Gabanya urusaku rw'ibanze rwa HPLC/UHPLC System kandi wongere ubushobozi bwo kumva ukoresheje 3D Printed Static Mixer nshya ikora neza cyane – 6 Gashyantare 2017 – James C. Steele, Christopher J. Martineau, Kenneth L. Rubow – Ingingo mu makuru y'ibinyabuzima

Hakozwe imvange nshya ihindura imiterere y’amazi ihindagurika (inline static mixer) yagenewe by’umwihariko kuzuza ibisabwa bikomeye bya sisitemu ya chromatography y’amazi ifite imikorere myiza (HPLC) na ultra high performance liquid chromatography (HPLC na UHPLC). Kuvanga nabi ibice bibiri cyangwa byinshi bishobora gutuma habaho ikigereranyo cyo hejuru cy’urusaku hagati y’ibimenyetso, bigabanya ubushobozi bwo kumva. Kuvanga neza amazi abiri cyangwa menshi afite ingano nto y’imbere n’ibipimo by’umubiri by’imvange ihindagurika ni byo bipimo byiza by’imvange ihindagurika. Imvange nshya ihindagurika ibigeraho ikoresheje ikoranabuhanga rishya rya 3D ryo gucapa kugira ngo ikore imiterere yihariye ya 3D itanga uburyo bwiza bwo kuvanga amazi ahindagurika hamwe n’igabanuka ryinshi ry’umuraba wa sine y’ibanze kuri buri gice cy’umuraba w’imbere w’imvange. Gukoresha 1/3 cy’umuraba w’imbere w’imvange isanzwe bigabanya umuraba w’ibanze wa sine ku kigero cya 98%. Imvange igizwe n’imiyoboro ya 3D ihujwe ifite ahantu hatandukanye hanyura hamwe n’uburebure bw’inzira uko amazi anyura mu ngero zikomeye za 3D. Kuvanga inzira nyinshi zihindagurika, hamwe n’imihindagurikire y’aho hantu n’imizunguruko, bituma habaho kuvanga kuri micro, meso na macro scale. Iyi mvange idasanzwe yakozwe hakoreshejwe simulation za CFD. Amakuru y’igerageza yatanzwe agaragaza ko kuvanga neza bigerwaho habayeho ingano ntoya y’imbere.
Mu myaka irenga 30, chromatography y'amazi imaze gukoreshwa mu nganda nyinshi, harimo imiti, imiti yica udukoko, kurengera ibidukikije, ubugenzuzi bw'ibiza, no gusesengura imiti. Ubushobozi bwo gupima ibice kuri miliyoni cyangwa munsi yabyo ni ingenzi cyane ku iterambere ry'ikoranabuhanga mu nganda izo ari zo zose. Kuvanga neza bitera igipimo kibi cy'urusaku hagati y'ibimenyetso n'urusaku, ibi bikaba ari ikibazo ku muryango w'abahanga mu gupima chromatography mu bijyanye n'aho badashobora kubona no kumenya. Mu gihe uvanga solvents ebyiri za HPLC, rimwe na rimwe biba ngombwa guhatira kuvanga hakoreshejwe uburyo bwo hanze kugira ngo uhuze solvents ebyiri kuko solvents zimwe na zimwe zidahura neza. Iyo solvents zitavanze neza, chromatography ya HPLC ishobora kwangirika, ikagaragara nk'urusaku rwinshi rw'ibanze cyangwa imiterere mibi y'umutwe. Mu gihe uvanga nabi, urusaku rw'ibanze ruzagaragara nk'umuraba wa sine (uri kuzamuka no kumanuka) w'ikimenyetso cy'ibiza uko igihe kigenda gihita. Muri icyo gihe, kuvanga nabi bishobora gutuma peaks zaguka kandi zitangana, bikagabanya imikorere yo gusesengura, imiterere y'umutwe, n'uburyo bwo kumenya imiterere y'umutwe. Inganda zemeye ko mixers ziri ku murongo n'izidahinduka ari uburyo bwo kunoza izi mipaka no kwemerera abakoresha kugera ku ngero nke zo kumenya (sensitivities). Imvange nziza ihuza ibyiza byo kuvanga neza, ingano ntoya y’amazi n’umuvuduko muke hamwe n’ingano ntoya n’umuvuduko ntarengwa w’imikorere ya sisitemu. Byongeye kandi, uko isesengura rigenda rirushaho kugorana, abasesenguzi bagomba gukoresha buri gihe imiti ivangavanga cyane kandi igoye kuvanga. Ibi bivuze ko kuvanga neza ari ngombwa mu igerageza ry’ejo hazaza, bikongera gukenerwa imiterere n’imikorere myiza y’imvange.
