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    Experimental

Apr.2008,Volume2,No.4(SerialNo.5)JournalofChemistryandChemicalEngineering,ISS

    N19347375,USA

    ;Experimentalstudyofrefiningsolanesolfromcrude ;solanesolbysap0nificati0n

    ;GUMei-juan,GUZhenggui,LIBo,CHENQi

    ;(CollegeofChemicalandEnviromnentalScience,NanjingNormalzn,ersity,Nanjing210

    097,China)

    ;Abstract:ThesaDOnicaLi0nconditionsofcrudesolanesol ;(30%1werestudiediflthiswork.Theresultsshowedthecontent ;ofsolaneso1arrivedto41.9%:theoptimalconditionsof ;solanesolsaponificationwerethesaponificationtimeof3hours. ;thesaponificationtemperatureabout45*C.amountof2.5g ;NaOHandamountof30mLC,HOH.NEWTONLAPUSON

    ;methodwasappliedtoiterate.Thecorrelativeequationsprovide ;aneffectivebasisforfurtherresearchofrefiningsolaneso1. ;Keywords:solanesol;saponification;experimentand ;correlation

    ;1.Introduction

    ;Solanesol(so1),alongchainpolyisoprenoid

    ;alcohol,wasfirstisolatedfromfluecuredtobaccoin

    ;1956bvRowlandeta1.?.

    ;Itcanbeusedascardiac

    ;stimulant,lipidantioxidantandantibiotics,clinical ;trialsarealsodevelopingtheuseofsolanesolasan ;anticancerdrug[2-3].Nowadayssolanesolis

    ;extensivelyusedinmedicineandcosmeticfields ;becauseofitsvalueasasourceofisopreneunitsforthe ;synthesisofmetabolicallyactivequinones,suchas ;coenzymeQ1oandvitaminKanalogs[6-71.

    ;H(GH2C’-’CHCH2)9OH’

    ;l

    ;CH3

    ;Solanesolmainlyexistsinplants.

    ;ofSolanaceae

    ;family,especiallyintobaccoleaves,containsabout ;0.03%3%.whichoccursintheformoffreeand

    ;esterifiedforms[7-91.

    ;numerousauthorshave

    ;investigatedboththefleeandesterifiedsolanesol

;Correspondingauthor:GUZheng?gui(1962),male,Ph.D.,

    ;professor;researchfields:chemicalengineeringandtechnology

    ;Email:guzhenggui@njnu.edu.cn.

    ;contentoftobaccoandfoundconcentrationsranging ;upto4%inthedrytobaccoleaf.Theobjectiveofthis ;researchistodevelopamethodofsaponification ;esterifiedsolanesolforthecrudesolaneso1. ;2.Experiment

    ;2.1Materialsandreagents

    ;Thesolanesolcontentwasabout30%incrude ;solanesol,whichwasprovidedbyRixinCo.,Yangzhou, ;China.SolventsforHPLCmobilephaseswereof ;HPLCgrade,obtainedfromAgilentCo.,USA.Other ;reagentsappliedinthisresearchwereofanalytical ;grade.

    ;2.2Methodsofanalyzing

    ;TheAgilentHPLC1100systemwasemployedin

    ;thepresentstudy.AC18columnwasusedatcolumn ;temperatureof30?andtheinjectionvolumewas

    ;10gL.Abinarysolventmixtureofmethanol-ethanol ;(50:50,v/v)wasusedasmobilephaseand

    ;measurementswereperformed.

    ;3.Resultsanddiscussion

    ;3.1Effect0fsaponificationtime

    ;30mLethano1and2.5gNaOHwereinputtedin ;5.0gcrudeproductofSolanesol,thetemperatureof ;saponificationwascontrolledat45?.the

    ;saponificationtimesetat0.5,1,2,3,4h,thereforewe ;gainedanoptimalsaponificationtime.Fig.1shows ;thattheoptimalsaponificationtimeisabout3hours. ;53

    ;Experimentalstudyofrefiningsolanesolfromcrudesolanesolbysaponification

    ;,

    ;;

    ;

    ;C

    ;Specificationtime(1/h)

    ;Fig.1Effectofsaponificationtime

    ;3.2Effectofsaponificationtemperature ;30mLethanoland2.5NaOHwereinputtedin

    ;5.0gcrudesolanesol,thesaponificationtimewassetat ;3h,andthetemperatureofsaponificationwas ;controlledat35,4O,45,50,55?.Therefore,wegained

    ;apropersaponificationtemperature.Theresults

    ;showedintheFig.2,thepurityofsolanesolvariedwith ;theincreaseofsaponificationtemperature,atthesame ;timewefoundthatthecurvereacheditstopwhenthe ;saponificationtemperaturecameto45?.S0we

    asthesaponificationtemperature. ;choose45?

