Cellulose Ether na-abụghị ionic nke Gas Chromatography

A na-ekpebi ọdịnaya nke ihe ndị na-anọchi anya na cellulose ether na-abụghị ionic site na chromatography gas, a na-atụlekwa nsonaazụ ya na titration kemịkalụ na-ewe oge, ọrụ, izi ezi, nkwughachi, ọnụ ahịa, wdg, na kọlụm okpomọkụ a tụlere. Mmetụta nke ọnọdụ chromatographic dị ka ogologo kọlụm na mmetụta nkewa. Nsonaazụ na-egosi na chromatography gas bụ usoro nyocha kwesịrị ka ewu ewu.
Isi okwu: ether cellulose na-abụghị ionic; chromatography gas; ọdịnaya dochie anya

Nonionic cellulose ethers na-agụnye methylcellulose (MC), hydroxypropylmethylcellulose (HPMC), hydroxyethylcellulose (HEC), wdg A na-eji ihe ndị a n'ọtụtụ ebe na nkà mmụta ọgwụ, nri, mmanụ ala, wdg Ebe ọ bụ na ọdịnaya nke substituents nwere mmetụta dị ukwuu na arụmọrụ nke ndị na-abụghị. ionic cellulose ether ihe, ọ dị mkpa iji chọpụta ọdịnaya nke ihe nnọchi anya nke ọma na ngwa ngwa. Ka ọ dị ugbu a, ọtụtụ ndị na-emepụta ụlọ na-agbaso usoro titration kemịkalụ ọdịnala maka nyocha, nke na-arụ ọrụ siri ike ma sie ike ikwenye izi ezi na nkwughachi. N'ihi nke a, akwụkwọ a na-amụ usoro iji chọpụta ihe ndị na-emepụta ihe na-abụghị ionic cellulose ether site na chromatography gas, na-enyocha ihe ndị na-emetụta nsonaazụ ule, ma nweta nsonaazụ dị mma.

1. Nnwale
1.1 Ngwa
GC-7800 gas chromatograph, nke Beijing Purui Analytical Instrument Co., Ltd mepụtara.
1.2 Reagent
Hydroxypropyl methylcellulose (HPMC), hydroxyethylcellulose (HEC), arụrụ n'ụlọ; methyl iodide, ethyl iodide, isopropane iodide, hydroiodic acid (57%), toluene, adipic acid, o-di Toluene bụ ọkwa nyocha.
1.3 Mkpebi chromatography gas
1.3.1 Ọnọdụ chromatography gas
Kọlụm igwe anaghị agba nchara ((SE-30, 3% Chmmosorb, WAW DMCS); ọnụ ụlọ okpomọkụ 200°C; nchọpụta: TCD, 200°C; kọlụm okpomọkụ 100°C; gas na-ebu: H2, 40 mL/min.
1.3.2 Nkwadebe nke ọkọlọtọ ngwọta
(1) Nkwadebe nke ngwọta dị n'ime: Were ihe dị ka 6.25g nke toluene ma tinye ya na 250mL volumetric flask, gbanye akara na o-xylene, maa jijiji nke ọma ma wepụ ya.
(2) Nkwadebe nke ọkọlọtọ ọkọlọtọ: dị iche iche samples nwere kwekọrọ ọkọlọtọ ngwọta, na HPMC samples na-ewere dị ka ihe atụ ebe a. Na vial kwesịrị ekwesị, tinye ntakịrị adipic acid, 2 ml nke hydroiodic acid na ngwọta dị n'ime, ma tụọ vial ahụ nke ọma. Tinye ego kwesịrị ekwesị nke iodoisopropane, tụọ ya, gbakọọ ego iodoisopropane agbakwunyere. Tinye methyl iodide ọzọ, tụọ nha nha, gbakọọ ego na-agbakwunye methyl iodide. Ma jijiji nke ọma, hapụ ya ka ọ guzoro maka stratification, ma mee ka ọ ghara ịdị ọkụ maka iji mechaa.
1.3.3 Nkwadebe nke ngwọta sample
Tụru nke ọma 0.065 g nke ihe nlele HPMC kpọrọ nkụ n'ime reactor nwere mgbidi 5 ml, gbakwunye adipic acid nha nha nha, 2 ml nke ihe ngwọta dị n'ime na hydroiodic acid, mechie karama mmeghachi omume ngwa ngwa, wee tụọ ya nke ọma. Ghichaa, ma kpoo ọkụ na 150 ° C maka nkeji 60, na-ama jijiji nke ọma n'oge oge ahụ. Jụụ wee tụọ. Ọ bụrụ na ọnwụ dị arọ tupu na mgbe mmeghachi omume ahụ karịrị 10 mg, ngwọta nlele abaghị uru ma ọ dị mkpa ka edozighachi ngwọta ahụ. Mgbe ahapụchara ihe nlele ahụ ka ọ guzoro maka stratification, jiri nlezianya dọpụta 2 μL nke ihe ngwọta nke elu organic, gbanye ya na chromatograph gas, wee dekọọ ụdịdị ahụ. A na-emeso ihe nlele ether cellulose ndị ọzọ na-abụghị ionic n'otu aka ahụ na HPMC.
1.3.4 Ụkpụrụ nha
N'iji HPMC dịka ọmụmaatụ, ọ bụ cellulose alkyl hydroxyalkyl agwakọta ether, nke a na-ejikọta ya na hydroiodic acid iji mebie methoxyl na hydroxypropoxyl ether bonds ma mepụta iodoalkane kwekọrọ.
N'okpuru ọnọdụ okpomọkụ dị elu na ikuku ikuku, yana adipic acid dị ka ihe na-eme ka ọ bụrụ ihe na-eme ka HPMC na-emeghachi omume na hydroiodic acid, na methoxyl na hydroxypropoxyl na-agbanwe ghọọ methyl iodide na isopropane iodide. N'iji o-xylene dị ka ihe mgbaze na ihe mgbaze, ọrụ nke na-akpali akpali na ntinye aka bụ ịkwalite mmeghachi omume hydrolysis zuru ezu. A na-ahọrọ Toluene dị ka ihe ngwọta dị n'ime, a na-ejikwa methyl iodide na isopropane iodide mee ihe dị ka ngwọta ọkọlọtọ. Dị ka akụkụ kachasị elu nke ọkọlọtọ dị n'ime na ngwọta ọkọlọtọ, enwere ike gbakọọ ọdịnaya nke metoxyl na hydroxypropoxyl na nlele.