Mott iherutse gukora ubwoko bushya bw'imashini zivangavanga za PerfectPeakTM zifite patenti zifite ingano eshatu z'imbere: 30 µl, 60 µl na 90 µl. Izi ngano zikubiyemo ingano n'imiterere y'imvange ikenewe mu bizamini byinshi bya HPLC aho hakenewe uburyo bwo kuvanga neza no gukwirakwiza buhoro. Izo moderi zose uko ari eshatu zifite umurambararo wa 0.5″ kandi zitanga umusaruro ukomeye mu nganda mu gishushanyo gito. Zikozwe mu cyuma cya 316L kitarangwamo ingese, ntizishobora gucika, ariko na titaniyumu n'ibindi byuma birwanya ingese kandi bitagira imiti birahari. Izi mashini zivanga zifite umuvuduko ntarengwa wo gukora ungana na psi 20.000. Ku ishusho ya 1a hari ifoto y'imashini ivangavanga ya Mott ya 60 µl yagenewe gutanga umusaruro mwiza wo kuvanga mu gihe ikoresha ingano nto y'imbere ugereranije n'imashini zivangavanga zisanzwe z'ubu bwoko. Iyi shusho nshya y'imashini ivangavanga ikoresha ikoranabuhanga rishya ryo gukora inyongera kugira ngo habeho imiterere yihariye ya 3D ikoresha umuvuduko muto w'imbere ugereranije n'indi mashini ivangavanga ikoreshwa mu nganda za chromatography kugira ngo igere ku kuvanga guhindagurika. Bene ibyo bivange bigizwe n'imiyoboro y'amazi ifite imiterere itatu ihujwe hamwe n'ahantu hatandukanye hamwe n'uburebure butandukanye bw'inzira uko amazi yambukiranya imipaka ikomeye y'ubuso bw'amazi imbere. Ku ishusho. Ishusho ya 1b igaragaza igishushanyo mbonera cy'imvange nshya, ikoresha ibikoresho bisanzwe by'inganda bya HPLC 10-32 byo gushyiramo imigozi yo kwinjira no gusohoka, kandi ifite imbibi z'ubururu bw'icyambu cy'imbere cy'imvange gifite patenti. Ahantu hatandukanye h'imiyoboro y'amazi imbere n'impinduka mu cyerekezo cy'amazi mu bunini bw'amazi imbere birema uturere tw'amazi ahindagurika kandi ahindagurika, bigatuma habaho kuvanga ku bipimo bito, bya meso na macro. Igishushanyo cy'iyi mvange yihariye cyakoresheje simulations za fluid dynamics (CFD) kugira ngo basesengure imiterere y'amazi no kunoza igishushanyo mbere yo gukora isuzuma ry'isesengura ry'imbere no gusuzuma abakiriya. Inyongera ni inzira yo gucapa ibice bya geometrike bya 3D bivuye mu bishushanyo bya CAD hatabayeho gukoresha imashini gakondo (imashini zisya, imashini zisya, nibindi). Izi mvange nshya zihoraho zagenewe gukorwa hakoreshejwe ubu buryo, aho umubiri w'imvange ukorwa uhereye ku bishushanyo bya CAD kandi ibice bigakorwa (byacapwe) urwego ku rundi hakoreshejwe imvange. Aha, hashyirwa urwego rw'ifu y'icyuma rufite ubugari bwa mikoroni 20, maze laser igenzurwa na mudasobwa ishonga neza ikayivanga mu buryo bukomeye. Shyira urundi rwego