Non-ionic Cellulose Ether ta Gas Chromatography

Abubuwan da ke cikin masu maye gurbin a cikin ether ba na ionic cellulose ether an ƙaddara su ta hanyar chromatography na gas, kuma an kwatanta sakamakon tare da titration na sinadarai dangane da cin lokaci, aiki, daidaito, maimaitawa, farashi, da dai sauransu, kuma an tattauna yanayin zafin jiki na shafi. Tasirin yanayin chromatographic kamar tsayin shafi akan tasirin rabuwa. Sakamakon ya nuna cewa gas chromatography hanya ce ta nazari wacce ta cancanci yaɗawa.
Mahimman kalmomi: ether ba ionic cellulose; gas chromatography; abun ciki maimakon

Nonionic cellulose ethers sun hada da methylcellulose (MC), hydroxypropylmethylcellulose (HPMC), hydroxyethylcellulose (HEC), da dai sauransu Wadannan kayan da ake amfani da ko'ina a magani, abinci, man fetur, da dai sauransu Tun da abun ciki na substituents yana da babban tasiri a kan yi na wadanda ba. ionic cellulose ether kayan, wajibi ne don ƙayyade abun ciki na masu maye gurbin daidai da sauri. A halin yanzu, yawancin masana'antun cikin gida suna ɗaukar hanyar titration sinadarai na gargajiya don bincike, wanda ke da aiki mai ƙarfi kuma mai wahala don tabbatar da daidaito da maimaitawa. A saboda wannan dalili, wannan takarda yana nazarin hanyar da za a iya ƙayyade abubuwan da ba a haɗa su ba tare da ion cellulose ether da gas chromatography, nazarin abubuwan da suka shafi sakamakon gwajin, kuma suna samun sakamako mai kyau.

1. Gwaji
1.1 Kayan aiki
GC-7800 gas chromatograph, samar da Beijing Purui Analytical Instrument Co., Ltd.
1.2 Reagents
Hydroxypropyl methylcellulose (HPMC), hydroxyethylcellulose (HEC), na gida; methyl iodide, ethyl iodide, isopropane iodide, hydroiodic acid (57%), toluene, adipic acid, o-di Toluene ya kasance na darajar nazari.
1.3 Gas chromatography ƙaddara
1.3.1 Gas chromatography yanayi
Bakin karfe ginshiƙi ((SE-30, 3% Chmmosorb, WAW DMCS); vaporization dakin zafin jiki 200°C; ganowa: TCD, 200°C; shafi zafin jiki 100°C; iskar gas: H2, 40 mL/min.
1.3.2 Shiri na daidaitaccen bayani
(1) Shiri na daidaitaccen bayani na ciki: Ɗauki kimanin 6.25g na toluene kuma sanya a cikin gilashin 250mL mai girma, tsarma zuwa alamar tare da o-xylene, girgiza da kyau kuma ajiye.
(2) Shiri na daidaitaccen bayani: samfurori daban-daban suna da daidaitattun daidaitattun mafita, kuma ana ɗaukar samfurori na HPMC a matsayin misali a nan. A cikin vial mai dacewa, ƙara wani adadin adipic acid, 2 ml na hydroiodic acid da daidaitaccen bayani na ciki, kuma auna gwargwado daidai. Ƙara adadin da ya dace na iodoisopropane, auna shi, kuma ƙididdige adadin iodoisopropane da aka ƙara. Ƙara methyl iodide kuma, auna daidai, ƙididdige adadin da ke ƙara methyl iodide. Yi rawar jiki sosai, bar shi ya tsaya don daidaitawa, kuma kiyaye shi daga haske don amfani daga baya.
1.3.3 Shiri na samfurin bayani
Daidai auna 0.065 g na busassun samfurin HPMC a cikin injin mai kauri mai kauri 5 ml, ƙara daidai nauyin adipic acid, 2 ml na daidaitaccen bayani na ciki da acid hydroiodic, da sauri rufe kwalban amsawa, kuma auna shi daidai. girgiza, da zafi a 150 ° C na minti 60, girgiza da kyau a lokacin lokacin. Sanyi da auna. Idan asarar nauyi kafin da bayan abin da ya fi girma fiye da 10 MG, samfurin samfurin ba shi da inganci kuma ana buƙatar sake shirya maganin. Bayan an ba da izinin samfurin samfurin ya tsaya don ƙaddamarwa, zana 2 μL a hankali na babban bayani na kwayoyin halitta, saka shi a cikin chromatograph gas, kuma rikodin bakan. Sauran samfuran ether da ba na ionic cellulose ba an bi da su daidai da HPMC.
1.3.4 Ka'idar aunawa
Ɗaukar HPMC a matsayin misali, shi ne cellulose alkyl hydroxyalkyl gauraye ether, wanda aka hade tare da hydroiodic acid don karya duk methoxyl da hydroxypropoxyl ether bond kuma samar da daidai iodoalkane.
A karkashin yanayin zafi mai zafi da iska, tare da adipic acid a matsayin mai haɓakawa, HPMC yana amsawa tare da acid hydroiodic, kuma metoxyl da hydroxypropoxyl an canza su zuwa methyl iodide da isopropane iodide. Yin amfani da o-xylene a matsayin mai narkewa da ƙarfi, aikin mai kara kuzari da abin sha shine don haɓaka cikakkiyar amsawar hydrolysis. An zaɓi Toluene a matsayin daidaitaccen bayani na ciki, kuma ana amfani da methyl iodide da isopropane iodide azaman daidaitaccen bayani. Dangane da wuraren kololuwar ma'auni na ciki da daidaitaccen bayani, ana iya ƙididdige abun ciki na methoxyl da hydroxypropoxyl a cikin samfurin.