    ;

    ;

    ;=

    ;

    ;

    ;Specificationlemperaturef.r/?,

    ;Fig.2Effectofsaponificationtemperature ;3.3EffectoftheamountofNaOH

    ;30mLethanolwasinputtedin5.Ogcrude

    ;Solanesol,thesaponificationtimewassetat3hours, ;thetemperatureofsaponificationwascontrolled ;around45?.andtheamountofNaOHputtedintothe ;systemwas1.5,2.O,2.5,3.0,3.5g.Therefore,wefound ;anoptimalamountofNaOHputtedintothesystem.As ;theFig.3dottedlineshows,alongwiththeincreaseof ;amountofNaOH,thepurityofsolanesolvaries.We ;canalsofindoutthatwhentheamountofNaOHcomes ;to2.5g.thecurvereachesitstop.Soweput2.5gNaOH ;intothesystem.

    ;

    ;,

    ;}

    ;=

    ;C

    ;

    ;TheamounlofNaOH(m/g)

    ;Fig.3EffectoftheamountofNaOH

    ;3.4EfrectoftheamountofC2HsOH

    ;2.5gNa0Hwasinputtedin5.0gcrudeproductof ;Solanesol,thesaponificationtimewassetat3hours, ;thetemperatureofsaponificationwascontrolled ;around45?,theamountofC2H5OHputtedintothe ;systemwas10,20,30,40,5OraL.Thereforewcfound ;anaptitudeamountofC2HsOHputtedintothesystem. ;Fig.4showsthatthepurityofsolanesolwasincreased ;withtheincFeaseofamountofC,HoHonthewhoe,

    ;buttheascendingtrendwasgentlewhentheamountof ;C’2H5OHreached30mL.So30mlwastheoptimal

    ;amountofC,HOH.

;Theamoun!oft2H5OH(V/mp

    ;Fig.4EffectoftheamountofC2HsoH

    ;3.5Correlationandcomparison

    ;TheMinimumVariancemethodwasusedto

    ;correlatetheresultsbyNEWTON-LAPUSOmethod, ;E

    ;x

    ;

    ;perimentalstudyofrefiningsolanesolfromcrudesolanesolbysaponification

    ;therelativeerrorwaslistedbetweenexperimentaland ;correlativeresultinTable1,andtheseresultswere ;labeledinFigs.14,thecorrelativeequationswere ;listedasfollowing(1)(4).

    ;y=42.52615(42.5261536.08784)exp

    ;((O.46497x)2.3478)(1)

    ;y=33.62562+48.49908exp

    ;((x45.58092)/3.96006))2(2)

    ;y=33.63317+7.11477exp

    ;(-o.5((x2.60435)/0.41101)2)(3)

    ;y=40.31962/{l+exp[0.19672(x9.68855)}

    ;(4

    ;Table1Comparisonofexpedmentdataandcorrelationdata ;4.Conclusions

    ;SaDOnincatiOnOfthecrudeSolanesolwas

    ;discussedinthiswork,theoptimalsaponification ;conditionsweresummarizedinTable2,thesolanesol ;contentofthesaponificatedproductwasabout41.9%. ;theconditionsofsaDonificationontheeffectof ;solanesolcontentwerecorrelated,andtherelative ;errorsaresmal1betweenexperimentalandcorrelative ;results.Thecorrelativemodelwasprovidedforfurther ;investigationofrefiningsolaneso1.

    ;Table2Optimizationresults

    ;Data

    ;Amountofsolanesol(g)’

    ;Saponificationtemperature(?)

    ;Saponificationtime(h)

    ;AmountofNaOH(g)

    ;AmountofC2H5OH(mL)

    ;5.O

    ;45

    ;3

    ;2.5

    ;30

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    ;Experimentalstudyofrefiningsolanesolfromcrudesolanesoibysaponification

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