2. Nsonaazụ na mkparịta ụka
Kọlụm chromatographic ejiri mee nnwale a abụghị polar. Dị ka isi ihe na-esi ísì ụtọ nke akụkụ nke ọ bụla, usoro kachasị elu bụ methyl iodide, isopropane iodide, toluene na o-xylene.
2.1 Ntụle n'etiti gas chromatography na kemịkalụ titration
Mkpebi nke methoxyl na hydroxypropoxyl nke HPMC site na titration kemịkalụ tozuru oke, ma ugbu a enwere ụzọ abụọ a na-ejikarị: usoro Pharmacopoeia na usoro emelitere. Otú ọ dị, ụzọ abụọ a nke kemịkal na-achọ nkwadebe nke nnukwu ngwọta, ọrụ ahụ na-agbagwoju anya, na-ewe oge, na-emetụtakwa ihe ndị dị n'èzí. N'ikwu okwu, chromatography gas dị nnọọ mfe, dị mfe ịmụta na nghọta.
Ihe nchoputa nke ọdịnaya metxyl (w1) na hydroxypropoxyl (w2) dị na HPMC bụ chromatography gas na titration kemịkalụ siri n'otu n'otu kpebisie ike. Enwere ike ịhụ na nsonaazụ nke ụzọ abụọ a dị ezigbo nso, na-egosi na ụzọ abụọ a nwere ike ikwe nkwa izi ezi nke nsonaazụ ya.
N'ịtụle kemịkalụ kemịkalụ na chromatography gas n'ihe gbasara oge oriri, ịdị mfe nke ịrụ ọrụ, nkwughachi na ọnụ ahịa, nsonaazụ na-egosi na nnukwu uru nke chromatography nke oge bụ ịdị mma, ngwa ngwa na arụmọrụ dị elu. Ọ dịghị mkpa iji kwadebe a nnukwu ego nke reagents na ngwọta, na ọ na-ewe ihe karịrị nkeji iri na-atụ a sample, na n'ezie oge echekwara ga-abụ ukwuu karịa ọnụ ọgụgụ. N'ime usoro titration kemịkalụ, njehie mmadụ na-ekpe ikpe njedebe njedebe titration buru ibu, ebe nsonaazụ ule chromatography gas na-emetụtaghị ihe mmadụ. Ọzọkwa, chromatography gas bụ usoro nkewa nke na-ekewa ngwaahịa mmeghachi omume ma na-atụle ha. Ọ bụrụ na ọ nwere ike imekọ ihe na ngwa ihe atụ ndị ọzọ, dị ka GC/MS, GC/FTIR, wdg, enwere ike iji ya chọpụta ụfọdụ ihe nlere anya amaghi ama (fibre emezigharị) Plain ether ngwaahịa) bara ezigbo uru, nke na-enweghị atụ na titration kemịkalụ. . Na mgbakwunye, mmeghari nke nsonaazụ chromatography gas dị mma karịa nke titration kemịkalụ.
Ihe ọghọm nke chromatography gas bụ na ọnụ ahịa ya dị elu. Ọnụ ego sitere na nguzobe nke gas chromatography ọdụ na-edozi ngwá ọrụ na nhọrọ nke kọlụm chromatographic dị elu karịa nke usoro titration kemịkalụ. Nhazi ngwá ọrụ dị iche iche na ọnọdụ ule ga-emetụtakwa nsonaazụ ya, dị ka ụdị nchọpụta, kọlụm chromatographic na nhọrọ nke oge nkwụsị, wdg.
2.2 Mmetụta nke ọnọdụ chromatography gas na nsonaazụ mkpebi siri ike
Maka nnwale chromatography gas, isi ihe bụ iji chọpụta ọnọdụ chromatographic kwesịrị ekwesị iji nweta nsonaazụ ziri ezi. Na nnwale a, a na-eji hydroxyethylcellulose (HEC) na hydroxypropylmethylcellulose (HPMC) mee ihe dị ka akụrụngwa, na mmetụta nke ihe abụọ, okpomọkụ kọlụm na ogologo kọlụm.
Mgbe ogo nkewa R ≥ 1.5, a na-akpọ ya nkewa zuru oke. Dị ka ndokwa nke "Chinese Pharmacopoeia", R kwesịrị ịbụ ihe karịrị 1.5. Ejikọtara ya na kọlụm okpomọkụ na okpomọkụ atọ, mkpebi nke akụkụ ọ bụla karịrị 1.5, nke na-ezute ihe ndị dị mkpa nkewa, nke bụ R90 ° C> R100 ° C> R110 ° C. N'ịtụle ihe kpatara ọdụdụ, ihe na-akpata ọdụ r> 1 bụ ọdụdụ ọdụdụ, r<1 bụ ọnụ ọgụgụ dị n'ihu, na nso r dị na 1, ka mma ịrụ ọrụ nke kọlụm chromatographic. Maka toluene na ethyl iodide, R90°C>R100°C>R110°C; o-xylene bụ ihe mgbaze nwere ebe isi mmiri kachasị elu, R90 Celsius
Mmetụta nke ogologo kọlụm na nsonaazụ nnwale na-egosi na n'okpuru otu ọnọdụ ahụ, naanị ogologo ogologo kọlụm chromatographic gbanwere. E jiri ya tụnyere kọlụm juru n'ọnụ nke 3m na 2m, nsonaazụ nyocha na mkpebi nke kọlụm 3m dị mma, na ogologo oge nke kọlụm, ka kọlụm dị mma. Ọnụ ahịa dị elu, nke a pụrụ ịdabere na ya pụta.

