Non-ionic Cellulose Etera na Gas Chromatography

Ua hoʻoholo ʻia ka maʻiʻo o nā mea pani i loko o ka non-ionic cellulose ether e ke kinoea chromatography, a ua hoʻohālikelike ʻia nā hopena me ka titration kemika ma ke ʻano o ka hoʻopau manawa, ka hana, ka pololei, ka repeatability, ke kumukūʻai, etc., a ua kūkākūkā ʻia ka mahana kolamu. ʻO ka mana o nā kūlana chromatographic e like me ka lōʻihi o ke kolamu i ka hopena kaʻawale. Hōʻike nā hualoaʻa i ka chromatography kinoea he ʻano analytical pono e hoʻolaha ʻia.
Hua'ōlelo nui: non-ionic cellulose ether; chromatography kinoea; maʻiʻo pani

Nonionic cellulose ethers me methylcellulose (MC), hydroxypropylmethylcellulose (HPMC), hydroxyethylcellulose (HEC), etc. Ua hoʻohana nui ʻia kēia mau mea i ka lāʻau lapaʻau, meaʻai, petroleum, etc. nā mea ionic cellulose ether, pono e hoʻoholo i ka ʻike o nā substituent me ka pololei a me ka wikiwiki. I kēia manawa, hoʻohana ka hapa nui o nā mea hana hale i ke ʻano titration chemical kuʻuna no ka nānā ʻana, ʻo ia ka mea paʻakikī a paʻakikī e hōʻoia i ka pololei a me ka hana hou. No kēia kumu, ke aʻo nei kēia pepa i ke ʻano o ka hoʻoholo ʻana i ka ʻike o ka non-ionic cellulose ether substituents e ka chromatography gas, e nānā i nā mea e pili ana i nā hopena hōʻike, a loaʻa nā hopena maikaʻi.

1. Hoao
1.1 Mea hana
GC-7800 kinoea chromatograph, hana ʻia e Beijing Purui Analytical Instrument Co., Ltd.
1.2 Reagents
Hydroxypropyl methylcellulose (HPMC), hydroxyethylcellulose (HEC), homemade; methyl iodide, ethyl iodide, isopropane iodide, hydroiodic acid (57%), toluene, adipic acid, o-di Toluene no ka helu analytical.
1.3 Ka hoʻoholo ʻana i ke kinoea chromatography
1.3.1 Nā kūlana chromatography kinoea
Koluma kila kila ((SE-30, 3% Chmmosorb, WAW DMCS); ka wela o ke keena vaporization 200°C; mea ike: TCD, 200°C; ka wela o ke kolamu 100°C; ke kinoea halihali: H2, 40 mL/min.
1.3.2 Hoʻomākaukau i ka hoʻonā maʻamau
(1) Hoʻomākaukau i ka hopena maʻamau i loko: E lawe i kahi 6.25g o toluene a waiho i loko o kahi pahu volumetric 250mL, hoʻoheheʻe i ka māka me ka o-xylene, lulu maikaʻi a waiho ʻia.
(2) Ka hoʻomākaukau ʻana i ka hāʻina maʻamau: loaʻa i nā laʻana like ʻole nā ​​hopena maʻamau, a lawe ʻia nā laʻana HPMC ma ke ʻano he laʻana ma aneʻi. I loko o kahi hue kūpono, e hoʻohui i kekahi nui o ka ʻakika adipic, 2 mL o ka waika hydroiodic a me ka hopena maʻamau i loko, a kaupaona pololei i ka hue. E hoʻohui i ka nui kūpono o ka iodoisopropane, e kaupaona, a e helu i ka nui o ka iodoisopropane i hoʻohui ʻia. E hoʻohui hou i ka methyl iodide, e kaupaona like, e helu i ka nui e hoʻohui i ka methyl iodide. E haʻalulu piha, e kū no ka stratification, a e mālama iā ia mai ka mālamalama no ka hoʻohana ʻana ma hope.