hejuru y'uru rwego hanyuma ushyireho laser sintering. Subiramo iki gikorwa kugeza igihe igice kirangiye neza. Hanyuma ifu ikurwa mu gice kitari gifite laser, hagasigara igice cyacapwe cya 3D gihuye n'igishushanyo cya CAD cya mbere. Umusaruro wa nyuma usa gato n'inzira ya microfluidic, itandukaniro rikomeye rikaba ari uko ibice bya microfluidic akenshi biba bifite imiterere ibiri (birambuye), mu gihe hakoreshejwe uburyo bwo kongeramo, imiterere y'urujya n'uruza irashobora gukorwa mu buryo bw'imiterere itatu. Izi robine ubu ziboneka nk'ibice byacapwe bya 3D mu cyuma kitagira umugese cya 316L na titaniyumu. Ibyuma byinshi, polimeri na bimwe mu byuma bishobora gukoreshwa mu gukora ibice hakoreshejwe ubu buryo kandi bizatekerezwaho mu bishushanyo/ibicuruzwa bizaza.
Umuceri. 1. Ifoto (a) n'igishushanyo (b) cy'icyuma gifunganye cya 90 μl Mott kigaragaza igice cy'inzira y'amazi yo gufunga gifite ibara ry'ubururu.
Koresha isuzuma ry’imikorere y’amazi ahindagurika (CFD) mu gihe cy’igishushanyo kugira ngo ufashe guteza imbere imiterere myiza no kugabanya igerageza ritwara igihe kinini kandi rihenze ryo kugerageza no gukora amakosa. Isuzuma rya CFD ry’imvange zihoraho n’imiyoboro isanzwe (simulation idahindagurika) ukoresheje porogaramu ya COMSOL Multiphysics. Gushushanya hakoreshejwe uburyo bwa laminar fluid bukoreshwa n’umuvuduko kugira ngo wumve umuvuduko w’amazi n’umuvuduko mu gice runaka. Ubu buryo bwa fluid, hamwe n’ubwikorezi bw’ibinyabutabire by’ibinyabutabire, bifasha gusobanukirwa ivanga ry’amazi abiri atandukanye. Icyitegererezo cyigwa nk’igihe, kingana n’amasegonda 10, kugira ngo byorohe kubara mu gihe hashakishwa ibisubizo bisa. Amakuru y’inyigo yabonetse mu nyigo ijyanye n’igihe hakoreshejwe igikoresho cyo gupima ingingo, aho agace kari hagati mu gusohoka katoranyijwe mu gukusanya amakuru. Icyitegererezo cya CFD n’ibizamini by’igerageza byakoresheje imvange ebyiri zitandukanye binyuze mu ivali y’isuzuma ingana na sisitemu yo gupima, bigatuma habaho ifunga risimbura buri mvange mu murongo w’isuzuma. Hanyuma iyi mvange ivangwa mu imvange ihoraho. Ishusho ya 2 na 3 zigaragaza igereranya ry’amazi binyuze mu muyoboro usanzwe (udakoresha imvange) no binyuze mu imvange ya Mott ihoraho, uko bikurikirana. Igereranya ryakozwe ku muyoboro ugororotse ufite uburebure bwa cm 5 na 0.25 mm ID kugira ngo ryerekane igitekerezo cyo guhinduranya amazi na acetonitrile mu muyoboro mu gihe nta mvange ihoraho irimo, nk'uko bigaragara ku Ishusho ya 2. Igereranya ryakoresheje ingano nyayo y’umuyoboro n’imvange ndetse n’umuvuduko w’amazi wa 0 .3 ml/min.
