Ukulungiswa kwesampula kanye ne-Filtration: Ukuqinisekisa ikhwalithi ku-Chromatography

Iziqukathi ezihlanzekile zesampula ezihleliwe, susa ama-concletes, ahlaziye ama-engcus, futhi, uma kudingeka, asule - aqede ngaphezulu kwama-90% omsindo wesisekelo kanye nokucindezela kwengcindezi, izisekelo ezibukhali kanye nezisekelo ezizinzile. Ukwehluleka lapha kuphumela ekuthayisweni okuphezulu, okuvuthayo izisekelo, noma ukuqhekeka kukholamu.

1. Ukuphazanyiswa kanye nokuphazanyiswa kwe-matrix

Inkinga

• I-Baseline Drift futhi ikhuphuke umsindo ocwilisa iziqongo ezincane.

• Iziqongo ezingalindelekile zivela ekungcoleni kwezikhonkwane.

• Ukudalula kabusha okungenampilo phakathi kwemijovo.
  

  

Dala

• Izinsalela ze-GlasLare: Izilimo ezingaphelele ze-acid-wash zilindile; I-Plastware ingalungisa amapulasitiki.

• Ukuhlanza Ama-Agents: Trace organics ku-hlanza solvents hlala ama-addedbed.

• Izinhlazitho zemvelo
  

  

Isixazululo

1. Ukuhlanza okuqinile kokuhlanza: I-acid scak → hlambulula amanzi we-ultrasonic → I-nitrogen yomile ye-glassware; Ukuzinikela okunikezelwe kwamapulasitiki.

2. Ukuhlunga kwangaphambili: I-centrifuge ku-3000rpm ye-10min noma usebenzise isiqalo esingu-5μm ngaphambi kokuhlungwa kokugcina kwe-0.22μm.

3. Imvelo Elawulwayo: Yenza i-prep ku-leaminar-flow hood ukuze unciphise ukungcoliswa kwezindiza.
   
   

2. Hlunga ukuvalwa kusuka ezingubeni ezingahambelani

Inkinga

• Ama-alamu wengcindezi ye-autosampler kanye nokushintshwa kwenaliti njalo.

• Ukunciphisa ukugeleza kwezinga, izindawo ezingahambisani neze.

• Ukuphakama kwe-backprestreaspressure nekholamu.
  

  

Dala

• UMembrane Mismatch: I-Nylon iyavuvukala kuma-organic solvents; I-PVDF ingena emazingeni okushisa aphakeme.

• Ubukhulu obungalungile Izihlungi ze-0.45μm zingahle zivale nge-microcrystals.

Isixazululo

1. Membrane-solvent matrix: Sebenzisa i-hydrophilic pes \ mce for aquous (Ph4-8), Hydrophobic Ptfe \ pvdf yezigaba ezi-organic; Gwema iselula acetate kuma-acid aqinile.

2. Khetha usayizi ofanele we-pore: Sebenzisa u-0.45μm we-HORDC HPLC, 0.22μm we-UHPLC noma ngomsebenzi wokulandela; Isiqalo samasampula aphezulu okuvuselela amasampula angu-5μM.

3. Qapha ΔP: Ukulandela ingcindezi kukhuphuka; Faka esikhundleni sokuhlunga lapho kuncipha i-backpressure> 15%.
   
   

   

3. I-solvent-membrane commage ingalo

Inkinga

• Isampula ehlungiwe ibonakala inamafu noma ithwala izinhlayiya.

• Umsindo omusha wesisekelo noma i-ghost peaks post-filtration.

• Ukululama okuncishisiwe kokuhlaziya.
  

  

Dala

• Ukuvuvukala kwe-solvent: thf ukuvuvukala kwe-PTFE, ukuguqula usayizi we-pore nokugeleza.

• I-membrane leaakeable: I-Nylon ku-Formic acid ikhipha ama-oligomers amunca ku-214NM.

Isixazululo

1. Ukuhlolwa kokuvumelana: Cwilisa isihlungi se-solvent ehlosiwe ngo-24h ngo-25 ° C; hlola ukuvuvukala noma ukuguqulwa kwesisindo.

2. Ukuhlolwa kwe-Pilot LC-MS: Qhathanisa ingqikithi ye-ion chromamograms yesampula ehlungiwe.

3. Sebenzisa izihlungi eziphansi ze-leach: I-ptfe ye-ultrasonic-welded noma i-pes ngaphandle kwezinamathela.
   
   

Uhlelo lwekhwalithi: Ukulungiswa kokuqapha kwezokuvikela

Ukuvika

Yenza ama-SOPs ahlele ukuhlanza, ukufona, kanye nokukhetha kukaMefbrane ukuvikela amaphutha.

Ukuqapha

Qopha ukugeleza kwezinga, i-backcersure, kanye nezisekelo zesampula ezingenalutho ukuze zibone ukudonsa.

Ukulungisa

Gcina ukuhlaziywa kwesihlahla ngephutha ukuze kuhlonziwe kwe-ROOT-ROOT-ROOT-ROOR -ORP

"Ukucacisa kokuhlaziya kuqala ngokunciphisa izinhlayiyana ezincane kakhulu."