1.3.3 Hoʻomākaukau i ka hāpana hāpana
Pono e kaupaona i ka 0.065 g o ka hāpana HPMC maloʻo i loko o ka 5 mL mānoanoa-pā reactor, e hoʻohui i ke kaumaha like o ka adipic acid, 2 mL o loko o ka wai maʻamau a me ka waika hydroiodic, e hoʻopaʻa koke i ka ʻōmole hopena, a kaupaona pono. E lulu, a e wela ma 150°C no 60 mau minuke, e lulu pono i ka manawa. Maanu a kaumaha. Inā ʻoi aku ka nui o ke kaumaha ma mua a ma hope o ka hopena ma mua o 10 mg, ʻaʻole pono ka hāpana hāpana a pono e hoʻomākaukau hou ʻia ka hopena. Ma hope o ka ʻae ʻia ʻana o ka hāpana hāpana e kū no ka stratification, e kahakii pono i 2 μL o ka hopena o ka lāʻau kūlohelohe luna, e hoʻokomo i loko o ka chromatograph kinoea, a hoʻopaʻa i ke kikoʻī. ʻO nā mea ʻē aʻe non-ionic cellulose ether samples i mālama like me HPMC.
1.3.4 Ana kumu
I ka lawe ʻana i ka HPMC ma ke ʻano he laʻana, he cellulose alkyl hydroxyalkyl mixed ether, i hui pū ʻia me ka waika hydroiodic e wāwahi i nā mea paʻa methoxyl a me hydroxypropoxyl ether a hoʻoulu i ka iodoalkane pili.
Ma lalo o ke kiʻekiʻe o ka wela a me ka ea, me ka adipic acid ma ke ʻano he catalyst, HPMC reacts me hydroiodic acid, a me ka methoxyl a me hydroxypropoxyl ua hoʻololi ʻia i methyl iodide a me isopropane iodide. Ke hoʻohana nei i ka o-xylene e like me ka absorbent a me ka solvent, ʻo ke kuleana o ka catalyst a me ka absorbent e hoʻolaha i ka hopena hydrolysis piha. Koho ʻia ʻo Toluene ma ke ʻano o ka hopena maʻamau i loko, a hoʻohana ʻia ka methyl iodide a me ka isopropane iodide e like me ka hopena maʻamau. Wahi a nā wahi kiʻekiʻe o ka maʻamau kūloko a me ka hopena maʻamau, hiki ke helu ʻia ka ʻike o ka methoxyl a me ka hydroxypropoxyl i ka hāpana.

2. Nā hopena a me ke kūkākūkā
ʻAʻole polar ke kolamu chromatographic i hoʻohana ʻia i kēia hoʻokolohua. Wahi a ka helu hoʻolapalapa o kēlā me kēia ʻāpana, ʻo ke kauoha kiʻekiʻe he methyl iodide, isopropane iodide, toluene a me ka o-xylene.
2.1 Hoʻohālikelike ma waena o ka chromatography kinoea a me ka titration kemika
ʻO ka hoʻoholo ʻana o ka methoxyl a me ka hydroxypropoxyl content o HPMC e ka titration kemika he ʻano makua, a i kēia manawa aia ʻelua ʻano hana maʻamau: ʻo ke ʻano Pharmacopoeia a me ke ʻano i hoʻomaikaʻi ʻia. Eia nō naʻe, ʻo kēia mau ʻano kemika ʻelua e koi i ka hoʻomākaukau ʻana i ka nui o nā hoʻonā, paʻakikī ka hana, hoʻopau manawa, a hoʻopilikia nui ʻia e nā kumu o waho. Ma ka ʻōlelo pili, maʻalahi loa ka chromatography gas, maʻalahi ke aʻo a hoʻomaopopo.
