Non-ionic Cellulose Ether neGasi Chromatography

Zviri mukati mezvinotsiva mu-non-ionic cellulose ether zvakatemwa negasi chromatography, uye mhedzisiro yakaenzaniswa nekemikari titration maererano nekutora nguva, kushanda, kurongeka, kudzokorora, mutengo, nezvimwewo, uye tembiricha yekoramu yakakurukurwa. Kurudziro yemamiriro echromatographic senge kureba kwekoramu pane yekuparadzanisa maitiro. Mhedzisiro yacho inoratidza kuti gasi chromatography inzira yekuongorora inofanirwa kufarirwa.
Mazwi akakosha: non-ionic cellulose ether; gasi chromatography; substituent content

Nonionic cellulose ethers inosanganisira methylcellulose (MC), hydroxypropylmethylcellulose (HPMC), hydroxyethylcellulose (HEC), etc. Zvinhu izvi zvinoshandiswa zvakanyanya mumishonga, zvokudya, petroleum, nezvimwewo. ionic cellulose ether zvinhu, zvinodikanwa kuti uone zvirimo zvezvinotsiva zvakarurama uye nekukurumidza. Parizvino, vagadziri vazhinji vepamba vanotora nzira yechinyakare chemakemikari titration yekuongorora, iyo inoshanda nesimba uye yakaoma kuvimbisa chokwadi uye kudzokorora. Nokuda kwechikonzero ichi, pepa rino rinoongorora nzira yekuona zvinyorwa zve-non-ionic cellulose ether substituents negasi chromatography, inoongorora zvinhu zvinokanganisa mhinduro dzebvunzo, uye inowana migumisiro yakanaka.

1. Kuedza
1.1 Chiridzwa
GC-7800 gasi chromatograph, yakagadzirwa naBeijing Purui Analytical Instrument Co., Ltd.
1.2 Reagents
Hydroxypropyl methylcellulose (HPMC), hydroxyethylcellulose (HEC), yakagadzirwa kumba; methyl iodide, ethyl iodide, isopropane iodide, hydroiodic acid (57%), toluene, adipic acid, o-di Toluene yaive yegiredhi rekuongorora.
1.3 Gasi chromatography kutsunga
1.3.1 Gasi chromatography mamiriro
Stainless simbi column ((SE-30, 3% Chmmosorb, WAW DMCS); vaporization mukamuri tembiricha 200°C; detector: TCD, 200°C; column tembiricha 100°C; mutakuri gasi: H2, 40 mL/min.
1.3.2 Kugadzirira kwemhinduro yakajairwa
(1) Kugadzirira kwemukati chiyero mhinduro: Tora inenge 6.25g ye toluene uye isa mu 250mL volumetric flask, dilue kune chiratidzo ne o-xylene, zunza zvakanaka uye uise parutivi.
(2) Kugadzirira kweyakajairwa mhinduro: masampuli akasiyana ane anoenderana akajairwa mhinduro, uye HPMC masampuli anotorwa semuenzaniso pano. Mubhodhoro rakakodzera, wedzera imwe chiyero cheadipic acid, 2 mL yehydroiodic acid uye mukati meyero mhinduro, uye kunyatsoyera vial. Wedzera huwandu hwakakodzera hweiodoisopropane, woiyera, uye verenga huwandu hweiodoisopropane yakawedzerwa. Wedzera methyl iodide zvakare, kuyera zvakaenzana, verenga huwandu hunowedzera methyl iodide. Vibrate zvizere, rega imirire stratification, uye ichengetedze kure nechiedza kuti ishandiswe gare gare.
1.3.3 Kugadzirira kwemuenzaniso mhinduro
Yakanyatso kuyera 0.065 g yeyakaomeswa HPMC sampuli mune 5 mL gobvu-yakavezwa reactor, wedzera huremu hwakaenzana hweadipic acid, 2 mL yemukati muyero mhinduro uye hydroiodic acid, nekukurumidza kuvhara bhodhoro rekuita, uye kunyatsoiyera. Kuzunungusa, uye kupisa pa 150 ° C kwemaminitsi makumi matanhatu, kuzunungusa zvakanaka munguva. Kutonhorera uye kuyera. Kana kurasikirwa kwehuremu kusati kwaitika uye mushure mekuita kwakakura kudarika 10 mg, mhinduro yemuenzaniso haina kukodzera uye mhinduro inoda kugadzirirwa zvakare. Mushure mekunge mhinduro yemuenzaniso yatenderwa kumirira stratification, nyatso dhirowa 2 μL yekumusoro organic chikamu mhinduro, jekiseni mugasi chromatograph, uye rekodha spectrum. Mamwe asiri-ionic cellulose ether samples akabatwa zvakafanana kune HPMC.
1.3.4 Kuyera musimboti
Tichitora HPMC semuenzaniso, ndeye cellulose alkyl hydroxyalkyl yakasanganiswa ether, iyo inodziya pamwe chete nehydroiodic acid kutyora ese methoxyl uye hydroxypropoxyl ether zvisungo uye kugadzira inoenderana iodoalkane .
Pasi pe tembiricha yakakwira uye isina mhepo, ine adipic acid sechinhu chinokonzeresa, HPMC inobata ne hydroiodic acid, uye methoxyl uye hydroxypropoxyl inoshandurwa kuita methyl iodide uye isopropane iodide. Uchishandisa o-xylene seinonyudza uye inonyungudutsa, basa recatalyst uye rinonyudza nderekusimudzira iyo yakazara hydrolysis reaction. Toluene inosarudzwa seyemukati chiyero mhinduro, uye methyl iodide uye isopropane iodide inoshandiswa seyakajairwa mhinduro. Zvinoenderana nepamusoro penzvimbo dzemukati chiyero uye yakajairwa mhinduro, zviri mukati methoxyl uye hydroxypropoxyl mumuenzaniso zvinogona kuverengerwa.