Umuceri. 2. Gushushanya urujya n'uruza rwa CFD mu muyoboro wa cm 5 ufite umurambararo w'imbere wa mm 0.25 kugira ngo ugaragaze ibibera mu muyoboro wa HPLC, ni ukuvuga iyo nta mashini ivanga. Umutuku wuzuye ugaragaza igice kinini cy'amazi. Ubururu bugaragaza ibura ry'amazi, ni ukuvuga acetonitrile y'umwimerere. Uduce dukwirakwira dushobora kugaragara hagati y'udupfundikizo tw'amazi abiri atandukanye.
Umuceri. 3. Imvange ihoraho ifite ingano ya mililitiro 30, yashushanyije muri porogaramu ya COMSOL CFD. Iyi nkuru igaragaza igice kinini cy'amazi mu mvange. Amazi meza agaragara mu ibara ry'umutuku n'ay'ubururu bw'acetonitrile. Impinduka mu gice kinini cy'amazi yashushanyijwe igaragazwa n'impinduka mu ibara ry'imvange y'amazi abiri.
Ku ishusho ya 4 hagaragazwa inyigo yo kwemeza isano iri hagati y’imikorere myiza yo kuvanga n’ubwinshi bw’ibivange. Uko ingano yo kuvanga yiyongera, imikorere myiza yo kuvanga iragenda yiyongera. Nk’uko abanditsi babizi, izindi mbaraga zikomeye zikora mu mvange ntizishobora kubarwa muri ubu buryo bwa CFD, bigatuma habaho imikorere myiza yo kuvanga mu bizamini by’igerageza. Umurimo wo kuvanga mu mvange wapimwe nk’igabanuka ry’ijanisha rya sinusoid y’ibanze. Byongeye kandi, kwiyongera k’umuvuduko w’umugongo akenshi bitera urwego rwo hejuru rwo kuvanga, rutafatwa nk’aho ruri mu buryo bwo kwigana.
Imiterere ya HPLC ikurikira hamwe n'uburyo bwo gupima byakoreshejwe mu gupima imiraba ya sine isanzwe kugira ngo hagereranywe imikorere y'imvange zitandukanye zihoraho. Ishusho iri ku Ishusho ya 5 igaragaza imiterere isanzwe ya sisitemu ya HPLC / UHPLC. Imvange ihoraho yageragejwe hashyirwa imvange nyuma ya pompe mbere y'inkingi ikoresha injector na separation. Ibipimo byinshi bya sinusoidal inyuma bikorwa hirengagijwe inkingi ikoresha injector na capillary hagati y'imvange ikoresha injector na UV detector. Mu gusuzuma ikigereranyo cy'ibimenyetso hagati y'urusaku cyangwa gusesengura imiterere y'umutwe, imiterere ya sisitemu igaragazwa ku Ishusho ya 5.
Ishusho ya 4. Ishusho yerekana uburyo bwo kuvanga neza ugereranije n'ingano y'ingano y'imvange ku mvange zitandukanye. Ubusembwa bw'ibitekerezo bukurikiza umurongo umwe n'amakuru y'ubusembwa bw'igerageza yemeza ko simulation za CFD ari ingirakamaro.
Sisitemu ya HPLC yakoreshejwe muri iki kizamini ni Agilent 1100 Series HPLC ifite icyuma gipima UV kigenzurwa na mudasobwa ikoresha porogaramu ya Chemstation. Imbonerahamwe ya 1 igaragaza imiterere isanzwe yo gupima ubushobozi bwo kuvanga hakoreshejwe kugenzura sinusoids z'ibanze mu bushakashatsi bubiri. Ibizamini by'igerageza byakozwe ku ngero ebyiri zitandukanye z'ibintu bisukura. Ibintu bibiri bisukura byavanzwe mu rubanza rwa 1 byari solvent A (20 mM ammonium acetate mu mazi yakuwemo ayoni) na solvent B (80% acetonitrile (ACN) / 20% amazi yakuwemo ayoni). Mu rubanza rwa 2, solvent A yari igisubizo cya 0.05% acetone (ikimenyetso) mu mazi yakuwemo ayoni. solvent B ni uruvange rwa 80/20% methanol n'amazi. Mu rubanza rwa 1, pompe yashyizwe ku gipimo cy'amazi kiri hagati ya 0.25 ml / min na 1.0 ml / min, naho mu rubanza rwa 2, pompe yashyizwe ku gipimo cy'amazi gihoraho cya 1 ml / min. Muri ibyo byiciro byombi, igipimo cy'uruvange rw'ibintu bishongesha A na B cyari 20% A/80% B. Igipimo cy'amashanyarazi cyashyizwe kuri 220 nm mu rubanza rwa 1, naho ubushobozi ntarengwa bwo kwinjiza acetone mu rubanza rwa 2 bwashyizwe ku rugero rwa 265 nm.
