Chemistry sab chromatography
2.Chromatogratographic Kem (Hloov Hom)
3.Chromatographic Tag (phau ntawv)
*** Daim ntawv teev npe rau tag nrho saum toj no, nug peb kom tau txais
Hauj lwm lawm
Kev tsis
Kem chromatography, ua ntej qhia los ntawm Mikhail Dwett nyob rau hauv 1906, tau hloov kho rau hauv cov khoom sib txuas ntau yam raws li lawv cov kev sib txuas lus sib txawv nrog cov theem nyob ruaj khov. Nws cov ntawv thov luv cov khoom siv tsis ntev los yog cov khoom siv rho tawm, tshuaj kho tes, ib puag ncig xyuas, thiab cov ntaub ntawv kawm txuj ci. Cov ntawv sau no tshawb txog cov ntsiab cai, cov tswv yim, thiab kev tsav tsheb tsav tsheb chromatography cov kev siv hluav taws xob txuas ntxiv hauv kev kawm tab.
Chaw ua uas tsis tau haus
Kev siv
Chemistry sab chromatography, raws li kev sib cais tseem ceeb thiab tsom xam cov txheej txheem, muaj ntau cov kev siv hauv kev ua haujlwm ntawm Chemistry. Nws yog raws li kev faib cov khoom sib txawv ntawm cov tshuaj sib txawv ntawm cov theem nyob ruaj khov ntawm cov theem hauv tsev thiab ua tiav qhov sib cais thiab ua kom huv ntawm cov khoom sib xyaw los ntawm chromatographic txhua.
Hauv cov organic synchises, (CC) yog tus qauv tseem ceeb rau kev txiav txim siab cov tshuaj tiv thaiv. Tom qab nqa tawm cov koob txheej txheem ntawm cov khoom siv hluav taws xob hauv tsev kawm ntawv hauv chav kuaj, ntsuas feem ntau tau txais cov khoom sib xyaw, cov khoom siv raw, los ntawm cov khoom lag luam, thiab lwm yam. Txij ntawm no, (CC) ua lub luag haujlwm tseem ceeb. Los ntawm txhaj cov tshuaj tiv thaiv sib tov sib xyaw rau hauv cov chromatographic kem, ntau lub zog yuav txav ntawm qhov sib txawv ntawm cov khoom sib txawv thiab cov khoom sib txawv ntawm cov tshuaj sib txawv, yog li ua tiav kev sib cais. Cov kws tshawb nrhiav tuaj yeem pom meej meej cov duab siab thiab cov kev huv ntawm cov khoom lag luam los txiav txim siab seb qhov kev hloov pauv tau ua tiav. Piv txwv li, nyob rau hauv cov txheej txheem ntawm synthesizing kev siv tshuaj nyob nruab nrab tshiab los ntawm cov hom phiaj sib xyaw ua ke, muab cov pov thawj ncaj qha rau kev ua haujlwm zoo tshaj plaws hauv cov organic synthemes.
Daim ntawv thov hauv tshuaj ntsuam xyuas
Hauv kev txheeb tshuaj ntawm kev tsom xam, kab chromatography yog siv dav rau kev ua yeeb yam kom paub cov tshuaj, thiab kev sib cais ntawm cov txheej txheem synthesis. Lub purity ntawm ib qho tshuaj yog ib qho ntawm cov ntsuas tseem ceeb ntawm nws qhov zoo. Los ntawm kab chromatography, impurities nyob rau hauv cov tshuaj tuaj yeem sib cais los ntawm lub ntsiab lus tseem ceeb, yog li tseeb txiav txim siab lub purity ntawm cov tshuaj. Qhov no yog qhov tseem ceeb tshaj plaws rau kev ua kom muaj kev nyab xeeb thiab ua tau zoo ntawm cov tshuaj. Ib qho ntxiv, kab chromatography kuj tseem siv hauv cov tshuaj metabolism tshawb fawb cais thiab txheeb xyuas cov metabolites ntawm cov yeeb tshuaj hauv vivo. Cov metabolites yog cov muaj txiaj ntsig zoo hauv kev nkag siab txog cov txheej txheem biotransformation ntawm cov tshuaj, ntsuas lawv cov tshuaj lom thiab kev ua tau zoo, thiab lwm yam. Nyob rau hauv cov txheej txheem ntawm cov tshuaj synthesis, kem chromatography kuj tseem siv tau cais thiab txhawb kev txhawb nqa cov tshuaj zoo ntawm cov tshuaj synthesis.
Nrog rau kev txhim kho nrawm dua ntawm kev lag luam thiab hauv nroog, ib puag ncig cov teeb meem papanization yog ib puag ncig ua dhau los ua loj. Daim ntawv thov ntawm kab chromatography nyob rau ib puag ncig saib xyuas muab cov kws tshawb fawb nrog cov cuab yeej muaj zog los kuaj pom thiab txheeb xyuas cov pa phem nyob hauv ib puag ncig. Piv txwv li, roj chos chromatography yog feem ntau siv los txheeb xyuas cov organiccov (vocs), uas yog cov kuab lom uas muaj kuab lom thiab cov neeg siv khoom. Los ntawm kev sib cais thiab kev tsom xam ntawm cov roj chromatography, kev pom zoo thiab cov qauv kev tshawb fawb tau raug teeb meem rau huab cua zoo thiab cov cai tswj hwm ib puag ncig thiab tsim cov txheej txheem ib puag ncig. Tsis tas li ntawd, kua cov tshuaj chromatography kuj tau siv los tshuaj xyuas cov pa phem organic, thiab lwm yam hauv dej. Ion txauv cov chromatography txhua feem ntau siv los tshuaj xyuas ions hauv kev nkag siab cov kab mob dej zoo, thiab kev tsim cov phiaj xwm dej qias neeg.
Daim Ntawv Thov hauv Kev Nyab Xeeb Khoom Noj
Khoom noj khoom haus nyab xeeb yog qhov teeb meem tseem ceeb muaj feem cuam tshuam nrog tib neeg kev noj qab haus huv thiab kev ruaj ntseg. Daim ntawv thov ntawm kem chromatography hauv kev nyab xeeb zaub mov muaj kev txhawb nqa muaj zog rau kev ntes cov khoom muaj teeb meem hauv cov zaub mov. Piv txwv li, kua chromatography txhua feem ntau siv los xyuas cov tshuaj tiv thaiv kev phom sij xws li cov tshuaj ntxiv, thiab hlau hnyav hauv cov zaub mov. Yog tias cov tshuaj no tau siv nyob rau hauv cov txheej txheem ntau dhau los lossis nyob hauv cov nyiaj ntau dhau, lawv tuaj yeem ua kev hem thawj rau tib neeg kev noj qab haus huv. Los ntawm kev sib cais thiab kev tsom xam ntawm cov kua chromatography, cov ntsiab lus ntawm cov tshuaj phem no tuaj yeem txiav txim siab, muab kev tshawb fawb txog kev saib xyuas kev nyab xeeb. Ib qho ntxiv, cov roj chos chromatography yog siv los kuaj cov khoom noj muaj zog hauv cov khoom noj, thiab lwm yam.
Tshuaj lom neeg siv cov khoom siv yog cov tshuaj tseem ceeb uas siv rau cov cuab yeej tseem ceeb, ntsuas qhov tseeb ntawm cov txheej txheem thiab kev ntseeg tau ntawm kev ntsuas ntsuas. Kab chromatography ua si lub luag haujlwm tseem ceeb hauv kev npaj cov tshuaj siv. Los ntawm kab chromatography sib cais thiab ua kom huv, impurities tuaj yeem raug tshem tawm kom tau txais cov tshuaj uas muaj raws li cov qauv thoob ntiaj teb. Cov tshuaj zoo-huv no ua si lub luag haujlwm tseem ceeb hauv kev noj tshuaj sloichiometry, tswj hwm zoo, thiab lwm yam. Lawv siv dav hauv kev ntsuas hluav taws xob ntawm ntau txoj kev ntsuas thiab cov twj paj nruag, kom ntseeg tau qhov tseeb thiab kev sib piv ntawm cov tshuaj ntsuam xyuas tshuaj lom neeg. Ib qho ntxiv, kem chromatography kuj tseem siv tau los npaj cov kev sib xyaw ua ke thiab cov qauv tshwj xeeb, muab kev txhawb nqa zoo rau kev tshawb fawb hauv kev tsom ntsuas tshuaj lom neeg.
Kawm Txog Cov Ntaub Ntawv
Txoj Kev Kawm Kev Kawm Kev Kawm 1: Purification ntawm Kev Siv Tshuaj Nruab Nrab Siv Hluav Taws Xob Siv Hluav Taws Xob Chairal Nyob Ruaj
1.1 Tom Qab
Ib lub tuam txhab ua lag luam nrhiav kom cais tawm cov (r) -enantiomer ntawm triazole-raws Kinase inhibitor (compound x) rau kev sim tshuaj. Cov kev sib tw sib xyaw ua kom pom tau xws li 50% qis dua vim yog (s) -Tantantiomer qhov kev ua tsis zoo.
