Non-ionic Cellulose Ether by Gas Chromatography

Ibiri mu nsimburangingo muri selile itari ionic selile byagenwe na chromatografi ya gaze, kandi ibisubizo byagereranijwe na titre ya chimique mubijyanye no gutwara igihe, imikorere, ubunyangamugayo, gusubiramo, ibiciro, nibindi, maze ubushyuhe bwinkingi buraganirwaho. Ingaruka yimiterere ya chromatografi nkuburebure bwinkingi ku ngaruka zo gutandukana. Ibisubizo byerekana ko gazi chromatografiya ari uburyo bwo gusesengura bukwiye kumenyekana.
Amagambo shingiro: non-ionic selulose ether; gazi ya chromatografiya; Ibirimo

Ethers ya nonionic selile harimo methylcellulose (MC), hydroxypropylmethylcellulose (HPMC), hydroxyethylcellulose (HEC), nibindi. Ibyo bikoresho bikoreshwa cyane mubuvuzi, ibiryo, peteroli, nibindi. ionic selulose ether ibikoresho, birakenewe kumenya ibirimo insimburangingo neza kandi vuba. Kugeza ubu, inganda nyinshi zo murugo zikoresha uburyo bwa gakondo bwo gutondekanya imiti kugirango isesengurwe, ikaba isaba akazi cyane kandi bigoye kwemeza ukuri no gusubiramo. Kubera iyo mpamvu, iyi mpapuro yiga uburyo bwo kumenya ibikubiye mu bintu bitari ionic selulose ether byasimbuwe na gazi chromatografiya, isesengura ibintu bigira ingaruka ku bisubizo, kandi ikabona ibisubizo byiza.

1. Ubushakashatsi
1.1 Igikoresho
GC-7800 gazi ya chromatograf, yakozwe na Beijing Purui Analytical Instrument Co., Ltd.
1.2 Reagents
Hydroxypropyl methylcellulose (HPMC), hydroxyethylcellulose (HEC), yakozwe mu rugo; methyl iyode, Ethyl iyode, isopropane iyode, aside hydroiodic (57%), toluene, aside adipic, o-di Toluene yari murwego rwo gusesengura.
1.3 Kugena gazi ya chromatografiya
1.3.1 Imiterere ya gazi ya chromatografiya
Inkingi idafite ibyuma ((SE-30, 3% Chmmosorb, WAW DMCS); ubushyuhe bwa chambre yubushyuhe bwa 200 ° C; detector: TCD, 200 ° C; ubushyuhe bwinkingi 100 ° C; gaze yabatwara: H2, 40 mL / min.
1.3.2 Gutegura igisubizo gisanzwe
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(2) Gutegura igisubizo gisanzwe: ingero zitandukanye zifite ibisubizo bihuye, kandi ingero za HPMC zifatwa nkurugero hano. Muri vial ikwiye, ongeramo urugero runaka rwa acide adipic, mL 2 ya acide hydroiodic nigisubizo cyimbere, hanyuma upime neza vial. Ongeramo ingano ikwiye ya iyodeisopropane, uyipime, kandi ubare ingano ya iodoisopropane yongeyeho. Ongeraho methyl iyode, upime kimwe, ubare umubare wongeyeho methyl iyode. Kunyeganyega byuzuye, reka bihagarare kuri stratifike, kandi ubigumane kure yumucyo kugirango bikoreshwe nyuma.
1.3.3 Gutegura igisubizo cyicyitegererezo
Gupima neza 0,065 g yicyitegererezo cya HPMC cyumye mumashanyarazi ya mL 5 yuzuye urukuta, ongeramo uburemere buke bwa acide adipic, mL 2 yumuti usanzwe wimbere hamwe na acide hydroiodic, funga vuba icupa rya reaction, kandi ubipime neza. Kunyeganyega, no gushyushya kuri 150 ° C muminota 60, kunyeganyega neza mugihe. Nkonje kandi upime. Niba gutakaza ibiro mbere na nyuma yo kubyitwara birenze mg 10, igisubizo cyicyitegererezo nticyemewe kandi igisubizo kigomba kongera gutegurwa. Igisubizo cyicyitegererezo kimaze kwemererwa guhagarara kumurongo, shushanya witonze 2 μL yumuti wo hejuru wicyiciro cyo hejuru, uyinjize muri chromatografi ya gaze, hanyuma wandike urutonde. Izindi ngero zitari ionic selulose ether zafashwe kimwe na HPMC.
1.3.4 Ihame ryo gupima
Dufashe HPMC nk'urugero, ni selile ya alkyl hydroxyalkyl ivanze na ether, ifatanyirizwa hamwe na aside hydroiodic kugirango isenye imigozi yose ya metoxyl na hydroxypropoxyl ether ikabyara iodoalkane.
Mugihe cy'ubushyuhe bwinshi hamwe nubushyuhe bwo mu kirere, hamwe na aside adipic nka catalizator, HPMC ikora na aside hydroiodic, na vitamine na hydroxypropoxyl ihinduka methyl iyode na isopropane iyode. Gukoresha o-xylene nkibikurura kandi bigashonga, uruhare rwa catalizator nogusohora ni uguteza imbere hydrolysis yuzuye. Toluene yatoranijwe nkigisubizo cyimbere cyimbere, na methyl iyode na isopropane iyode ikoreshwa nkigisubizo gisanzwe. Ukurikije ahantu hahanamye h'imbere h'imbere hamwe nigisubizo gisanzwe, ibirimo mikorobe na hydroxypropoxyl murugero birashobora kubarwa.

2. Ibisubizo n'ibiganiro
Inkingi ya chromatografique ikoreshwa murubu bushakashatsi ntabwo ari polar. Ukurikije ingingo itetse ya buri kintu, gahunda yo hejuru ni methyl iyode, isopropane iyode, toluene na o-xylene.
2.1 Kugereranya hagati ya gaz chromatografiya na titre ya chimique
Igenamigambi ryimikorere ya hydroxypropoxyl ya HPMC ukoresheje titre ya chimique irakuze, kandi kuri ubu hariho uburyo bubiri bukunze gukoreshwa: uburyo bwa Pharmacopoeia nuburyo bunoze. Nyamara, ubwo buryo bwombi muburyo bwimiti busaba gutegura ibisubizo byinshi, ibikorwa biragoye, bitwara igihe, kandi bigira ingaruka cyane kubintu byo hanze. Ugereranije, gazi chromatografiya iroroshye cyane, byoroshye kwiga no kubyumva.
Ibisubizo by'ibikoresho bya metoxyl (w1) hamwe na hydroxypropoxyl (w2) muri HPMC byagenwe na gazi ya chromatografiya hamwe na titre ya chimique. Birashobora kugaragara ko ibisubizo byuburyo bubiri byegeranye cyane, byerekana ko ubwo buryo bwombi bushobora kwemeza neza ibisubizo.
Ugereranije titre ya chimique na gazi chromatografi muburyo bwo gukoresha igihe, koroshya imikorere, gusubiramo nibiciro, ibisubizo byerekana ko inyungu nini ya chromatografi yicyiciro ari ubworoherane, kwihuta no gukora neza. Nta mpamvu yo gutegura umubare munini wa reagent nigisubizo, kandi bisaba iminota irenga icumi yo gupima icyitegererezo, kandi igihe nyacyo cyakijijwe kizaba kinini kuruta imibare. Muburyo bwa titre chimique, ikosa ryumuntu mugucira impera yanyuma ni nini, mugihe ibisubizo bya gazi ya chromatografiya bitagerwaho cyane nibintu byabantu. Byongeye kandi, gazi chromatografiya ni tekinike yo gutandukanya itandukanya ibicuruzwa byerekana kandi ikabigereranya. Niba ishobora gufatanya nibindi bikoresho byo gupima, nka GC / MS, GC / FTIR, nibindi, irashobora gukoreshwa kugirango hamenyekane ingero zimwe na zimwe zitazwi (fibre zahinduwe) Ibicuruzwa bya ether byo mu kibaya) nibyiza cyane, bitagereranywa na titre ya chimique . Mubyongeyeho, kubyara gaze chromatografiya ibisubizo nibyiza kuruta ibya titre ya chimique.
Ingaruka za gazi chromatografiya nuko igiciro ari kinini. Igiciro kuva hashyirwaho sitasiyo ya gazi ya chromatografi kugeza kubungabunga ibikoresho no gutoranya inkingi ya chromatografiya irenze iy'uburyo bwa titre chimique. Ibikoresho bitandukanye bigereranywa nibizamini bizanagira ingaruka kubisubizo, nk'ubwoko bwa Detector, inkingi ya chromatografi no guhitamo icyiciro gihagaze, nibindi.
2.2 Ingaruka yimiterere ya gaz chromatografiya kubisubizo byagenwe
Kubushakashatsi bwa gazi ya chromatografiya, urufunguzo ni ukumenya imiterere ya chromatografi kugirango ubone ibisubizo nyabyo. Muri ubu bushakashatsi, hydroxyethylcellulose (HEC) na hydroxypropylmethylcellulose (HPMC) byakoreshejwe nkibikoresho fatizo, kandi ubushakashatsi bwakozwe ku ngaruka zibiri, ubushyuhe bwinkingi nuburebure bwinkingi.
Iyo urwego rwo gutandukana R ≥ 1.5, byitwa gutandukana byuzuye. Ukurikije ibivugwa muri "Pharmacopoeia yo mu Bushinwa", R igomba kuba irenze 1.5. Ufatanije nubushyuhe bwinkingi kubushyuhe butatu, imikemurire ya buri kintu irenze 1.5, yujuje ibyangombwa byingenzi byo gutandukana, aribyo R90 ° C> R100 ° C> R110 ° C. Urebye ibintu birebire, umurizo r> 1 ni impinga yumurizo, r <1 nimpinga yimbere, naho hafi ya r ni kuri 1, nibyiza imikorere yinkingi ya chromatografiya. Kuri iyode ya toluene na Ethyl, R90 ° C> R100 ° C> R110 ° C; o-xylene ni umusemburo ufite ingingo ndende cyane, R90 ° C.
Ingaruka yuburebure bwinkingi kubisubizo byubushakashatsi yerekana ko mubihe bimwe, gusa uburebure bwinkingi ya chromatografique burahinduka. Ugereranije ninkingi yuzuye ya 3m na 2m, ibisubizo byisesengura nibisubizo bya 3m inkingi nibyiza, kandi birebire inkingi, niko inkingi ikora neza. Kurenza agaciro, ibisubizo byizewe cyane.