Ua hoʻoholo ʻia nā hopena o ka maʻiʻo methoxyl (w1) a me ka maʻiʻo hydroxypropoxyl (w2) ma HPMC e ka chromatography kinoea a me ka titration kemika. Hiki ke ʻike ʻia he kokoke loa nā hopena o kēia mau ʻano ʻelua, e hōʻike ana e hiki i nā ʻano ʻelua ke hōʻoia i ka pololei o nā hopena.
Ke hoʻohālikelike nei i ka titration kemika a me ka chromatography gas e pili ana i ka hoʻohana ʻana i ka manawa, ka maʻalahi o ka hana, ka hoʻihoʻi ʻana a me ke kumukūʻai, hōʻike nā hopena i ka pōmaikaʻi nui loa o ka chromatography phase ʻo ia ka maʻalahi, ka wikiwiki a me ka hana kiʻekiʻe. ʻAʻohe pono e hoʻomākaukau i ka nui o nā reagents a me nā hoʻonā, a ʻoi aku ka nui o nā minuke he ʻumi e ana i kahi hāpana, a ʻoi aku ka nui o ka manawa maoli i mālama ʻia ma mua o nā helu. Ma ke ʻano titration chemical, ʻoi aku ka nui o ka hewa o ke kanaka i ka hoʻoholo ʻana i ka helu hope titration, ʻoiai ʻoi aku ka liʻiliʻi o nā hopena hoʻāʻo chromatography gas e nā kumu kanaka. Eia kekahi, ʻo ke kinoea chromatography kahi ʻenehana hoʻokaʻawale e hoʻokaʻawale i nā huahana hopena a helu iā lākou. Inā hiki iā ia ke hana pū me nā mea ana ʻē aʻe, e like me GC/MS, GC/FTIR, a me nā mea ʻē aʻe, hiki ke hoʻohana ʻia e ʻike i kekahi mau laʻana paʻakikī i ʻike ʻole ʻia (nā fibers i hoʻololi ʻia) ʻoi aku ka maikaʻi o nā huahana ether. . Eia kekahi, ʻoi aku ka maikaʻi o ka hana hou ʻana o nā hopena chromatography kinoea ma mua o ka titration kemika.
ʻO ka hemahema o ka chromatography kinoea he kiʻekiʻe ke kumukūʻai. ʻO ke kumukūʻai mai ka hoʻokumu ʻia ʻana o ke kahua chromatography gas a hiki i ka mālama ʻana i ka mea kani a me ke koho ʻana i ke kolamu chromatographic ʻoi aku ka kiʻekiʻe ma mua o ke ʻano o ka titration chemical. ʻO nā ʻano hoʻonohonoho like ʻole a me nā kūlana hoʻāʻo e pili pū i nā hopena, e like me ke ʻano Detector, kolamu chromatographic a me ke koho ʻana o ka pae paʻa, etc.
2.2 Ka hopena o nā kūlana chromatography kinoea i nā hopena hoʻoholo
No nā hoʻokolohua chromatography kinoea, ʻo ke kī ke hoʻoholo i nā kūlana chromatographic kūpono e loaʻa ai nā hopena pololei. I loko o kēia hoʻokolohua, ua hoʻohana ʻia ka hydroxyethylcellulose (HEC) a me ka hydroxypropylmethylcellulose (HPMC) ma ke ʻano he mea maka, a ua aʻo ʻia ka mana o nā kumu ʻelua, ka mahana o ke kolamu a me ka lōʻihi o ke kolamu.