1.2 vib this
Theem nyob ruaj ruaj: Chiralpak Ad-H (Amylose Tris- (3, {3}} dimethylphenylcarbamate) coated on silica).
Mobile theem: Hexane-isopropanol (95: 5, {3}}. 1% diethylamine).
Tus txheej txheem:
Yaj 500 mg ntawm Racemic sib xyaw X hauv 2 ml ntawm dichhlorometeane.
Thauj cov qauv rau hauv 250 × 10 hli kem.
Eluted thaum 1 ml \/ min, khaws 5 ml feem.
Kuaj pom peaks ntawm UV ntawm 254 nm.
1.3 cov txiaj ntsig
Lub (R) -enantiomer eluted ua ntej (cia sij hawm: 12.3 feeb), tom qab (s) -enantiomer (18.7 min).
Raug cais tawm los: 42% (R) -enantiomer, 38% (s) -enantiomer.
Enantiomer ntau dhau (EE): 95% (txiav txim siab los ntawm Chiral HPLC).
1.4 qhov tseem ceeb
Lub lim dej (r) -enantiomer qhia tawm 10- fold ntau dua potency hauv vitro, tsuas yog qhia nws nce qib kuv sim.
► Kev tshawb nrhiav Case 2: Kev tsom xam ib puag ncig ntawm polycyclic aromatic pydrocarbons (PAHS) hauv av tsis huv
2.1 Tom Qab
Pah, carcinogenic byproducts ntawm tsis tiav kev sib txuas, paug cov av kom tsis muaj chaw nyob ze. Lub chaw ua haujlwm tswj hwm nrhiav kom ua kom muaj nuj nqis 16s Pahs (piv txwv li, benzo [a] pyrenee) hauv ib qho qub steel site.
2.2 Kev Ntseeg
Kev Npaj Qauv:
Soxhlet muab rho tawm 10 g ntawm cov av nrog dichloromomethane rau 24 teev.
Mloog cov extract rau 1 ml ntawm kev siv teb av evaporation.
Sab chromatography:
Theem nyob ruaj ruaj: Silica gel (10 g, 60-200 mesh).
Mobile theem: Hexane-Dichloromethane Gradient (1 0}} rau 0:10).
Kev tsom xam:
Txhaj tshuaj 1 μl ntawm txhua feem kev tawm mus rau GC-MS (Electron ionization hom).
2.3 TSHAJ
Rov qab rau 16 PAHS tau nyob ntawm 82% (Naphthalene) rau 95% (Benzo [G, H, Kuv] Spylene).
Tag nrho PAH lub siab: 1,250 ug \/ kg (saum toj uas tsis muaj kev txwv ntawm 500 ug \/ kg).
Benzo [a] Pyrenee remental: 150 Ug \/ kg (Carcinogenic Florhol: 10 ug \/ kg).
2.4 Tseem Ceeb
Lub xaib tau faib ua kev zam txim rau kev noj qab haus huv rau tib neeg txoj kev noj qab haus huv.
► Kev Kawm Kev Kawm Ntawv 3: Synthesis thiab kev ua kom huv ntawm cov organic-organic qauv (mofs) rau roj cia
3.1 Tom Qab
ZiF -8, ib zinc-ipidanolate mof, qhia cog lus tias cog lus rau kev sib koom tes. Txawm li cas los xij, synthesis los ntawm kev ua haujlwm (piv txwv li, tsis paub tseeb ntawm ligands, zinc oxide) yuav tsum raug tshem tawm kom ua kom pom tau cov porosity.
3.2 Kev Ntseeg
Synthesis: Solvothermal cov tshuaj tiv thaiv ntawm Zn (No₃) ₂ 6 2- Metylimidazole hauv methanil.
Sab chromatography:
Theem nyob ruaj khov: Reptex lh -20 (qhov loj me (qhov loj-cais tawm resin).
Mobile theem: methanol.
Tus txheej txheem:
Yaj 500 mg ntawm crude zif -8} hauv 10 ml ntawm methanol.
Thauj cov qauv rau hauv 300 × 10 hli kem.
Eluted ntawm 0. 5 ml \/ min, khaws 2 ml feem.
