Kev txiav txim siab ntawm Cheebtsam los ntawm Herba Cistanehes Los ntawm Kev Tshawb Fawb Supercritical Fluid Extraction Nrog GC / MS
Mar 08, 2022
Hu rau: Audrey Hu Whatsapp / hp: 0086 13880143964 Email:audrey.hu@wecistanche.com
Intro
Supercritical fluid extraction (SFE) thev naus laus zis, nrog rau nws qhov tshwj xeeb zoo, yog qhov ntxim nyiam ua tus qauv npaj tshiab hauv kev tshuaj ntsuam chemistry thiab pib tsim ib qho kev tshuaj ntsuam xyuas lossis micro SFE thev naus laus zis. Nws tau raug pov thawj los ntawm kev sib cais zoo los ntawm kev sib cais thiab kev txiav txim siab ntawm cov kab organic sib txuas hauv ib puag ncig, khoom noj khoom haus, cov khoom siv ntuj tsim, thiab lwm cov qauv kev ua haujlwm nyuaj, Thaum lub sij hawm cov txheej txheem rho tawm, cov khoom hauv cov qauv tsis muaj kuab paug los yog ploj.
Hauv qhov kev sim no, cov pa roj carbon dioxide supercritical (los yog ntxiv methanol los ua tus hloov pauv) tau siv los ua cov kua dej, analytical SFE system tau siv, thiab ua ke nrog roj chromatography thiab huab hwm coj spectrometry, cov tshuaj lom neeg ntawm cov khoom tsis haum hauvCistanche deserticolaraug txiav txim. Cov txiaj ntsig tau txawv ntawm qhov tuaj yeem tau txais los ntawm cov txheej txheem ib txwm muaj.
Kev sim ib feem
1 supercritical kua extraction system
Cov cuab yeej tshuaj ntsuam xyuas SFE tau tsim thiab teeb tsa los ntawm peb lub chaw kuaj mob, thiab cov txheej txheem tau qhia hauv daim duab 1. Lub microextraction tank yog tsim los ntawm stainless hlau kua chromatography kem raj. Lub throttle raj yog elastic quartz lossis stainless hlau capillary nrog ib txoj kab uas hla ntawm 0.1mm. Nws lub luag haujlwm tseem ceeb yog tswj thiab kho tus nqi ntws thiab siab hauv cov txheej txheem rho tawm, thiab cov khoom rho tawm tau nkag mus rau hauv cov khoom siv los yog chromatographic system. Cov extract tau sau los ntawm hnyav sau rau chromatographic/mass spectrometry tsom xam. Cov kuab tshuaj yog isopropyl cawv.
Cov kua dej siv hauv qhov kev sim yog carbon dioxide (Beijing Experimental Plant) thiab qhov hloov pauv yog methanol (kev tshuaj ntsuam purity, Beijing tshuaj cog)
Cistanche deserticolayog ib co xim av xim av stems yuav los ntawm lub khw. Nws tau tawg thiab hauv av rau hauv granules kom nce qhov chaw saum npoo ua ntej kev rho tawm.
Weighted 0.5g ntawm cov qauv mus rau hauv lub tank extraction thiab txais cov txheej txheem dynamic extraction ntawm lub siab thiab kub. Qhov kev tshem tawm siab thiab ntws tus nqi yog tswj los ntawm kev ua haujlwm ntawm lub twj tso kua mis thiab lub tog raj kheej, thiab ntsuas qhov ntim ntawm cov kua.
