红外光谱法测定咖啡因的含量

©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.(,230039):.,,,,.ATR-FTIR.,,.,.:10250mgg-1,r=0.9953;HPLC;98.0%100.5%,,,.:;,;;;:O657.33:A:1000-2162(2009)01-0085-05(Caffeine,),,,.,.,[1][1][2-3].,,.[2],[4].[5-6],272274nm,.[7],,,,.[8-9](ATR-FTIR),,.,(ATR-FTIR),,.(AttenuatedTotalReflectance,ATR),,[10],,.,,,.11.1:FT-IR,NEXUS-870,Nicolet;:VarianProstar210,Varian;:FA1004,.(AR),(AR),(99.9%,),:2008-10-07:(2005KJ100);:(1964),,,,.20091331()JournalofAnhuiUniversityNaturalScienceEditionJanuary2009Vol.33No.1©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.::32,:4cm-1.1.21.2.1,,.1.2.2,6KBr0.08g0.01g,1.0mg3.7mg7.1mg10.0mg16.0mg27.7mg(0.0002g),,.,,3,.22.112,,1698cm-1,,61655cm-1[11],16981655cm-1,,1698cm-1,,2117cm-1,,2.OMNIC,,.2.2[9],(3),,3,,(123456),4,Y=-0.1250+0.02618X,Yh2/h1,X;r=0.9953,,,.68()33©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.(29.33mgg-1)(112.40mgg-1)(203.10mgg-1),(RSD)0.52%0.34%0.26%,.1/(mgg-1)/(mgg-1)RSD/%29.10,29.35,29.27,29.41,29.5029.330.52112.30,112.65,112.48,111.80,112.79112.400.34203.75,203.52,202.50,202.67,203.06203.100.262.4,98.00%100.50%(2),.2/(mgg-1)/(mgg-1)/(mgg-1)/%8.1010.0017.9098.008.1020.0027.9099.008.1040.0048.30100.502.510mg,80mg10mg,,,,3,(5).(1698cm-1)h2=0.059;(2117cm-1)h1=0.030,h2/h11.967.h2/h1,C=79.91mgg-1,:=79.91%.781,:©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.(gmL-1)/counts1103095262205483543309232724401339428550153963566503656,,,:Y=34512.9X-43344.6,r=0.9940,7,25.00gmL-1HPLC.:C=20.10gmL-1,C0=25.00gmL-1,HPLC80.40%,(79.91%-80.40%)/80.40%=-0.61%,,.3ATR,,.(ATR),Ge,,,.,.:,,;,;,;;;,;,;,.HPLC88()33©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.=0.9953,,:1%.:98.0%100.5%.ATR,,.:[1]HorieH,NesumiA,UjiharaT,etal.Rapiddeterminationofcaffeineintealeaves[J].JournalofChromatographyA,2002,942(2):271-273.[2]ParadkarMM,IrudayarajJ.RapiddeterminationofcaffeinecontentinsoftdrinksusingFTIR2ATRspectroscopy[J].FoodChemistry,2002,78(2):261-266.[3],,.[J].:,2007,23(1):71-74.[4],,,.[J].,2001,19(5):398-402.[5],,,.[J].,2005,17(6):636-637.[6],.[J].:,2000,23(3):309-311.[7],.[J].,1998,2(2):36-38.[8],,,.[J].,2006,23(2):377-379.[9],.A[J].,2005,40(20):1587-1589.[10],,.[M].:,2002:23-125.[11],.FTIR[J].,2008,6(3):46-48.DeterminationofcaffeinebyATR2infraredspectroscopyYANGJie,SONGJi2mei,FANGFang(CollegeofChemistryandChemicalEngineering,AnhuiUniversity,Hefei230039,China)Abstract:Inthisthesis,asimple,rapid,solvent2freemethodhasbeenputforwardandestablishedforthequantitativeanalysisofcaffeine.Referencesubstancesuitableforcaffeinewaspreciselyweighed,byaddingthesamevolumeofpotassiumferricyanideasaninternalstandardsubstanceandKBrusedasadiluentandmixingthemuniformly.Thenaserieswasprepared.TheATR2FTIRabsorptionspectrumsoftheseriesweremeasured.Thecharacteristicabsorptionpeakofcarbonylincaffeineandthecharacteristiccyan2peakinpotassiumferricyanideasthepeaksforquantitativeanalysiswereselectedforthedetermination.Bycalculatingtheratioofthetwopeakheightsbetweencaffeineandpotassiumferricyanide.Weconcludedthatthetwopeakheightratioshowedagoodlinearity(r=0.9953)withtheconcentrationofcaffeineinthesolidmixtureattherangeof10250mgg-1.Thereforetheconcentrationoftheneedcheckingcaffeinewasobtained.Theaveragerecoverywas99.05%.TheexperimentresultofATR2FTIRwasbasicallyinaccordwiththatofHPLCmethod.TheATR2FTIRmethodforthequantitativeanalysisofcaffeineisofhighaccuracyandreliability.Thismethodcouldbeusedintherapidquantitativeanalysisforcaffeineandothersaswell.Keywords:ATR2FTIR;caffeine;quantitativeanalysis;potassiumferricyanide;internalstandardsubstance;regressionanalysis:,981,: