I-Etere yeSelulosi engeyiyo i-ionic ngeChromatography yeGesi

Umxholo wabaxumi kwi-ether ye-cellulose engeyiyo i-ionic inqunywe yi-chromatography yegesi, kwaye iziphumo zafaniswa ne-titration yeekhemikhali ngokwexesha lokutya, ukusebenza, ukuchaneka, ukuphindaphinda, iindleko, njl., kunye nokushisa kwekholomu kwaxoxwa. Impembelelo yeemeko zechromatographic ezifana nobude bekholamu kwisiphumo sokwahlula. Iziphumo zibonisa ukuba i-chromatography yegesi yindlela yokuhlalutya efanele ukuthandwa.
Amagama angundoqo: i-non-ionic cellulose ether; ichromatography yegesi; umxholo obambeleyo

I-nonionic cellulose ethers ibandakanya i-methylcellulose (MC), i-hydroxypropylmethylcellulose (HPMC), i-hydroxyethylcellulose (HEC), njl. Ezi zixhobo zisetyenziswa kakhulu kumayeza, ukutya, i-petroleum, njl. izixhobo ze-ionic cellulose ether, kuyimfuneko ukumisela umxholo wezinto ezibambeleyo ngokuchanekileyo kwaye ngokukhawuleza. Okwangoku, uninzi lwabavelisi basekhaya bamkela indlela yesiqhelo yokuhlaziya imichiza yokuhlalutya, esebenza nzima kwaye kunzima ukuqinisekisa ukuchaneka kunye nokuphindaphinda. Ngenxa yesi sizathu, eli phepha lifunda indlela yokumisela umxholo we-non-ionic cellulose ether substituents nge-chromatography yegesi, ihlalutya izinto ezichaphazela iziphumo zovavanyo, kwaye ifumana iziphumo ezilungileyo.

1. Linge
1.1 Isixhobo
I-GC-7800 yegesi yechromatograph, eveliswe yiBeijing Purui Analytical Instrument Co., Ltd.
1.2 IiReagents
I-Hydroxypropyl methylcellulose (HPMC), i-hydroxyethylcellulose (HEC), eyenziwe ekhaya; i-methyl iodide, i-ethyl iodide, i-isopropane iodide, i-hydroiodic acid (57%), i-toluene, i-adipic acid, i-o-di Toluene yayikwibakala lohlalutyo.
1.3 Ukumiselwa kwechromatography yegesi
1.3.1 Iimeko zekhromatografi yegesi
Ikholomu yensimbi engenasici ((SE-30, 3% Chmmosorb, WAW DMCS); ubushushu begumbi le-vaporization 200 ° C; i-detector: TCD, 200 ° C; ubushushu bekholamu 100 ° C; igesi ethwala: H2, 40 mL / min.
1.3.2 Ukulungiswa kwesisombululo esisemgangathweni
(1) Ukulungiswa kwesisombululo somgangatho wangaphakathi: Thatha malunga ne-6.25g ye-toluene kwaye ubeke kwi-flask ye-volumetric ye-250mL, udibanise uphawu nge-o-xylene, xubha kakuhle kwaye ubeke eceleni.
(2) Ukulungiswa kwesisombululo esisemgangathweni: iisampuli ezahlukeneyo zinezisombululo ezisemgangathweni ezihambelanayo, kunye neesampuli ze-HPMC zithathwa njengomzekelo apha. Kwi-vial efanelekileyo, yongeza inani elithile le-adipic acid, i-2 mL ye-hydroiodic acid kunye nesisombululo esisemgangathweni sangaphakathi, kwaye ulinganise ngokuchanekileyo i-vial. Yongeza inani elifanelekileyo le-iodoisopropane, ulinganise, kwaye ubale inani le-iodoisopropane eyongeziweyo. Yongeza i-methyl iodide kwakhona, ulinganise ngokulinganayo, ubale inani elongeza i-methyl iodide. Vibrawuza ngokupheleleyo, yiyeke ime istratification, kwaye uyigcine kude nokukhanya ukuze isetyenziswe kamva.
1.3.3 Ukulungiswa kwesisombululo sesampuli
Ukulinganisa ngokuchanekileyo i-0.065 g yesampuli eyomileyo ye-HPMC kwi-reactor ye-5 mL engqingqwa, yongeza ubunzima obulinganayo be-adipic acid, i-2 mL yesisombululo esiqhelekileyo sangaphakathi kunye ne-hydroiodic acid, ngokukhawuleza uvale ibhotile yokusabela, kwaye uyilinganise ngokuchanekileyo. Shake, kwaye ushushu kwi-150 ° C imizuzu engama-60, ukugubha ngokufanelekileyo ngeli xesha. Phola kwaye ulinganise. Ukuba ukulahleka kwesisindo ngaphambi nangemva kokuphendula kukhulu kune-10 mg, isisombululo sesampuli asivumelekile kwaye isisombululo kufuneka siphinde silungiswe. Emva kokuba isisombululo sesampuli sivunyelwe ukuma kwi-stratification, udwebe ngokucophelela i-2 μL yesisombululo sesigaba esiphezulu se-organic, uyifake kwi-chromatograph yegesi, kwaye urekhode i-spectrum. Ezinye iisampuli ze-cellulose ze-ether ezingezo-ionic zaphathwa ngokufanayo kwi-HPMC.
1.3.4 Umgaqo wokulinganisa
Ukuthatha i-HPMC njengomzekelo, yi-cellulose alkyl hydroxyalkyl ether exutywe ne-hydroiodic acid ukuphula zonke iibhondi ze-ether ze-methoxyl kunye ne-hydroxypropoxyl kunye nokuvelisa iodoalkane ehambelanayo.
Ngaphantsi kobushushu obuphezulu kunye neemeko zomoya, kunye ne-adipic acid njenge-catalyst, i-HPMC isabela nge-hydroiodic acid, kunye ne-methoxyl kunye ne-hydroxypropoxyl ziguqulwa zibe yi-methyl iodide kunye ne-isopropane iodide. Ukusebenzisa i-o-xylene njenge-absorbent kunye ne-solvent, indima ye-catalyst kunye ne-absorbent kukukhuthaza ukusabela okupheleleyo kwe-hydrolysis. I-Toluene ikhethwe njengesisombululo esisemgangathweni sangaphakathi, kwaye i-methyl iodide kunye ne-isopropane iodide isetyenziswa njengesisombululo esiqhelekileyo. Ngokweendawo eziphakamileyo zomgangatho wangaphakathi kunye nesisombululo esiqhelekileyo, umxholo we-methoxyl kunye ne-hydroxypropoxyl kwisampuli ingabalwa.

