SepaBean™ umshini

Ukulinganisa kwekholomu kungavikela ikholomu ekubeni yonakaliswe umphumela we-exothermic lapho i-solvent igeleza ngokushesha kukholomu. Ngenkathi i-silica eyomile ifakwe ngaphambili kukholomu ithintwa yi-solvent okokuqala ngqa ngesikhathi sokuhlukaniswa, ukushisa okuningi kungase kukhishwe ikakhulukazi lapho i-solvent iguquguquka ngezinga lokugeleza okuphezulu. Lokhu kushisa kungase kubangele umzimba wekholomu ukuthi uwohloke futhi ngaleyo ndlela ukuvuza kwe-solvent kusuka kukholamu. Kwezinye izimo, lokhu kushisa kungase futhi kulimaze isampuli ezwela ukushisa.

Kungenzeka ukuthi kubangelwa ukuntuleka kwamafutha okugcoba ku-shaft ejikelezayo yepompo.

Umthamo ophelele wamashubhu wesistimu, izixhumi negumbi lokuxuba cishe u-25 mL.

Iseli eligelezayo lemojula yomtshina lingcoliswe isampula elinokumunca okuqinile kwe-UV. Noma kungase kube ngenxa yokumuncwa kwe-solvent ye-UV okuyinto evamile. Sicela wenze lokhu okulandelayo:

1. Khipha ikholomu ye-flash bese usula ishubhu yesistimu nge-solvent ye-polar enamandla bese ulandelwa yi-solvent ye-polar ebuthakathaka.

2. Inkinga yokumuncwa kwe-UV ye-solvent: isb ngenkathi i-n-hexane ne-dichloromethane (DCM) kusetshenziswa njengesinyibilikisi esincibilikayo, njengoba ingxenye ye-DCM ikhula, isisekelo se-chromatogram singase siqhubeke sibe ngaphansi kukaziro ku-Y-axis kusukela ekumuncwani kwe-DCM. ku-254 nm iphansi kunaleyo ye-n-hexane. Uma kwenzeka lesi simo, singasisingatha ngokuchofoza inkinobho ethi "Zero" ekhasini elisebenzayo lokuhlukanisa kuhlelo lokusebenza lwe-SepaBean.

3.Iseli lokugeleza lemojula yomtshina lingcoliswe kakhulu futhi lidinga ukuhlanzwa nge-ultrasonically.

Kungase kube ngenxa yokuthi izixhumi ezisekhanda lomphathi wekholomu kanye nengxenye yesisekelo zivuvukale nge-solvent ukuze izixhumi zibambeke.

Umsebenzisi angakwazi ukuphakamisa ngesandla isibambi sekholomu ngokusebenzisa amandla amancane. Uma inhloko yesibambi sekholomu iphakanyiselwa phezulu ifinyelela ubude obuthile, inhloko yesibambi sekholomu kufanele ikwazi ukunyakaza ngokuthinta izinkinobho ezikuyo. Uma isibambi sekholomu singakwazi ukuphakanyiswa mathupha, umsebenzisi kufanele axhumane nosekelo lwasendaweni lobuchwepheshe.

Enye indlela yesimo esiphuthumayo: Umsebenzisi angafaka ikholomu phezulu kwekhanda lesiphathi sekholomu esikhundleni salokho. Isampula yoketshezi ingajovwa ngqo kukholomu. Ikholomu yokulayisha isampula eqinile ingafakwa ngaphezulu kwekholomu yokuhlukanisa.

1. Amandla aphansi omthombo wokukhanya;

2. Ichibi lokujikeleza lingcolile; I-Intuitively, akukho ukuphakama kwe-spectral noma ukuphakama kwe-spectral kuncane ekuhlukaniseni , I-spectra yamandla ibonisa inani elingaphansi kwama-25%.

Sicela ugeze ishubhu nge-solvent efanele ku-10ml/min imizuzu engu-30 bese ubheka i-spectrum yamandla.Uma lungekho ushintsho ku-spectrum, kubonakala amandla aphansi omthombo wokukhanya, sicela ufake isibani se-deuterium; Uma i-spectrum ishintshile, ichibi lokujikeleza liyangcoliswa, sicela uqhubeke nokuhlanza ngesincibilikisi esifanele.

Sicela uhlole ishubhu nesixhumi njalo.

Ubude begagasi bokutholwa busethwe kubude be-wav obungaphansi kuka-245 nm njengoba i-ethyl acetate inokumuncwa okuqinile ebangeni lokutholwa elingaphansi kuka-245nm. Isisekelo sokukhukhuleka sizoba kakhulu uma i-ethyl acetate isetshenziswa njenge-solvent encibilikayo futhi sikhetha u-220 nm njengobude begagasi bokutholwa.

Sicela uguqule ubude bezansi bokutholwa. Kunconywa ukuthi ukhethe i-254nm njengobude begagasi bokutholwa. Uma u-220 nm kuwukuphela kwe-wavelength efanelekile ukutholwa kwesampula, umsebenzisi kufanele aqoqe i-eluent ngokwahlulela ngokucophelela futhi i-solvent eyeqile ingase iqoqwe kulesi simo.

Hlanza ikhanda lesihlungi se-solvent ngokuphelele ukuze ususe noma yikuphi ukungcola. Sebenzisa i-ethanol noma i-isopropanol ukuze usule isistimu ngokuphelele ukuze ugweme izinkinga ze-solvent ezingahlangani.

Ukuze uhlanze ikhanda lesihlungi se-solvent, qaqa isihlungi kusuka ekhanda lesihlungi bese usihlanza ngebhulashi elincane. Bese ugeza isihlungi nge-ethanol bese usomisa ngokufutheka. Phinda uhlanganise inhloko yokuhlunga ukuze uyisebenzise esikhathini esizayo.

Kuphakathi kokuthi ushintshe usuke ekwehlukaneni kwesigaba esivamile uye ekwehlukanisweni kwesigaba esihlehlisiwe noma okuphambene nalokho, i-ethanol noma i-isopropanol kufanele isetshenziswe njengesixazululi soshintsho ukuze kukhishwe ngokuphelele noma yiziphi izincibilikisi ezingahlangani kushubhu.

Kunconywa ukusetha izinga lokugeleza ku-40 mL/min ukuze usule imigqa ye-solvent kanye nawo wonke amashubhu angaphakathi.

Sicela ubeke kabusha phansi isibambi sekholomu ngemva kokukhulula isikulufu.

1. Izinga lokugeleza kwesistimu liphezulu kakhulu kukholomu yefuleshi yamanje.

2. Isampula inokuncibilika okungekuhle futhi imvula isuka esigabeni esihambayo, ngaleyo ndlela kubangele ukuvaleka kwamashubhu.

3. Esinye isizathu sibangela ukuvaleka kwamashubhu.