2. Sakamako da tattaunawa
Rukunin chromatographic da aka yi amfani da shi a cikin wannan gwaji ba iyakacin duniya ba ne. Dangane da wurin tafasa na kowane sashi, tsari mafi girma shine methyl iodide, isopropane iodide, toluene da o-xylene.
2.1 Kwatanta tsakanin gas chromatography da sinadarai titration
Ƙayyadaddun abun ciki na methoxyl da hydroxypropoxyl na HPMC ta hanyar sinadarai yana da ɗan girma, kuma a halin yanzu akwai hanyoyi guda biyu da ake amfani da su: hanyar Pharmacopoeia da ingantacciyar hanya. Koyaya, duka waɗannan hanyoyin sinadarai guda biyu suna buƙatar shirye-shiryen babban adadin mafita, aikin yana da rikitarwa, yana ɗaukar lokaci, kuma abubuwan waje suna da tasiri sosai. Dangantakar magana, chromatography gas abu ne mai sauqi, mai sauƙin koya da fahimta.
Sakamakon abun ciki na methoxyl (w1) da abun ciki na hydroxypropoxyl (w2) a cikin HPMC an ƙaddara su ta hanyar chromatography gas da sinadarai bi da bi. Ana iya ganin cewa sakamakon wadannan hanyoyin guda biyu yana da kusanci sosai, wanda ke nuni da cewa dukkan hanyoyin biyu za su iya tabbatar da daidaiton sakamakon.
Kwatanta titration na sinadarai da gas chromatography dangane da amfani da lokaci, sauƙin aiki, maimaitawa da farashi, sakamakon ya nuna cewa babbar fa'idar chromatography na lokaci shine dacewa, saurin sauri da inganci. Babu buƙatar shirya babban adadin reagents da mafita, kuma yana ɗaukar fiye da mintuna goma don auna samfurin, kuma ainihin lokacin da aka adana zai zama mafi girma fiye da kididdiga. A cikin hanyar titration na sinadarai, kuskuren ɗan adam wajen yin hukunci akan ƙarshen ƙarshen titration yana da girma, yayin da sakamakon gwajin chromatography na gas ba shi da tasiri ga abubuwan ɗan adam. Haka kuma, iskar gas chromatography dabara ce ta rabuwa da ke raba samfuran amsawa da ƙididdige su. Idan za ta iya yin aiki tare da sauran kayan aunawa, kamar GC/MS, GC/FTIR, da sauransu, ana iya amfani da shi don gano wasu hadaddun samfuran da ba a san su ba (filayen da aka gyara) samfuran ether na Plain) suna da fa'ida sosai, wanda bai dace da titration na sinadarai ba. . Bugu da ƙari, sake haifar da sakamakon chromatography gas ya fi na titration sunadarai.
Rashin hasara na chromatography gas shine cewa farashin yana da yawa. Farashin daga kafa tashar chromatography gas zuwa kiyaye kayan aiki da zaɓin ginshiƙi na chromatographic ya fi na hanyar titration sinadarai. Saitunan kayan aiki daban-daban da yanayin gwaji kuma zasu shafi sakamakon, kamar nau'in ganowa, ginshiƙin chromatographic da zaɓi na lokaci mai tsayi, da sauransu.
2.2 Tasirin yanayin chromatography gas akan sakamakon ƙaddara
Don gwaje-gwajen chromatography na gas, mabuɗin shine don ƙayyade yanayin chromatographic da ya dace don samun ƙarin ingantaccen sakamako. A cikin wannan gwaji, an yi amfani da hydroxyethylcellulose (HEC) da hydroxypropylmethylcellulose (HPMC) azaman albarkatun ƙasa, kuma an yi nazarin tasirin abubuwa biyu, zafin shafi da tsayin shafi.
Lokacin da matakin rabuwa R ≥ 1.5, ana kiran shi cikakken rabuwa. Bisa ga tanadi na "Pharmacopoeia na kasar Sin", R ya kamata ya fi 1.5. Haɗe tare da zafin jiki na ginshiƙi a yanayin zafi uku, ƙudurin kowane sashi ya fi 1.5, wanda ya dace da ainihin buƙatun rabuwa, waɗanda R90 ° C> R100 ° C> R110 ° C. Idan aka yi la'akari da ma'aunin wutsiya, factor r> 1 shine mafi girman wutsiya, r<1 shine tsayin gaba, kuma mafi kusa da r shine 1, mafi kyawun aikin ginshiƙi na chromatographic. Don toluene da ethyl iodide, R90 ° C> R100 ° C> R110 ° C; o-xylene shine sauran ƙarfi tare da mafi girman wurin tafasa, R90 ° C
Tasirin tsayin ginshiƙi akan sakamakon gwaji ya nuna cewa a ƙarƙashin yanayi iri ɗaya, kawai tsawon ginshiƙin chromatographic ya canza. Idan aka kwatanta da ginshiƙi mai cike da 3m da 2m, sakamakon bincike da ƙuduri na ginshiƙi na 3m sun fi kyau, kuma tsayin ginshiƙi, mafi kyawun ingancin shafi. Mafi girman darajar, mafi yawan abin dogara sakamakon.