Cistanche deserticola ntxiv
2 kev sib cais thiab kev txheeb xyuas ntawm cov khoom rho tawm
Cov khoom rho tawm tau muab cais thiab txheeb xyuas los ntawm capillary gas chromatography (CGC) thiab roj chromatography/mass spectrometry (GC/MS)
Hom roj chromatograph yog Perkin Elmer F17. Kab capillary yog 50mx0.24mm id, SE-30 kem (Shimadzu. Co.). FID, sib cais txhaj tshuaj, thiab kub-programmed ua haujlwm. Lub Varian 3400 GC tau txuas nrog ITD 800 ion ntxiab ntes (Finnigan lev CO) los ntawm kev sib cais qhib. Cov kab chromatographic yog 30mx0.25mln id, DB-5 kem (J & W Scientific). Lub linear tshaj tawm ntawm cov cab kuj roj (Nws) yog 30cm / s. Thaum tsis muaj kev txhaj tshuaj, qhov kub ntawm qhov chaw txhaj tshuaj yog 250 degree. Thawj qhov kub ntawm kab yog 50 degree, khaws cia rau 5min, thiab tom qab ntawd nce mus rau 300 degree ntawm qhov cua sov ntawm 5 degree / min.
Lub ion ntxiab ntes tau ua haujlwm nyob rau hauv tag nrho-scan electron cuam tshuam (EI) hom, nrog ntau yam ntawm 40 ~ 450u, thiab siv 1 thib ob rau txhua qhov scan. Lub ion ntxiab thiab kis kab mob kub yog 215 degree thiab 250 degree feem. Ntxiv rau El, tshuaj ionization (CI) pawg spectrometry tau txais nyob rau hauv tib lub chromatographic tej yam kev mob. CI cov tshuaj tiv thaiv roj yog methane. Xav txog qhov muaj nyob ntawm homologs thiab isomers, GC tag nrho ion flow diagram, thiab huab hwm coj spectrum ntawm C10-C14, C17-C20 n-alkane sib tov tau siv los ua cov qauv zoo sab nraud.
Cistanche deserticola extract
Cov txiaj ntsig thiab kev sib tham
Cistanche deserticolayog ib tug Yang txhawb cov tshuaj nrog complex Cheebtsam, thiab muaj ob peb cov lus ceeb toom ntawm nws volatile Cheebtsam. Ib txoj hauv kev los rho tawm nws cov khoom yog reflux cov tshuaj ethanol uas muaj hydrochloric acid thiab tom qab ntawd los ntawm cov txheej txheem tshuaj kho mob kom tau txais cov qauv uas tuaj yeem txheeb xyuas ncaj qha los ntawm chromatography. Nws cov tshuaj lom neeg tseem ceeb yog cov tshuaj hydrocarbon xws li heptadecane. Cov txheej txheem rho tawm yog yooj yim heev los ntawm CO2-SFE txoj kev, Nyob rau hauv cov xwm txheej ntawm 20MPa siab thiab 50 degree, tsuas yog kaum tawm milliliters ntawm CO2 kua, uas tuaj yeem ua tiav hauv 1h. Cov txiaj ntsig sib cais tau pom hauv daim duab 2
Nws tuaj yeem pom los ntawm daim duab 2 tias muaj ntau dua 30 lub ntsiab lus tsis sib haum xeeb sib cais los ntawm cov roj chromatography. Qhov hnyav molecular yog txiav txim los ntawm CI huab hwm coj spectrum. Lub Cheebtsam yuav roughly muab faib ua peb pawg:
Thawj qeb yog ib txwm alkanes ntawm C16 txog C28. Tsawg carbon hydrocarbons thiab lawv cov isomers kuj muaj nyob rau hauv extract, tab sis lawv cov ntsiab lus yog tsawg.
Qib thib ob yog esters. Peb lub ntsiab tseem ceeb yog dibutyl phthalate, dibutyl sebacate, thiab dioctyl phthalate, suav txog ntau dua 90 feem pua ntawm cov esters.
Cov qeb thib peb yog cov muaj oxygen thiab muaj nitrogen-muaj cov sib txuas nrog qhov hnyav molecular. Eugenol yog cov khoom tseem ceeb tshaj plaws. Qhov sib piv ntawm cov spectrometry retrieval ntawm lwm cov tebchaw xws li vanillin thiab isoeugenol kuj yog ntau tshaj 97 feem pua, thiab lawv cov chromatographic retention cov ntaub ntawv kuj zoo ib yam nrog cov ntaub ntawv. Lub CI loj spectrometry qhia tau hais tias lub MH ntxiv rau ion masses ntawm cov tebchaw nrog ncov tooj 8 thiab 12 yog 144 thiab 180 raws, Nws qhia tau hais tias ob leeg ntawm lawv yog cov tebchaw uas muaj ib tug nitrogen atom. Lawv yog 5-oxyproline methyl ester thiab 1-Methyl-2 (lH) - pyridine ethyl acetate feem. Los ntawm cov txiaj ntsig saum toj no, nws tsis yog qhov nyuaj kom pom tias cov khoom rho tawm ntawm SFE txawv ntawm cov ntaub ntawv.
Cov txiaj ntsig ntawm Cistanche deserticola
Cov pa roj carbon dioxide tuaj yeem yaj thiab tshem tawm cov polar compounds nyob rau hauv cov xwm txheej supercritical, uas muaj cov yam ntxwv ntawm cov kuab tshuaj polar. Txawm li cas los xij, ntxiv methanol, NO2 thiab lwm yam hloov pauv rau CO2 tuaj yeem txhim kho kev ua haujlwm ntawm CO2 rho tawm ntawm cov polar tebchaw. Hauv qhov kev sim no, ntxiv 3 feem pua methanol rau cov ntshiab CO2 ua rau kom cov qoob loo ntawm cov polar compounds (Fig. 3), thiab cov extraction npaum li cas ntawm alkanes kuj inhibited. Qhov no yog ib txoj hauv kev los txhim kho cov kev xaiv extraction ntawm supercritical kua los ntawm kev ntxiv modifiers. Vim tias hom thiab tus nqi ntawm kev hloov pauv tau tswj tau, qhov kev xaiv kuj tuaj yeem tswj tau raws li cov qauv.
Kev xaiv ntawm SFE kuj nyob ntawm nws lub xeev. Lub zog hnyav ntawm cov kua dej supercritical yog proportional rau nws qhov ntom (, hauv cov qauv no ρ Yog qhov ntom ntawm cov kua ρL yog qhov ntom ntawm cov kua hauv cov kua hauv lub xeev, thiab Pc yog lub siab tseem ceeb). Thaum qhov ntsuas kub yog tas li, cov kua dej ntom nce ntxiv tsis muaj kev cuam tshuam nrog kev nce ntawm cov txheej txheem siab, thiab solubility nce. Ntawm qhov tsis sib xws, thaum lub siab yog tsawg, kev ntom ntom, thiab rho tawm kev ua tau zoo. Daim duab 4 qhia tau hais tias thaum lub siab qis mus rau 9 MPa, tsuas yog ib qho me me ntawm cov kuab tshuaj xws li dibutyl phthalate yog muab rho tawm los ntawm covCistanche deserticolaqauv, Lub extraction efficiency ntawm lwm yam khoom yog tsawg heev. Nws kuj qhia tau hais tias lub solubility ntawm cov kua nyob rau hauv ib tug supercritical kua kuj muaj feem xyuam rau nws cov qauv thiab cov khoom.
Cistanche deserticola ntxiv
Cov txiaj ntsig kev sim ntawm SFE ntawmCistanche deserticolakuj qhia tau hais tias nyob rau hauv CO2 kua, txawm lub modifier yog ntxiv los yog tsis, nce qhov kub thiab txias tsis conducive rau kev txhim kho ntawm extraction efficiency. Tshwj tsis yog tias qhov ntom ntom tseem tsis hloov pauv, qhov kub siab yuav ua rau muaj kev cuam tshuam rau kev rho tawm ntawm qee yam khoom. Cov xwm txheej yooj yim rau CO2 kua rho tawm ntawm cov khoom tsis hloov pauv los ntawm cov qauv Cistanche deserticola yog qhov siab tshaj 20MPa thiab qhov kub ntawm 50 degree. Ntxiv methanol me me (3 feem pua) raws li kev hloov kho muaj txiaj ntsig zoo rau kev rho tawm ntawm cov polar tebchaw.