2. Iziphumo kunye nengxoxo
Uluhlu lwechromatographic olusetyenziswe kolu vavanyo alukho polar. Ngokwendawo yokubilisa yecandelo ngalinye, i-peak order yi-methyl iodide, i-isopropane iodide, i-toluene kunye ne-o-xylene.
2.1 Ukuthelekisa phakathi kwe-chromatography yegesi kunye ne-chemical titration
Ukumiselwa komxholo we-methoxyl kunye ne-hydroxypropoxyl ye-HPMC nge-titration yekhemikhali ikhulile, kwaye ngoku kukho iindlela ezimbini eziqhelekileyo ezisetyenziswayo: indlela ye-Pharmacopoeia kunye nendlela ephuculweyo. Nangona kunjalo, zombini ezi ndlela zimbini zeekhemikhali zifuna ukulungiswa kwesixa esikhulu sezisombululo, umsebenzi unzima, udla ixesha, kwaye uchaphazeleka kakhulu yimiba yangaphandle. Ngokwentelekiso, ichromatography yegesi ilula kakhulu, kulula ukuyifunda nokuqonda.
Iziphumo zomxholo we-methoxyl (w1) kunye nomxholo we-hydroxypropoxyl (w2) kwi-HPMC zinqunywe yi-chromatography yegesi kunye ne-titration yekhemikhali ngokulandelelanayo. Kuyabonakala ukuba iziphumo zezi ndlela zimbini zisondele kakhulu, zibonisa ukuba zombini iindlela zinokuqinisekisa ukuchaneka kweziphumo.
Ukuthelekisa i-chemical titration kunye ne-chromatography yegesi ngokwemigaqo yokusetyenziswa kwexesha, ukulula ukusebenza, ukuphindaphinda kunye neendleko, iziphumo zibonisa ukuba inzuzo enkulu ye-chromatography yesigaba ilula, ukukhawuleza kunye nokusebenza kakuhle. Akukho mfuneko yokulungiselela isixa esikhulu se-reagents kunye nezisombululo, kwaye kuthatha imizuzu engaphezu kweshumi kuphela ukulinganisa isampuli, kwaye ixesha langempela eligciniweyo liya kuba likhulu kunezibalo. Kwindlela yekhemikhali ye-titration, impazamo yomntu ekugwebeni indawo yokuphela kwe-titration inkulu, ngelixa iziphumo zovavanyo lwe-chromatography yegesi azichatshazelwa kangako zizinto zabantu. Ngapha koko, i-chromatography yegesi yindlela yokwahlulahlula imveliso yokusabela kwaye ilinganise. Ukuba inokusebenzisana nezinye izixhobo zokulinganisa, ezifana neGC/MS, GC/FTIR, njl. njl., ingasetyenziselwa ukuchonga iisampulu ezintsonkothileyo ezingaziwayo (iifibers eziguquliweyo) Iimveliso ze-ether eziziiPlain) zinenzuzo kakhulu, ezingahambelaniyo nekhemikhali titration. . Ukongeza, ukuveliswa kwakhona kweziphumo ze-chromatography yegesi kungcono kunezo zekhemikhali titration.
Ukungalungi kwe-chromatography yegesi kukuba ixabiso liphezulu. Iindleko ezivela ekusekweni kwesikhululo se-chromatography yegesi ekugcinweni kwesixhobo kunye nokukhethwa kwekholamu yechromatographic iphezulu kunendlela ye-chemical titration. Ulungelelwaniso lwezixhobo ezahlukeneyo kunye neemeko zovavanyo ziya kuchaphazela iziphumo, ezifana nohlobo lwe-Detector, ikholamu yechromatographic kunye nokukhethwa kwesigaba esimileyo, njl.
2.2 Impembelelo yeemeko ze-chromatography yegesi kwiziphumo zokumisela
Kwimifuniselo yegesi yechromatography, undoqo kukumisela iimeko ezifanelekileyo zechromatographic ukufumana iziphumo ezichanekileyo. Kulo vavanyo, i-hydroxyethylcellulose (HEC) kunye ne-hydroxypropylmethylcellulose (HPMC) isetyenziswe njengezinto ezibonakalayo, kwaye impembelelo yezinto ezimbini, ukushisa kwekholomu kunye nobude bekholomu, yafundwa.
Xa iqondo lokuhlukana R ≥ 1.5, kuthiwa ukuhlukana okupheleleyo. Ngokutsho kwemimiselo ye "Chinese Pharmacopoeia", i-R kufuneka ibe mkhulu kune-1.5. Idityaniswe nobushushu bekholomu kumaqondo obushushu amathathu, isisombululo secandelo ngalinye sikhulu kune-1.5, esihlangabezana neemfuno ezisisiseko zokuhlukana, eziyi-R90 ° C>R100 ° C>R110 ° C. Ukuqwalasela i-tailing factor, i-tailing factor r> i-1 yincopho yomsila, i-r<1 yincopho yangaphambili, kwaye i-r isondele ku-1, ngcono ukusebenza kwekholamu yechromatographic. Kwi-toluene kunye ne-ethyl iodide, i-R90°C>R100°C>R110°C; I-o-xylene sisinyibilikisi esineqondo eliphezulu lokubila, i-R90°C
Impembelelo yobude bekholomu kwiziphumo zovavanyo ibonisa ukuba phantsi kweemeko ezifanayo, ubude kuphela bekholamu yechromatographic butshintshiwe. Xa kuthelekiswa nekholomu epakishweyo ye-3m kunye ne-2m, iziphumo zokuhlalutya kunye nesisombululo sekholamu ye-3m zingcono, kwaye ikholomu ende, ingcono ukusebenza kwekholomu. Ixabiso eliphezulu, isiphumo sinokuthenjwa.