3. Kammalawa
Ana amfani da acid hydroiodic don lalata haɗin ether na ether maras ionic cellulose don samar da ƙananan ƙwayoyin iodide, wanda aka rabu da gas chromatography kuma an ƙididdige shi ta hanyar daidaitaccen ciki don samun abun ciki na madaidaicin. Baya ga hydroxypropyl methylcellulose, ethers cellulose da suka dace da wannan hanya sun haɗa da hydroxyethyl cellulose, hydroxyethyl methyl cellulose, da methyl cellulose, kuma hanyar samfurin magani yana kama da haka.
Idan aka kwatanta da hanyar titration na sinadarai na gargajiya, bincike na chromatography na iskar gas na madaidaicin abun ciki na ether maras ionic cellulose yana da fa'idodi da yawa. Ka'idar ita ce mai sauƙi kuma mai sauƙin fahimta, aikin ya dace, kuma babu buƙatar shirya babban adadin magunguna da reagents, wanda ke adana lokacin bincike sosai. Sakamakon da aka samu ta wannan hanyar ya yi daidai da waɗanda aka samu ta hanyar sinadarai.
Lokacin nazarin abubuwan da ke musanya ta hanyar chromatography gas, yana da matukar mahimmanci a zaɓi dacewa kuma mafi kyawun yanayin chromatographic. Gabaɗaya, rage zafin ginshiƙi ko haɓaka tsayin ginshiƙi na iya haɓaka ƙuduri yadda ya kamata, amma dole ne a kula don hana abubuwan haɗin gwiwa daga takura a cikin ginshiƙi saboda ƙarancin zafin shafi.
A halin yanzu, yawancin masana'antun cikin gida har yanzu suna amfani da titration na sinadarai don tantance abubuwan da ke maye gurbinsu. Duk da haka, la'akari da fa'ida da rashin amfani na bangarori daban-daban, chromatography gas hanya ce mai sauƙi da sauri don ingantawa daga yanayin ci gaba.