均匀设计法研究八角油β环糊精包合物的制备工艺.docx
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均匀设计法研究八角油β环糊精包合物的制备工艺.docx
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均匀设计法研究八角油β环糊精包合物的制备工艺
均匀设计法研究八角油β-环糊精包合物的制备工艺
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【摘要】 目的 研究β-环糊精对八角油的包合作用。
方法以挥发油包合率为指标,应用3因素6水平的均匀设计法,筛选出八角油包合物的最佳制备条件,即温度、研磨时间、样品与β-CD的比例。
结果实验得出最佳条件:
当温度为35.0℃,研磨时间为4.0h,八角茴香油与β-CD的比例1∶13.0(ml∶g)时,包合率为81.4%;红外测定包合作用是否完全。
结论优选得到的工艺结果稳定可行。
【关键词】八角油;β-环糊精;包合物制备;均匀设计 Abstract:
ObjectiveTostudytheinclusioncomplexofStaraniseoilwithβ-cyclodextrin.Methods3factorsand6levelsofconditionsforthepreparationoftheinclusioncomplexwereselectedbytheuniformdesign.TheratioofStaraniseoilintheinclusioncomplexwasusedascriterionintheseexperiments.Theinclusioncomplexwasmadebypestlingmethod.ResultsThebestconditionsoftheinclusioncomplexwerethat:
theratioofStaraniseoilandβ-Cyclodextrinwas1:
13.0(mL/g),andgrindingfor4.0hoursat35.0℃.Theratioofvolatileoilintheinclusioncomplexwasabout81.4%,andtheinclusioncomplexwasidentifiedbyIR.ConclusionTheoptimizedprocessisstableandhighlyefficient. KeywordsStaraniseoil;β-Cyclodextrin;Inclusionprocess;UniformdesignGuangxiisaChineseautonomousprovince,locatedinasubtropicalzone,southwestofChina.Inparticular,ithasextensiveresourcesofdifferentplants.Amongthem,thereisaspecialandcommercialproduct,essentialoil,whichiswidelyrecognized.Essentialoilsarethevolatile,fragrantsubstancesresidingintheflowers,fruits,leaves,androotsofmanyplants[1].Mostofthemareacomplexmixtureofchemicalconstituents,includingnitrogenandsulfur-containingmolecules,aromaticchemicals,andterpenes. ThefollowingoilsarethemostfamousandarefoundinlargequantityinGuangxi.Eucalyptusoi1hasbeenemployedinointmentsasatopicalcounter-irritantandtogetherwithmentholasaninhalation[1].StaraniseoilisthemainproductinthefruitsofIlliciumverum.Theplantcontainsremarkableessentialoil,whichisusedasflavoringandmedicinetocontrolcaught[2].Therelatedcontentoftrans-CinnamaldehydeinGuangxicinnamonoilwas11.58%,higherthanthatinYunnancinnamonoil.ThesetwoprovincesarethemainproducingareasofcinnamonoilinChina[3]. StaraniseoilisseparatedfromthefruitsofIlliciumverumHook.f.ThisplantisusedasflavoringsaswellasChineseherbalmedicine.InStaraniseoil,anethole(structurebelow)isthemajorcomponentwhichhasstructuresastheCistransisomersoccurringinnature.Remarkably,theTransisomerisalwaysbeingmoreabundant.Staraniseoilhasadistincteffectonraisingleucocytes(thewhiteblood-cells),soinAmericanpatent,ithasbeenappliedintheremedyforanti-leukemia.Anditalsohasbeenusedaspoultryfeedadditivecomposition[4].However,theeffectivenessdecreaseswithlongtimestorage,andbothphysicalandchemicalcharacteristicschangerelatively. β-CyclodextrinX(structureabove)hasbeenofinterestinnumerousindustriesincludingthepharmaceutica1field.Thisisduetotheirparticularstructureswhichimpartinterestingphysiochemicalproperties.Todayβ-CDisknownfortheirabilitytomolecularlyencapsulateawidevarietyofthedrugsintotheirhydrophobiccavity,resultingintheenhancementofwatersolubilityanddrugdissolution’srate[1].Theresultsofphysicochemicaltestsshowedthatafterinclusionthesolubilityandstabilityofpaprikapigment,thebindingabilityofβ-cyclodextrinforinclusioncomplexwithguestcurcumin,wasimprovedobviously[5~7].Soitisconsideredasagoodsupplementarymaterialforinjection[8]. Uptodate,althoughtheuniformdesignhasbeenwidelyusedinmanysynthesisandseparationfields[9],noreportsrelatedwiththeinclusioncomplexofStaraniseoilandβ-cyclodextrin,bythreefactorsandsixlevelsuniformdesign,hasbeenavailable.However,byusingthispracticaldesign,thevalueofStaraniseoilwoulddefinitelyenhanceandwouldbenefitmanypharmaceuticalandcommercialindustries. 1Reagentsβ-Cyclodextrin:
wasobtainedfromPharmaceuticalManufacturingFactory.Shanghai;Staraniseoil:
wasabstractedfromthefruitsofIlliciumverumHook.f.Alltheotherchemicalsandreagentsusedwereofthereagentgradeobtainedcommercially. 2Methods 2.1UseUniformDesignfortheexperimentsAmongmanyfactorsthateffectthepreparationofthecomplex,thetemperature,theratioofoilandCD,andthetimetomixtwocompounds,aremostimportant[10].Hence,U*(63)threefactorsandsixlevelsoftheuniformdesignwasconsidered.Toseedetails,intable1. 2.2Researchesintheinclusioncomplex 2.2.1Thecomplexformation:
Certainamountofβ-CDwasdissolvedin2~5timesofwater,lmlofoilwasdeludedby1mlofalcohol,andthephysicalmixtureoftheoilandβ-CDwasalsopreparedinthedifferentratiobygraduallymixingboth,groundfor1.5~4.0hoursatthesametemperature.Thecomplexwasfilteredandtheresidue(complex)waswashedwith30mlofabsolutepetroleumether,3times.Finallykeptinthedesiccatorsuntildriedandtheweightthenrecorded. 2.2.2Theinstrumentalerror:
1mlofpureoilwasaddedin500mLbottle.AndfollowedthestepsdescribedbyChinesePharmacopoeias(2000),thefirstmethod,calculatedtheerrorwithfollowingformandtheresultwas70.0%. Theinstrumentalerror=(thevolumeofthepureoilafterboiling/thevolumeofthepureoilbeforeboiling)×100% 2.2.3Evaluationofthecomplex:
Theβ-CDandStaraniseoilmixturewasevaluatedbytheratioofStaraniseoil.Andtheratioofoilwascalculatedbyfollowingequation:
Theratioofoil=theoilinthemixture/(theoiladdedinCD*theinstrumentalerror)×100%Note:
Therdumeoftheoilinthemixturewasmeasuredbythethesamemethodin2.2.2. 2.3IRdiffractionmanifestationSinceIRisaveryusefultooltoconfirmthepresenceofbothhostandguestcomponents[7],theinclusioncomplexwereexaminedtoverifytheinclusionprocedureshadbeencompletedbyIRdiffraction.Bothpurechemicalsandinclusioncomplexwereexaminedunderthesameconditions. 3Results 3.1TheexperimentaldataTheexperimentaldataunderuniformdesignwasshownintable1.Tab1ExperimentsofuniformdesignU*(63)&datatable(略) 3.2DatareturnanalysisUsedcomputertechnologyforreturninganalysis,eventuallygottheequationandparametersasbelow:
I=1B=-5.571405E-02F=15.98871I=2B=3.300001F=560.9341I=3B=10.81882F=2647.349I=6B=-0.4165219F=1307.24617B=-0.4502945F=2705.412R=0.9999538S=0.2815565Y=0.4502945+(-5.571405E-02)×X1+3.300001×X2+10.81882×X3+(-0.4165219)×X3×X3(Y-theoptimumratioofoil;X1-temperature;X2-timetogrind;X3-β-CD) 3.3SearchthebestconditionsEmployedspecializedcomputersoftware,theoptimummethod,forsearchingthebestconditionstoproducetheinclusioncomplex.Theresultswere:
X1=35.0X2=4.0001X3=12.96552Y=81.05204Confidentinternal:
Y’=Yu×s =81.1±1.96×0.2185565 =81.1±0.6 3.4TheexperimentalverificationVerifiedtheresultsfromoptimummethodbypreparinganewinclusioncomplexunderallfactorsandconditionsasfollowing:
X1=35.0℃;X2=4.0h;X3=1∶13.0(ml/g);Repeatedtheexperimentin2.2.2,calculatedtheratioofoilfromtheequationin2.2.381.4%. Sincetheratiooftheoilreachedthehighestandmaintainedinconfidentinternal(79.5~81.7%),thebestconditionswereprovenreasonableandreliable.Thiswouldbenefitsomepharmaceuticalandfoodindustries. 3.5IRverificationVerifiedbyIRtoprovewhethertheinclusionprocesseswereproperlycompleteornot.Andthediffractogramsshowbelow(Fig1,Fig2,andFig3).It’sobviousthatafterinclusion,mostofthetypicalstructureswhichappearinstaraniseoildisappear.AndthesestronglymanifestthattheinclusionbyCDisefficientandeffective. 4ConclusionUniformdesignforpreparingstaraniseoilandcyclodextrininclusioncomplexisreliableandpractical.Andtheresultsareoptimumandeasytoreinforceformodernindustries.Thurthermore,thestabilityandtheabilitytohidethestrongsmellofstaraniseoilafterinclusionwasimprovedobviously. 【参考文献】 [1]DayoAbdullah,PingQi-neng,LiuGuo-jie[J].JournalofChinaPharmaceuticalUniversity,1996,27
(2):
77. [2]ZhouJie-ming,LüGao-rong,ZhongXiao-qing,etal[J].ChineseTraditionalandHerbalDrugs,2005,28
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106. [3]HanYa-ming,JiangLin,HuangZheng-en,etal[J].CentralSouthPharmacy,2005,3(4):
216. [4]JEAN.R.Poultryfeedadditivecomposition[P].WO.9613175,1996. [5]LinRong-feng,WangLi,LiuXiang-feng[J].FoodResearchandDevelopment,2006,27(3):
191. [6]QiAi-di,LiLi,LiuYu[J].JournalofChinesePharmaceuticalSciences,2002,12
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15. [7]WangLu,WangJing-liang,DongChang-ming[J].ChineseJ.ofPolymerScience,2006,24(3):
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749. [9]JoaquinQuesada,MarieMorard,CarlosVaca-Garcia,etal[J].JournaloftheAmericanOilChemists’Society,2003,80(3):
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- 均匀 设计 研究 八角 环糊精 包合物 制备 工艺
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