Imbonerahamwe ya 1. Imiterere ya HPLC ku nshuro ya 1 na 2 Inshuro ya 1 Inshuro ya 2 Umuvuduko wa Pompe 0.25 ml/umunota kugeza kuri 1.0 ml/umunota 1.0 ml/umunota Isosi A 20 mM ammonium acetate mu mazi yakuwemo ioni 0.05% Asetone mu mazi yakuwemo ioni Isosi B 80% Asetonitrile (ACN) / 20% amazi yakuwemo ioni 80% methanol / 20% amazi yakuwemo ioni Igipimo cya 20% A / 80% B 20% A / 80% B Isosi 220 nm 265 nm
Umuceri. 6. Ibishushanyo by'imiraba ivanze yapimwe mbere na nyuma yo gukoresha akayunguruzo ko hasi kugira ngo ukureho ibice by'ibanze by'ikimenyetso.
Ishusho ya 6 ni urugero rusanzwe rw'urusaku rw'ibanze ruvanze mu rubanza rwa 1, rugaragazwa nk'icyitegererezo gisubiramo cy'urusaku rw'amazi rushyirwa hejuru y'urusaku rw'ibanze. Uguhindagurika kw'ibanze ni ukwiyongera cyangwa kugabanuka buhoro buhoro kw'ikimenyetso cy'inyuma. Iyo sisitemu itemerewe kuringaniza igihe gihagije, akenshi iragwa, ariko izagenda ihindagurika mu buryo butunguranye nubwo sisitemu ihamye rwose. Uku kunyura kw'ibanze gukunze kwiyongera iyo sisitemu ikora mu buryo bukabije cyangwa mu miterere y'umuvuduko mwinshi w'umugongo. Iyo uku kunyura kw'ibanze kuhari, bishobora kugorana kugereranya ibisubizo bivuye ku rugero rumwe n'urundi, bishobora gukemurwa hakoreshejwe akayunguruzo k'amazi gaciriritse ku makuru asanzwe kugira ngo hamenyekane izi mpinduka z'umuvuduko muto, bityo bigatanga ishusho y'ihindagurika rifite umurongo ugororotse. Ku ishusho ya 6 kandi herekana ishusho y'urusaku rw'amazi nyuma yo gukoresha akayunguruzo k'amazi gaciriritse.
Nyuma yo kurangiza igerageza rya CFD no kugerageza igerageza rya mbere, hakozwe imvange eshatu zitandukanye zihoraho hakoreshejwe ibice by'imbere byavuzwe haruguru hamwe n'ingano eshatu z'imbere: 30 µl, 60 µl na 90 µl. Uru rwego rukubiyemo ingano y'ingano n'imikorere yo kuvanga ikenewe kugira ngo HPLC ikoreshwe mu buryo buke aho kuvanga neza no gutatanya bike bikenewe kugira ngo habeho imiterere y'ubugari buke. Ku ishusho ya 7 hagaragazwa ibipimo by'ibanze bya sine wave byabonetse kuri sisitemu y'igerageza ry'Urugero rwa 1 (acetonitrile na ammonium acetate nk'ibipimo bya tracers) hamwe n'ingano eshatu z'imvange zihoraho kandi nta mvange zashyizweho. Imiterere y'igerageza ry'ibisubizo byagaragajwe ku Ishusho ya 7 yagumyeho mu bizamini byose 4 hakurikijwe uburyo bwavuzwe mu mbonerahamwe ya 1 ku gipimo cy'umuvuduko wa solvent cya 0.5 ml / min. Shyira agaciro k'umuvuduko ku makuru kugira ngo ashobore kwerekwa iruhande nta guhurirana kw'ibimenyetso. Guhagarika ntibigira ingaruka ku bugari bw'ikimenyetso cyakoreshejwe mu gupima urwego rw'imikorere y'imvange. Ubwinshi bw'ubugari bwa sinusoidal butarimo imvange bwari 0.221 mAi, mu gihe ubugari bw'imvange za Mott zitajegajega kuri 30 µl, 60 µl, na 90 µl bwagabanutse bugera kuri 0.077, 0.017, na 0.004 mAi, uko bikurikirana.