2. Migumisiro uye nhaurirano
Koramu yechromatographic yakashandiswa muchiyedzo ichi haisi-polar. Zvinoenderana nenzvimbo yekubikira yechikamu chimwe nechimwe, iyo peak order ndeye methyl iodide, isopropane iodide, toluene uye o-xylene.
2.1 Kuenzanisa pakati pegasi chromatography uye makemikari titration
Kutemerwa kwemethoxyl uye hydroxypropoxyl zvemukati zveHPMC nekemikari titration yakakura, uye parizvino kune nzira mbiri dzinowanzoshandiswa: iyo Pharmacopoeia nzira uye yakagadziridzwa nzira. Zvisinei, nzira mbiri idzi dzemakemikari dzinoda kugadzirirwa kwehuwandu hwekugadzirisa, kushanda kwakaoma, kunotora nguva, uye kunokonzerwa zvakanyanya nekunze kwezvinhu. Zvichienderana, gasi chromatography iri nyore, iri nyore kudzidza uye kunzwisisa.
Mhedzisiro yemethoxyl yemukati (w1) uye hydroxypropoxyl yemukati (w2) muHPMC yakatemwa negasi chromatography uye kemikari titration zvichiteerana. Zvinogona kuonekwa kuti migumisiro yenzira mbiri idzi dziri pedyo zvikuru, zvichiratidza kuti nzira mbiri dzinogona kuvimbisa chokwadi chemigumisiro.
Kuenzanisa kemikari titration uye gasi chromatography maererano nekushandisa nguva, nyore kushanda, kudzokorora uye mutengo, mhedzisiro inoratidza kuti mukana mukuru wechikamu chromatography kuve nyore, kukurumidza uye kugona kwakanyanya. Hapana chikonzero chekugadzirira yakawanda reagents uye mhinduro, uye zvinongotora anopfuura maminetsi gumi kuyera sampuli, uye nguva chaiyo yakachengetwa ichava yakakura kupfuura manhamba. Mune kemikari titration nzira, kukanganisa kwemunhu mukutonga iyo titration yekupedzisira nzvimbo yakakura, nepo gasi chromatography mhedzisiro yebvunzo haina kukanganiswa nezvinhu zvevanhu. Uyezve, gasi chromatography inzira yekuparadzanisa inoparadzanisa zvigadzirwa zvekuita uye nekuzvienzanisa. Kana ichikwanisa kubatira pamwe nezvimwe zviridzwa zvekuyeresa, zvakaita seGC/MS, GC/FTIR, zvichingodaro, inogona kushandiswa kuona mamwe akaomarara asingazivikanwe samples (modified fibers) Plain ether zvigadzirwa) zvinobatsira kwazvo, izvo zvisingaenzaniswi nekemikari titration. . Uye zvakare, kuberekana kwegasi chromatography mhedzisiro iri nani pane iyo yemakemikari titration.
Izvo zvisingabatsiri zvegasi chromatography ndezvekuti mutengo wakakwira. Mutengo kubva pakugadzwa kwegasi chromatography station kusvika pakuchengetedza chiridzwa uye kusarudzwa kwekromatographic column yakakwirira kupfuura iyo yemakemikari titration nzira. Yakasiyana magadzirirwo ezviridzwa uye mamiriro ekuyedzwa anozokanganisawo mhedzisiro, senge Detector mhando, chromatographic column uye sarudzo yeyakamira chikamu, nezvimwe.
2.2 Kupesvedzera kwegasi chromatography mamiriro pamhedzisiro yekutsunga
Kune gasi chromatography kuyedza, kiyi ndeye kuona akakodzera chromatographic mamiriro kuti uwane mamwe mhedzisiro. Muchiyedzo ichi, hydroxyethylcellulose (HEC) uye hydroxypropylmethylcellulose (HPMC) yakashandiswa seyakagadzirwa, uye pesvedzero yezvinhu zviviri, kupisa kwekoramu uye kureba kwekoramu, zvakadzidzwa.
Apo dhigirii yekuparadzanisa R ≥ 1.5, inonzi kupatsanurwa kwakakwana. Zvinoenderana nezvinodiwa zve "Chinese Pharmacopoeia", R inofanira kunge yakakura kupfuura 1.5. Yakasanganiswa nembiru tembiricha pamatembiricha matatu, kugadzirisa kwechikamu chimwe nechimwe kunopfuura 1.5, iyo inosangana nezvinodiwa zvekuparadzanisa, zvinova R90°C>R100°C>R110°C. Tichifunga nezvemuswe, iyo inoswerera r> 1 ndiyo inoswerera peak, r<1 ndiyo yepamusoro peak, uye iri pedyo r ndeye 1, zvirinani kuita kwekromatographic column. Pa toluene uye ethyl iodide, R90°C>R100°C>R110°C; o-xylene ndiyo inonyungudutsa ine painofashaira yepamusoro, R90°C
Kurudziro yehurefu hwekoramu pamhedzisiro yekuyedza inoratidza kuti pasi pemamiriro mamwe chete, kureba chete kwekoramu yekromatographic kunoshandurwa. Zvichienzaniswa nekoramu yakazara ye3m uye 2m, mhinduro dzekuongorora uye kugadziriswa kwe3m column zviri nani, uye kureba kwekoramu, zviri nani kushanda kwekoramu. Iyo yakakwirira kukosha, iyo yakavimbika mhedzisiro.