Ke degere o ka hoʻokaʻawale ʻana R ≥ 1.5, ua kapa ʻia ʻo ia ka hoʻokaʻawale piha. Wahi a nā ʻōlelo o "Pharmacopoeia Kina", ʻoi aku ka nui o R ma mua o 1.5. Hoʻohuiʻia me ka mahana o ke kolamu iʻekolu mau mahana,ʻoi aku ka nui o ka hoʻonāʻana o kēlā me kēia māhele ma mua o 1.5, e kūpono ana i nā koi hoʻokaʻawale kumu,ʻo ia hoʻi R90 ° C> R100 ° C> R110 ° C. Ma ka noʻonoʻo ʻana i ke kumu huelo, ʻo ke kumu huelo r>1 ka piko huelo, ʻo ka r<1 ka piko mua, a ʻo ka hoʻokokoke ʻana o ka r i ka 1, ʻoi aku ka maikaʻi o ka hana o ke kolamu chromatographic. No ka toluene a me ka ethyl iodide, R90 ° C> R100 ° C> R110 ° C; ʻO ka o-xylene ka mea hoʻoheheʻe me ka helu hoʻolapalapa kiʻekiʻe loa, R90°C
Hōʻike ka mana o ka lōʻihi o ke kolamu ma nā hopena hoʻokolohua ma lalo o nā kūlana like, hoʻololi wale ʻia ka lōʻihi o ke kolamu chromatographic. Ke hoʻohālikelike ʻia me ke kolamu i hoʻopaʻa ʻia o 3m a me 2m, ʻoi aku ka maikaʻi o nā hopena loiloi a me ka hoʻonā ʻana o ke kolamu 3m, a ʻoi aku ka lōʻihi o ke kolamu, ʻoi aku ka maikaʻi o ke kolamu. ʻO ke kiʻekiʻe o ka waiwai, ʻoi aku ka hilinaʻi o ka hopena.

3. Ka hopena
Hoʻohana ʻia ka waikawa Hydroiodic e hoʻopau i ka paʻa eter o ka non-ionic cellulose ether e hana i ka iodide mole liʻiliʻi, i hoʻokaʻawale ʻia e ka chromatography kinoea a helu ʻia e ke ʻano maʻamau o loko e loaʻa ai ka ʻike o ka mea pani. Ma waho aʻe o ka hydroxypropyl methylcellulose, nā cellulose ethers kūpono no kēia ʻano hana me ka hydroxyethyl cellulose, hydroxyethyl methyl cellulose, a me ka methyl cellulose, a ua like ke ʻano o ka lāʻau lapaʻau.
Hoʻohālikelike ʻia me ke ʻano titration kemika kuʻuna, ʻo ka loiloi chromatography kinoea o ka ʻike substituent o ka non-ionic cellulose ether he nui nā pono. He maʻalahi a maʻalahi ka hoʻomaopopo ʻana i ka loina, maʻalahi ka hana, ʻaʻohe pono e hoʻomākaukau i ka nui o nā lāʻau lapaʻau a me nā reagents, kahi e mālama nui ai i ka manawa loiloi. Ua kūlike nā hopena i loaʻa ma kēia ʻano me nā hopena i loaʻa ma ka titration kemika.
I ka nānā ʻana i nā ʻike substituent e ka chromatography gas, he mea nui e koho i nā kūlana chromatographic kūpono a maikaʻi loa. ʻO ka mea maʻamau, ʻo ka hoʻemi ʻana i ka mahana o ke kolamu a i ʻole ka hoʻonui ʻana i ka lōʻihi o ke kolamu hiki ke hoʻomaikaʻi maikaʻi i ka hoʻonā ʻana, akā pono e mālama i ka pale ʻana i nā ʻāpana mai ka condensing i ke kolamu ma muli o ka haʻahaʻa haʻahaʻa o ke kolamu.
I kēia manawa, ke hoʻohana nei ka hapa nui o nā mea hana hale i ka titration kemika e hoʻoholo i ka ʻike o nā substituent. Eia nō naʻe, e noʻonoʻo ana i nā pono a me nā hemahema o nā ʻano like ʻole, ʻo ka gas chromatography kahi ala hoʻāʻo maʻalahi a wikiwiki hoʻi e hoʻolaha ʻia mai ka ʻike o nā ʻano hoʻomohala.