Ishusho ya 7. HPLC UV Detector Signal Offset vs. Time for Case 1 (acetonitrile ifite ammonium acetate indicator) igaragaza solvent vange idafite mixer, 30 µl, 60 µl na 90 µl Mott mixers igaragaza quanding nziza (signal amplitude iri hasi) uko ingano y'imvange ihindagurika yiyongera. (quandition nyayo y'amakuru: 0.13 (nta mixer ihari), 0.32, 0.4, 0.45mA kugira ngo hagaragazwe neza).
Amakuru agaragara ku ishusho ya 8 ni amwe n’agaragara ku ishusho ya 7, ariko kuri iyi nshuro arimo ibyavuye mu mvange eshatu zisanzwe zikoreshwa za HPLC zifite ingano y’imbere ya 50 µl, 150 µl na 250 µl. Umuceri. Ishusho ya 8. HPLC UV Detector Signal Offset ugereranyije n’igihe cyagenwe ku rubanza rwa 1 (Acetonitrile na Ammonium Acetate nk'ibimenyetso) bigaragaza ivangwa ry’umusemburo udafite mvange uhoraho, uruhererekane rushya rwa Mott static mixers, n’izindi mvange eshatu zisanzwe (ivangwa ry’amakuru nyayo ni 0.1 (nta mvange), 0.32, 0.48, 0.6, 0.7, 0.8, 0.9 mA kugira ngo hagaragazwe neza). Igabanuka ry’umusemburo w’ibanze rya sine ribarwa hakurikijwe igipimo cy’umusemburo w’umusemburo wa sine ugera ku musemburo udafite mvange ushyizweho. Ijanisha ryapimwe ry’igabanuka ry’umuraba wa sine ku mashami ya 1 na 2 riri ku rutonde rwa 2, hamwe n’ingano y’imbere y’umuraba mushya uhuza ibintu bishya n’imitako irindwi isanzwe ikoreshwa mu nganda. Amakuru ari ku Ishusho ya 8 na 9, ndetse n’imibare yagaragajwe mu Imbonerahamwe ya 2, agaragaza ko Mott Static Mixer ishobora gutanga igabanuka rya sine wave rigera kuri 98.1%, rirenze cyane imikorere y’umutako usanzwe wa HPLC muri ibi bihe by’igeragezwa. Ishusho ya 9. HPLC UV detector signal offset ugereranyije n’igihe cyagenwe ku mashami ya 2 (methanol na acetone nk’ibipimo) bitagaragaza ihinduka ry’umuraba (bivanze), urukurikirane rushya rw’imitako ihuza ibintu bishya bya Mott na mitako ibiri isanzwe (ihinduka ry’amakuru nyayo ni 0, 11 (idafite imitako), 0.22, 0.3, 0.35 mA no kwerekana neza). Imitako irindwi ikoreshwa mu nganda nayo yarasuzumwe. Ibi birimo imvange zifite ingano eshatu zitandukanye z’imbere muri sosiyete A (imvange yagenwe A1, A2 na A3) na sosiyete B (imvange yagenwe B1, B2 na B3). Isosiyete C yatanze amanota ku ngano imwe gusa.
