Rui Huang, Bo Xu
Cibiyar R&D Application
Gabatarwa
Ion musayar chromatography (IEC) hanya ce ta chromatographic da aka saba amfani da ita don rarrabewa da tsarkake mahaɗan waɗanda aka gabatar a cikin sigar ionic a cikin bayani.Dangane da jihohin caji daban-daban na ions masu musanya, IEC na iya kasu kashi biyu, chromatography musayar cation da chromatography musayar anion.A cikin chromatography musayar cation, ƙungiyoyin acidic suna haɗe zuwa saman kafofin watsa labarai na rabuwa.Misali, sulfonic acid (-SO3H) rukuni ne da aka saba amfani dashi a cikin musayar musayar ƙarfi mai ƙarfi (SCX), wanda ke raba H + da ƙungiyar da ba ta da caji -SO3- don haka za ta iya tallata wasu cations a cikin mafita.A cikin chromatography musayar anion, ƙungiyoyin alkaline suna ɗaure zuwa saman kafofin watsa labarai na rabuwa.Misali, quaternary amine (-NR3OH, inda R shine rukunin hydrocarbon) yawanci ana amfani dashi a cikin musayar musayar ƙarfi (SAX), wanda ke raba OH- da ƙungiyar da aka caje ta gaskiya -N + R3 na iya ɗaukar sauran anions a cikin maganin, yana haifar da anion. musayar tasiri.
Daga cikin samfuran halitta, flavonoids sun ja hankalin masu bincike saboda rawar da suke takawa wajen rigakafi da magance cututtukan zuciya.Tun da ƙwayoyin flavonoid acidic ne saboda kasancewar ƙungiyoyin phenolic hydroxyl, ion musayar chromatography shine madadin zaɓi ban da yanayin al'ada na al'ada ko jujjuya lokaci chromatography don rabuwa da tsarkakewar waɗannan mahadi na acidic.A cikin chromatography mai walƙiya, kafofin watsa labarun da aka saba amfani da su don musayar ion shine silica gel matrix inda ƙungiyoyin musayar ion ke da alaƙa da saman sa.Hanyoyin musayar ion da aka fi amfani da su a cikin chromatography na walƙiya sune SCX (yawanci rukunin sulfonic acid) da SAX (yawanci rukunin aminin quaternary).A cikin bayanin kula da aikace-aikacen da aka buga a baya tare da taken "Aikace-aikacen SepaFlash Strong Cation Musanya ginshiƙan Chromatography a cikin Tsabtace Haɗin Alkaline" ta Santai Technologies, ginshiƙan SCX an yi amfani da su don tsarkake mahaɗan alkaline.A cikin wannan sakon, an yi amfani da cakuda tsaka-tsakin tsaka-tsaki da acidic a matsayin samfurin don bincika aikace-aikacen ginshiƙan SAX a cikin tsarkakewar mahaɗan acidic.
Sashen Gwaji
Hoto 1. Zane-zane na tsarin lokaci na tsaye wanda aka danganta da saman kafofin watsa labarai na SAX.
A cikin wannan sakon, an yi amfani da ginshiƙin SAX wanda aka riga aka cika shi tare da silica na amine na quaternary (kamar yadda aka nuna a hoto 1).An yi amfani da cakuda Chromone da 2,4-dihydroxybenzoic acid azaman samfurin da za a tsarkake (kamar yadda aka nuna a cikin Hoto 2).An narkar da cakuda a cikin methanol kuma an ɗora shi a kan harsashi mai walƙiya ta wani injector.An jera saitin gwajin filasha a cikin Tebur 1.
Hoto 2. Tsarin sinadarai na sassan biyu a cikin cakuda samfurin.
| Kayan aiki | SepaBean™ inji T | |||||
| Harsashi | 4 g SepaFlash Standard Series flash cartridge (silica mara daidaituwa, 40 - 63 μm, 60 Å, Lambar oda: S-5101-0004) | 4 g SepaFlash Bonded Series SAX flash cartridge (silica mara daidaituwa, 40 - 63 μm, 60 Å, Lambar oda: SW-5001-004-IR) | ||||
| Tsawon tsayi | 254 nm (gane), 280 nm (sa idanu) | |||||
| Zaman wayar hannu | Magani A: N-hexane | |||||
| Maganin B: Ethyl acetate | ||||||
| Yawan kwarara | 30 ml/min | 20 ml/min | ||||
| Samfurin lodi | 20 MG (cakude na Bangaren A da Bangaren B) | |||||
| Gradient | Lokaci (CV) | Mai narkewa B (%) | Lokaci (CV) | Mai narkewa B (%) | ||
| 0 | 0 | 0 | 0 | |||
| 1.7 | 12 | 14 | 100 | |||
| 3.7 | 12 | / | / | |||
| 16 | 100 | / | / | |||
| 18 | 100 | / | / | |||
Sakamako da Tattaunawa
Da fari dai, an raba cakuda samfurin ta kwandon walƙiya na al'ada wanda aka riga aka cika shi da silica na yau da kullun.Kamar yadda aka nuna a cikin hoto na 3, an cire abubuwa biyu a cikin samfurin daga harsashi ɗaya bayan ɗaya.Bayan haka, an yi amfani da harsashin filasha na SAX don tsaftace samfurin.Kamar yadda aka nuna a cikin Hoto na 4, Bangaren acid na B ya kasance gabaɗaya akan harsashin SAX.Bangaren tsaka-tsakin A ya kasance a hankali ya kuɓuce daga harsashi tare da haɓakar lokacin wayar hannu.