Saib xyuas cov feem ntawm UV-VIS (254 nm) thiab hmoov x-roor diffraction (PXRD).
3.3 TSHAJ
Feem dawb 10-15 muaj ntshiab zif -8 (paub tseeb los ntawm pxrd).
Kev twv thawj cheeb tsam: 1,620 m² \/ g (vs. 1,200 m² \/ g rau unpurified zif {{4 4}}).
CO₂ XTTAKE ntawm 298 K thiab 1 MMOL \/ G (Vs. 2.1 MMOL \/ G rau unpurified zif -8).
3.4 Tseem Ceeb
Lub lim dej Zif -8 outperformed kev lag luam adsorbus, nce qib nws txoj kev sib tw rau kev lag luam sib zog.
Mine Kev Kawm 4: Kev tsom xam ntawm hluavtaws cannabinoids hauv kev kuaj cov tshuaj uas pom tau
4.1 Tom Qab
Synthetic cannabinoids (piv txwv li, jwh -018) yog tsim txom raws li "txuj lom". Ib lub chaw ntsuas hluav taws xob tshawb nrhiav kom paub thiab ntsuas cov tebchaw no hauv cov khoom siv cog ntoo.
4.2 Kev Ntseeg
Extraction:
Ultrasonicated 1 g ntawm cov khoom cog ntoo nrog 10 ml ntawm methanol rau 30 feeb.
Lim thiab mloog cov extract rau 1 ml.
Sab chromatography:
Theem nyob theem: C18 thim rov qab-theem silica (500 mg).
Txawb theem: methanol-dej (80:20).
Kev tsom xam:
Txhaj 5 μl ntawm lub lim dej feem rau hauv LC-MS \/ MS (MRM hom).
4.3 Cov Ntsiab Lus
Kuaj pom Jwh {{{{{0}}} ntawm 12,5 mg \/ g (txwv ntawm kev kuaj pom: 0.1 mg \/ g).
Txheeb xyuas ob metabolites (jwh -018 n - ({} hydroxypic acid) ntawm MS \/ MS Frandmentation.
Kev paub tseeb tau ua los ntawm kev sib piv nrog cov qauv tseeb.
4.4 Tseem Ceeb
Cov kev tshawb pom kev ua txhaum kev raug foob thiab qhia cov lus qhia kev noj qab haus huv rau pej xeem ntawm cov hluavtaws cannabissoid txaus ntshai.
Kev nce qib thiab yav tom ntej cov lus qhia
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Multidimensional kem chromatography Cov txheej txheem no cov khub niam txiv muaj ntau yam nrog kev xaiv sib txawv los txhim kho cov kev daws teeb meem. Piv txwv, cais chairal tebchaw siv kev sib txuas ntawm cov theem li silica thiab chairal nyob theem. Automation thiab High-Cuaved SystemsKev nce qib hauv cov neeg hlau thiab microfluidics tau qhib: Automated Flasraphy Tshuab (piv txwv li, bioteage yog raws li kev ntsuas, combiflash). MOTICCALE COLLICE rau qib siab-los ntawm kev kuaj xyuas hauv kev tshuaj pom tshuaj. Cov Khoom Noj Ua Si NtsuabTiam sis niaj hnub ua ke suav nrog: Recycling cov kuab tshuaj ntawm distillation lossis membrane sib cais. Siv biodegradable chaw nyob theem (piv txwv li, cellulose-based adsorbents). Tsis tas li cov pov tseg los ntawm cov kuab kub kho tau zoo. Kev sib koom ua ke nrog cov txheej txheem hyphenatedKem chromatography feem ntau yog txuas nrog: Pawg Spectrometry (LC-MS) rau cov cim kev sib txuas tiag. NMR spectroscopy rau cov txheej txheem elucidation ntawm cais cov zauv feem. Cov cuab yeej online kuaj (piv txwv li, UV, cov ntsiab lus tshiab) rau kev saib xyuas tas mus li. Nanoscale thiab microfluidic kemCov thev naus laus zis muaj xws li: Nanoscale kab (sab hauv inch <100 μm) rau cov kev sib cais ultraigh-desolution sib cais. Microfluidic chips nrog kev ua haujlwm chromatography txhua rau kev saib xyuas cov kev kuaj mob. |
Cim npe nrov: Chemistry sab chromatography, Tuam Tshoj Chemistry kem chromatography manufacturers, lwm tus neeg, Hoobkas
Tom ntej
Kem chromatography khoomXa kev nug
