HCl (TFA) [14] ;,, 1,2 4mol/L TFA 2mol/L,, 2mol/L 2mol/L 80,90,100, ( 2), 100

4 mol/L, 100, 30,60,90,120, min ( 3), 120 min ; 120 min 30min 50% 2 Fig.2 Eftectoftemperatureonhydrolysis Fig.3 Eftectoflastingtimeonhydrolysis 10 2 y (!Smin),x (mg/l) 10 (S/N =3) 2.5~75.0!g/L, 2 2 Table2 Linearequation,correlationcoeficientandlimitofdetection Linearrange (mg/l) Linearequation Correlationcoeficient (r) Limitofdetection (!g/l) Fuc 0.01~5.0 y=1.109x Rha 0.02~10.0 y=0.911x Ara 0.02~10.0 y=0.864x GlcN 0.02~10.0 y=1.833x Gal 0.02~5.0 y=0.920x Glc 0.05~12.5 y=0.946x Xyl 0.1~10.0 y=0.606x Man 0.1~10.0 y=0.345x Fru 0.2~10.0 y=0.171x Rib 0.1~5.0 y=0.571x , 3 3 [1,2], 3, 3 3, 84%~104% 50% 50%

5 9 : Table3 Determinationresultsandrecoveriesoflyciumbarbarumpolysaccharide Lyciumbarbarum polysaccharide Concentrationofspiked Amountof Proportion Concentration samplesolution sample ofmole ofsolution (mg/l) (mg/g) (%) Recovery (%) Fuc Rha Ara GlcN Gal Glc Xyl Man Fru Rib References 1 WANGZhan-Yong,YANSong,SHANGLi-Ying,YAO Cai-Lin.Amino Acidsand Biotic Resources,2008,30(1): 22-24,,,.,2008,30(1): ZHU Cai-Ping,ZHANG Min,ZHANGSheng-Hua.Chinese Traditionaland Herbal Drugs,2006,37(6): ,,.,2006,37(6): ZHUANG Wen-Bin,CHEN Ji-Sheng,LIN Jie-Shan.ChineseJournalof Modern Applied Pharmacy,2009, 26(13): ,,.,2009,26(13): JIANG Min,LEIDan,CHEN Ke-Quan,LIJian,YAO Jia-Min,WEIPing.ChineseJ.Anal.Chem.,2009, 37(4): ,,,.,2009,37(4): DAIJun,ZHUSong,TANGJian.Journalof Instrumental Analysis,2007,26(2): ,,.,2007,26(2): LIGuo-Liang,SUO You-Rui,SHIJun-You,SUN Zhi-Wei,LIU Yong-Jun.Food and FermentationIndustries, 2009,35(12):39-42,,,,.,2009,35(12): LIFa-Sheng,XU Heng-Gui,LIMing-Yang,LIU Hui.Physical Testing and Chemical Analysis PartB(Chemical Analysis),2008,44(4): ,,. -,2008,44(4): ZHENG Guo-Qi,LUJie,XU Xing,WANGJun.Journalof AgriculturalSciences,2008,29(3):1-4,,,.,2008,29(3):1-4 9 LIGuo-Qiang,YIN Ping-He,ZHAO Ling,OU Yun-Fu,HUANG Xue-Song.Journalof Instrumental Analysis, 2007,26(3): ,,,.,2007,26(3): RocklinR D,ClarkeA P,WeitzhandlerM.Anal.Chem.,1998,70(8): CaiY Q,LiuJS,ShiY L,LiangL N,MouSF.J.Chromatogr.A,2005,1085(1): Cees B, Manfred W,Carolien A M K,Victor B,Yan L,Chris P,ArndI,Cornelis H H,André M D. J.Chromatogr.B,2005,829(1-2): MOUShi-Fen,LIU Ke-Na,DING Xiao-Jing.Method and Applicationof Ion Chromatography,2005:76-80,,.,2005: TAO Le-Ping,DINGZai-Fu,ZHANGBu-Chang.ChineseJournalof Chromatography,1994,12(5): ,,.,1994,12(5):

6 DeterminationofMonosaccharideConstituentsinLycium Barbarum PolysaccharideUsingCapilaryIonChromatographywith PulsedAmperometricDetection LIJing *,LIRen-Yong,LIANGLi-Na (Thermo FisherScientific,Bejing100080,China) Abstract A methodforthedetermination often kindsof monosaccharidein Lycium barbarum polysaccharidewasestablishedusingics-5000capilaryicsystem.inthepretreatmentprocess,the typeand concentration of acid,the hydrolysis temperature and lasting time were selected or optimized.theoptimizedhydrolysisconditionwas100 lasting120minwith2mol/ltrifluoroacetic acidsolution.underthisconditiontherecoveryrateoffructosewasabout50%.recoveryrateofthe restmonosaccharidewas84% to104%.intheexperiment,newtypeofeluentgenerator,capilary CarborPac PA20 column,and improved capilary amperometric detection cel were used. The calibrationcurvesoftenkindsof monosaccharideshowedgoodlinearity withcorrelationcoeficient above0.999.the LOD is between 2.5 to 75!g/L.Itis suitableforthe determination of monosaccharideconstituentsinlyciumbarbarumpolysaccharide. Keywords Capilary ion chromatography; Pulsed amperometric detection; Lycium barbarum polysaccharide;monosaccharide (Received17January2012;accepted23April2012) 櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫 ( ),,, ; : 1 Aminuddin M,MilerJN.Talanta,1995,42(6): LU Xiao-Quan,MOJin-Yuan.ChineseJ.Anal.Chem.,1996,24(9): ,.,1996,24(9): DONGShao-Jun,CHE Guang-Li,XIE Yuan-Wu.Chemicaly Modified Electrodes.Beijing:SciencePress,1995: ,,. :,1995: SuchaL,KotrlyS.TranslatedbyZHOU Xi-Shun,DAIMing,LIJun-Yi.Solution Equilibriain AnalyticalChem- istry.beijing:people seducationpress,1979:25-30 SuchaL,KotrlyS.,,. :,1979: MalinowskiER.Factor Analysisin Chemistry.2nded.,New York:WileyInterscience,1991:40 6 StevensT M,MilerJrT E.U.S.Patent, , GB/T ,Determinationof Antimonyin Polyester Resinand Productsfor Food Containersand Pack- aging Materials.NationalStandardsofthePeople srepublicofchina..gb/t NATA.Technical Note #17-Guidelinesforthe Validationand Verificationof Chemical Test Methods,htp://

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