栀子药材提取工艺的近红外光谱实时控制方法研究

26,6Vol126,No16,pp10262103020066SpectroscopyandSpectralAnalysisJune,20061,2,23,2,11.,3100312.,100084,SIMCA,26,,SIMCA,,,;;SIMCA;:O65713:A:100020593(2006)0621026205:2005203206,:2005206216:973(G1999054404)(2002BA906A2923):,1974,3,,,,,,,[124],[5,6][7,8],,,,,,,,,,[9212],[13215],,[16,17],,,,(GardeniaJasminoides,Ellis),,,,SIMCA,,1SIMCA,1976Wold[18],,SIMCA,,,,N,p,MpN,q,nq,x(q)ik(i=1,2,,p;k=1,2,,nq),:x(q)ik=…a(q)i+Aa=1iaak+(q)ik…a(q)iqnqi,A,ik,iaakikqS(q)0=ik((q)ik)2/(nq-A-1)(p-A)1/2,xik(i=1,2,,p)q,,,,,Ca,(q)iu,x(q)u=…a(q)i+Aa=1iaCa+(q)iuq,,S(q)u=pi=1((q)iu)2/(q-A)1/2S(q)0S(q)u,q,SIMCAF,F=S(q)2uS(q)20FF0,FF0,uq,2211MicronEs2512A(9301670nm);(10mm,1m);InGaAs;,20ms,114nmNIRMicronOpticalSystems(MicroOpitcalSystemInc1);SIMCASNVMSC[9212]MAT2LAB513(MathworksInc1)212,,,,4046,110g,1,,46NIRTable146samplesextractedindifferentproceduresNo1ExtractionmethodSolventSolventvolume/mL1233ultrasonicextraction30minmethanol1034ultrasonicextraction30min90%methanol1035ultrasonicextraction20minmethanol936ultrasonicextraction35minmethanol1037ultrasonicextraction35minmethanol838ultrasonicextraction20minmethanol1039ultrasonicextraction15minmethanol1140ultrasonicextraction25minmethanol1241roughpowderwithoutsievedultrasonicextraction30minmethanol1042ultrasonicextraction30minmethanol843soakingfor10min,thenultrasonicextraction30minmethanol1044soakingfor15min,thenultrasonicextraction30minmethanol1045soakingfor20min,thenultrasonicextraction30minmethanol1046soakingfor200minat60methanol10213NIR2111Fig11OriginalNIRspectraofthesamplesofGardenia503311,,,S2G(1stor2ndderivative)(MSC,MultiplicativeScatterCorrection),(SNV,StandardNormalVariate),MSCSNV,(PRESS),272016Table2ModelperformancesfordifferentpretreatmentmethodsPretreatmentmethodOriginMSCSNV1stde12ndde11stde1+MSC2ndde1+MSCPRESS/10-43127313291994135615031926188Predictionaccuraterate91%94%91%98%85%100%94%,MSC,,,SIM2CA312[19],,PRESS,,,PRESS2(120)MSC,PRESS,3PRESS,3SIM2CAFig12Plotofpressvaluevsnumberofprincipalcomponents313,,,,[19],,3(120Fig13StandarddeviationsoftheNIRspectradataofthesamples),11401420nm31446,133,,4(86%),,133,,Fig143Dplotofscoresforallthesamples(86%varianceexplained)3:sample1=33;:sample33246120,,214611401420nm13,MSC,3SIMCA,315SIMCA5SIMCAF,120(),2146()SIMCA0101(F0112592),2133F,,,3446,,53446F,,3446,,4660,34,820126Fig15PredictedresultsofunknownsamplesandtrainingsetsamplesbySIMCAmodelBarsinblack()denotethecross2validationpredictedresultsoftrainingsetsamples,whilebarsinwhite()forthepredictedresultsofunknownsamples,andthelinerepresentsF0(99%confidence),,26,,Ward,6,,,,,3446,SIMCA,SIMCA,,Fig16Dendrogramfor26unknownsamplesbyWardsclusteringanalysisNumbersof1226onX2axisrepresentthesample21246respectively4SIMCA,,,,[1]CAOJin,RAOYi,SHENQun,etal(,,,).WorldScienceandTechnology/ModernizationofTraditionalChineseMedicine(),2001,3(4):20.[2]CAOJin,RAOYi,SHENQun,etal(,,,).TraditionalChineseDrugResearchandClinicalPharmacology(),2001,12(3):200.[3]StateFoodandDrugAdministrationBureauofChina().RequirementsforStudyingFingerprintofTradi2tionalChineseMedicineInjections(Draft)(()),2000.[4]CHENMin2jun,QUHai2bin,CHENGYi2yu(,,).ChemicalJournalofChineseUniversities(),2003,24:2181.[5]LUOGuo2an,WANGYi2ming,CAOJin,etal(,,,).WorldScienceandTechnology/ModernizationofTra2ditionalChineseMedicine(),2002,4(4):5.[6]CAOJin,WANGYi2ming,LUOGuo2an,etal(,,,).WorldScienceandTechnology/ModernizationofTra2ditionalChineseMedicine(),2002,4(5):32.[7]YANYu2zhen,XIEPei2shan,SONGLi2fei,etal(,,,).ChineseTraditionalPatentMedicine(),2004,26(8):603.[8]JIAXiao2bin,CHENYan,CAIBao2chang,etal(,,,).ChineseTraditionalPatentMedicine(),2003,25(11):866.[9]MachoM,LarrechiMS.TrendsinAnalyticalChemistry,2002,21(12):799.[10]LafargueME,FeinbergMH,DaudinJJ,etal.Anal.Bioanal.Chem.,2003,375(4):496.[11]McCaigTN.FoodRes.Int.,2002,35(8):731.[12]ThosarSS,ForbessRA,EbubeNK.Pharm.Dev.Technol.2001,6(1):19.[13]ZHAOChen,QUHai2bin,CHENGYi2yu(,,).SpectroscopyandSpectralAnalysis(),2004,24(1):50.[14]GUXiao2yu,WANGYan,XUKe2xin,etal(,,,).SpectroscopyandSpectralAnalysis(),920162004,24(2):155.[15]QUHai2bin,LIUXiao2xuan,CHENGYi2yu(,,).ChemicalJournalofChineseUniversities(),2004,25(1):39.[16]YANGNan2lin,CHENGYi2yu,QUHai2bin(,,).ActaChimicaSinica(),2003,61(5):742.[17]LIUQuan,QUHai2bin,CHENGYi2yu((,,).JournalofChemicalIndustryandEngineering(),2003,54(11):1586.[18]WoldS,SjostromM.Chemometrics:TheoryandApplication.KowalskiBREd.WashingtonDC:AmericanChemicalSociety,1977.242.[19]LIUShu2shen,YIZhong2sheng(,).BasicChemometrics().Beijing:SciencePress(:),1999.127,145.StudyonReal2TimeControlofExtractionProcedureofFuritusGardeniabyNearInfraredSpectroscopyYANShi2kai1,2,LUOGuo2an23,WANGYi2ming2,CHENGYi2yu11.DepartmentofChineseMedicineScienceandEngineering,CollegeofPharmaceuticalSciences,ZhejiangUniversity,Hangzhou310031,China2.DepartmentofChemistry,TsinghuaUniversity,Beijing100084,ChinaAbstractAnewapproachtothereal2timecontrolofextractionproceduresbasedonfiberopticnearinfraredspectroscopy(NIR)wasdescribed.VariousextractionsamplesofgardeniawererapidlyscannedbyNIR,andtheSIMCAmonitoringmodelwasde2velope