3. Mhedziso
Hydroiodic acid inoshandiswa kuparadza ether bond ye-non-ionic cellulose ether kuti ibudise molecule iodide, iyo inoparadzaniswa negasi chromatography uye inofananidzwa nemukati chiyero nzira yekuwana zvinyorwa zvezvinotsiva. Mukuwedzera kune hydroxypropyl methylcellulose, cellulose ethers yakakodzera nzira iyi inosanganisira hydroxyethyl cellulose, hydroxyethyl methyl cellulose, uye methyl cellulose, uye nzira yekurapa yemuenzaniso yakafanana.
Kuenzaniswa neyechinyakare kemikari titration nzira, gasi chromatography kuongororwa kweinotsiva yezvinyorwa zvisiri-ionic cellulose ether ine zvakawanda zvakanaka. Nheyo yacho iri nyore uye iri nyore kunzwisisa, kushanda kuri nyore, uye hapana chikonzero chekugadzirira huwandu hwemishonga uye reagents, iyo inochengetedza zvakanyanya nguva yekuongorora. Migumisiro inowanikwa nenzira iyi inopindirana neiyo inowanikwa nemakemikari titration.
Paunenge uchiongorora substituent content negasi chromatography, zvakakosha zvikuru kusarudza kwakakodzera uye kwakaringana chromatographic mamiriro. Kazhinji, kuderedza kupisa kwembiru kana kuwedzera urefu hwembiru kunogona kuvandudza kugadzirisa, asi kuchenjerera kunofanira kutorwa kudzivirira zvikamu kubva pakunyunguduka mukoramu nekuda kwekuderera kwakanyanya kwekoramu.
Parizvino, vagadziri vazhinji vekumba vachiri kushandisa kemikari titration kuona zvirimo zvezvinotsiva. Nekudaro, tichifunga zvakanakira uye zvakaipira zveakasiyana maficha, gasi chromatography inzira yakapusa uye inokurumidza yekuyedza yakakodzera kusimudzira kubva pamaonero ebudiriro.