Hoto 3. Hasken chromatogram na samfurin akan harsashin lokaci na yau da kullun.
Hoto 4. Hasken chromatogram na samfurin akan harsashin SAX.
Kwatanta Hoto na 3 da Hoto na 4, Bangaren A yana da siffar kololuwa mara daidaituwa akan harsashi daban-daban guda biyu.Don tabbatar da ko kololuwar ƙoƙon ya yi daidai da ɓangaren, za mu iya amfani da cikakken yanayin sikanin tsayi wanda aka gina a cikin software mai sarrafa na'urar SepaBean™.Bude bayanan gwaji na rabuwa biyu, ja zuwa layin nuna alama akan axis lokaci (CV) a cikin chromatogram zuwa mafi girman matsayi da matsayi na biyu mafi girma na ƙoƙon elution wanda ya dace da Bangaren A, da cikakken bakan na waɗannan biyun. Za a nuna maki kai tsaye a ƙasan chromatogram (kamar yadda aka nuna a hoto na 5 da hoto 6).Kwatanta cikakken bayanan bakan raƙuman ruwa na waɗannan rarrabuwar kawuna biyu, Bangaren A yana da daidaitaccen bakan sha a cikin gwaje-gwaje biyu.Saboda Bangaren A yana da siffar kololuwa mara daidaituwa akan harsashin filasha daban-daban guda biyu, ana hasashe cewa akwai ƙayyadaddun ƙazanta a cikin Bangaren A wanda ke da riƙe daban-daban akan harsashin lokaci na al'ada da harsashin SAX.Don haka, jerin abubuwan da ke fitowa sun bambanta ga Bangaren A da ƙazanta a kan waɗannan harsashi masu walƙiya guda biyu, wanda ya haifar da rashin daidaiton siffar kololuwa akan chromatograms.
Hoto 5. Cikakken bakan bakan na Bangaren A da ƙazanta da ke raba ta da harsashi na al'ada.
Hoto 6. Cikakken nau'in bakan na Bangaren A da ƙazantar da SAX harsashi ya raba.
Idan samfurin da aka yi niyya da za a tattara shine sashin tsaka tsaki na A, ana iya kammala aikin tsarkakewa cikin sauƙi ta amfani da harsashin SAX kai tsaye don haɓakawa bayan ɗaukar samfurin.A gefe guda, idan samfurin da aka yi niyya da za a tattara shine sashin acidic B, hanyar sake kamawa za a iya ɗauka tare da ɗan daidaitawa kawai a cikin matakan gwaji: lokacin da aka ɗora samfurin akan harsashin SAX da sashin tsaka tsaki A. An cire gaba ɗaya tare da abubuwan kaushi na zamani na yau da kullun, canza yanayin wayar zuwa maganin methanol mai ɗauke da 5% acetic acid.Acetate ions a cikin tsarin wayar hannu za su yi gasa tare da Bangaren B don ɗaure ga ƙungiyoyin amine ion na quaternary akan lokaci na harsashi na SAX, ta haka ne ke fitar da Bangaren B daga harsashi don samun samfurin da aka yi niyya.An nuna chromatogram na samfurin da aka rabu a yanayin musayar ion a cikin hoto 7.
Hoto 7. Fish chromatogram na Bangaren B ya ɓullo a yanayin musayar ion akan harsashin SAX.
A ƙarshe, samfurin acidic ko tsaka tsaki na iya zama cikin sauri ta hanyar SAX harsashi tare da harsashi na al'ada ta amfani da dabarun tsarkakewa daban-daban.Bugu da ƙari, tare da taimakon cikakken fasalin sikanin raƙuman raƙuman ruwa da aka gina a cikin software mai sarrafa na'ura na SepaBean ™, za'a iya kwatanta nau'in nau'in nau'in nau'in nau'i na ɓangarorin da ba a iya kwatanta su cikin sauƙi da kuma tabbatar da su, yana taimakawa masu bincike da sauri su ƙayyade abun da ke ciki da tsabta na ɓangarorin da aka lalata don haka ingantawa. ingancin aiki.
| Lambar Abu | Girman Rukunin | Yawan kwarara (ml/min) | Max.Matsi (psi/bar) |
| Saukewa: SW-5001-004-IR | 5.9g ku | 10-20 | 400/27.5 |
| Saukewa: SW-5001-012-IR | 23 g ku | 15-30 | 400/27.5 |
| Saukewa: SW-5001-025-IR | 38g ku | 15-30 | 400/27.5 |
| Saukewa: SW-5001-040-IR | 55g ku | 20-40 | 400/27.5 |
| Saukewa: SW-5001-080 | 122 g | 30-60 | 350/24.0 |
| Saukewa: SW-5001-120 | 180 g | 40-80 | 300/20.7 |
| Saukewa: SW-5001-220 | 340 g | 50-100 | 300/20.7 |
| Saukewa: SW-5001-330 | 475g ku | 50-100 | 250/17.2
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Tebur 2. SepaFlash Bonded Series SAX harsashi filasha.Kayan tattarawa: Silica mai haɗaɗɗen SAX mara ƙarfi mai tsafta, 40 - 63 μm, 60 Å.
Don ƙarin bayani kan cikakkun bayanai na SepaBean™inji, ko bayanin oda akan sepaFlash jerin harsashi flash, da fatan za a ziyarci gidan yanar gizon mu.
Lokacin aikawa: Nov-09-2018