3. Nkwubi okwu
A na-eji hydroiodic acid mebie njikọ ether nke cellulose ether na-abụghị ionic iji mepụta obere iodide molecule, nke kewapụrụ site na chromatography gas ma tụọ ya site na usoro ọkọlọtọ dị n'ime iji nweta ọdịnaya nke ihe nnọchi anya. Na mgbakwunye na hydroxypropyl methylcellulose, cellulose ethers kwesịrị ekwesị maka usoro a gụnyere hydroxyethyl cellulose, hydroxyethyl methyl cellulose, na methyl cellulose, na sample usoro ọgwụgwọ yiri.
E jiri ya tụnyere usoro titration kemịkalụ ọdịnala, nyocha chromatography gas nke ihe ngbanwe nke ether cellulose na-abụghị ionic nwere ọtụtụ uru. Ụkpụrụ ahụ dị mfe ma dị mfe nghọta, ọrụ ahụ dị mma, ọ dịghịkwa mkpa ịkwadebe nnukwu ọgwụ na reagents, nke na-echekwa oge nyocha nke ukwuu. Nsonaazụ enwetara site na usoro a kwekọrọ na nke enwetara site na titration kemịkalụ.
Mgbe ị na-enyocha ọdịnaya nọchiri anya site na chromatography gas, ọ dị ezigbo mkpa ịhọrọ ọnọdụ chromatographic kwesịrị ekwesị na kacha mma. N'ozuzu, ibelata okpomoku kọlụm ma ọ bụ ịbawanye ogologo kọlụm nwere ike imezi mkpebi ahụ nke ọma, mana a ga-akpachapụ anya iji gbochie ihe mejupụtara ya na kọlụm n'ihi oke okpomoku kọlụm.
Ka ọ dị ugbu a, ọtụtụ ndị na-emepụta ụlọ ka na-eji kemịkalụ titration iji chọpụta ọdịnaya nke ihe nnọchi anya. Otú ọ dị, n'ịtụle uru na adịghị ike nke akụkụ dị iche iche, gas chromatography bụ usoro nyocha dị mfe na ngwa ngwa kwesịrị ịkwalite site n'echiche nke mmepe mmepe.