3. Umwanzuro
Acide Hydroiodic ikoreshwa mugusenya ether yumubumbe wa selile utari ionic selulose ether kugirango ubyare molekile ntoya ya iyode, itandukanijwe na gaz chromatografiya kandi ikagereranywa nuburyo busanzwe bwimbere kugirango ibone ibiyigize. Usibye hydroxypropyl methylcellulose, ethers ya selile ikwiranye nubu buryo harimo hydroxyethyl selulose, hydroxyethyl methyl selulose, na methyl selulose, kandi uburyo bwo kuvura icyitegererezo burasa.
Ugereranije nuburyo bwa gakondo bwo gutondekanya imiti, isesengura rya gazi chromatografi yisesengura ryibintu bigize selile ya ionic selulose ether ifite ibyiza byinshi. Ihame riroroshye kandi ryoroshye kubyumva, kubaga biroroshye, kandi nta mpamvu yo gutegura imiti myinshi na reagent, bikiza cyane igihe cyo gusesengura. Ibisubizo byabonetse muri ubu buryo birahuye nibyabonetse na titre ya chimique.
Iyo usesenguye ibintu byasimbuwe na gazi chromatografiya, ni ngombwa cyane guhitamo imiterere ikwiye kandi nziza. Mubisanzwe, kugabanya ubushyuhe bwinkingi cyangwa kongera uburebure bwinkingi birashobora kunoza neza imyanzuro, ariko hagomba kwitonderwa kugirango wirinde ibice guhurira mu nkingi kubera ubushyuhe buke bwinkingi.
Kugeza ubu, benshi mu bakora uruganda baracyakoresha titre yimiti kugirango bamenye ibikubiye mubisimburwa. Nyamara, urebye ibyiza nibibi byingingo zinyuranye, gazi chromatografiya nuburyo bworoshye kandi bwihuse bwo kugerageza bukwiye gutezimbere duhereye kubitekerezo byiterambere.