3. Isiphelo
I-Hydroiodic acid isetyenziselwa ukutshabalalisa ibhondi ye-ether ye-ether ye-cellulose engekho i-ionic ukuvelisa i-iodide ye-molecule encinci, eyahlulwe yi-chromatography yegesi kwaye ibalwa ngendlela esemgangathweni yangaphakathi ukufumana umxholo we-substituent. Ukongeza kwi-hydroxypropyl methylcellulose, i-cellulose ethers efanelekileyo kule ndlela ibandakanya i-hydroxyethyl cellulose, i-hydroxyethyl methyl cellulose, kunye ne-methyl cellulose, kwaye indlela yonyango yesampuli iyafana.
Xa kuthelekiswa nendlela yesiqhelo yekhemikhali ye-titration, uhlalutyo lwe-chromatography yegesi ye-substituent content ye-non-ionic cellulose ether ineenzuzo ezininzi. Umgaqo ulula kwaye kulula ukuwuqonda, ukusebenza kukulungele, kwaye akukho mfuneko yokulungiselela inani elikhulu lamayeza kunye ne-reagents, egcina kakhulu ixesha lokuhlalutya. Iziphumo ezifunyenwe ngale ndlela zihambelana nezo zifunyenwe nge-chemical titration.
Xa uhlalutya umxholo obambeleyo ngechromatography yegesi, kubaluleke kakhulu ukukhetha iimeko ezifanelekileyo kunye nezifanelekileyo zechromatographic. Ngokuqhelekileyo, ukunciphisa ukushisa kwekholomu okanye ukwandisa ubude bekholomu kunokuphucula ngokufanelekileyo isisombululo, kodwa kufuneka kuthathelwe ingqalelo ukuthintela amacandelo ekunciphiseni kwikholomu ngenxa yokushisa kwekholomu ephantsi kakhulu.
Okwangoku, uninzi lwabavelisi basekhaya basasebenzisa i-titration yeekhemikhali ukumisela umxholo wezinto ezibambeleyo. Nangona kunjalo, ngokuqwalasela izibonelelo kunye nokungalunganga kwimiba eyahlukeneyo, i-chromatography yegesi yindlela elula nekhawulezayo yokuvavanya ekufanele ukuba iphakanyiswe ngokwembono yeendlela zophuhliso.