Imbonerahamwe ya 2. Ibiranga imvange ihoraho n'ingano y'imbere imvange ihoraho 1 Imvange ihoraho: Ikizamini cya Acetonitrile (Ingano) Icyiciro cya 2 Imvange ihoraho: Ikizamini cy'amazi ya Methanol (Ingano) Ingano y'imbere (µl) Nta mvange – - 0 Mott 30 65% 67.2% 30 Mott 60 92.2% 91.3% 60 Mott 90 98.1% 97.5% 90 Imvange A1 66.4% 73.7% 50 Imvange A2 89.8% 91.6% 150 Imvange A3 92.2% 94.5% 250 Imvange B1 44.8% 45.7% 9 35 Imvange B2 845.% 96.2% 370 Imvange C 97.2% 97.4% 250
Isesengura ry'ibyavuye mu Ishusho ya 8 n'Imbonerahamwe ya 2 rigaragaza ko imvange ya 30 µl Mott ifite ubushobozi bwo kuvanga nk'ubw'imvange ya A1, ni ukuvuga 50 µl, icyakora, imvange ya 30 µl ifite ingano ntoya y'imbere ku kigero cya 30%. Mu kugereranya imvange ya 60 µl Mott n'imvange ya 150 µl A2, habayeho iterambere rito mu bushobozi bwo kuvanga bwa 92% ugereranyije na 89%, ariko ikiruta byose, uru rwego rwo hejuru rwo kuvanga rwagezweho kuri 1/3 cy'ingano y'imvange. Imvange ya 90 µl Mott yakurikije umurongo umwe n'imvange ya A3 ifite ingano y'imbere ya 250 µl. Iterambere mu bushobozi bwo kuvanga rya 98% na 92% naryo ryagaragaye hamwe no kugabanuka inshuro 3 k'ingano y'imbere. Ibisubizo n'igereranya nk'ibyo byabonetse ku mvange B na C. Kubera iyo mpamvu, uruhererekane rushya rw'imvange zitajegajega Mott PerfectPeakTM itanga ubushobozi bwo kuvanga kurusha imvange zisanzwe, ariko hamwe n'ubwinshi bw'imbere, itanga urusaku rwiza rw'inyuma n'igipimo cyiza cy'ikimenyetso hagati y'urusaku, Analyte nziza yo kumva, imiterere y'impeshyi n'ubushobozi bwo hejuru. Ingendo nk'izo mu bushobozi bwo kuvanga zagaragaye mu bushakashatsi bwa C1 na C2. Ku kibazo cya 2, ibizamini byakozwe hakoreshejwe (methanol na acetone nk'ibipimo) kugira ngo hagereranywe ubushobozi bwo kuvanga bwa mililitiro 60 za Mott, imvange A1 ingana (ingano y'imbere 50 µl) n'imvange B1 ingana (ingano y'imbere 35 µl). , imikorere yari mibi nta mvange yashyizweho, ariko yakoreshejwe mu isesengura ry'ibanze. Imvange ya Mott ya mililitiro 60 yagaragaye ko ari yo mvange nziza mu itsinda ry'igerageza, itanga ubwinshi bwa 90% mu bushobozi bwo kuvanga. Imvange A1 ingana yabonye iterambere rya 75% mu bushobozi bwo kuvanga rikurikirwa n'izamuka rya 45% mu mvange B1 ingana. Ikizamini cy’ibanze cyo kugabanya umuraba wa sine hamwe n’umuvuduko w’amazi cyakozwe ku mashini zivangavanze mu buryo bumwe n’ikizamini cya sine curve mu rubanza rwa 1, aho umuvuduko w’amazi wahindutse gusa. Amakuru yagaragaje ko mu rugero rw’umuvuduko w’amazi kuva kuri 0.25 kugeza kuri 1 ml/umunota, kugabanuka kwa mbere k’umuraba wa sine kwakomeje kuba ntagereranywa kuri buri ngano eshatu z’imashini zivangavanze. Ku mashini ebyiri nto zivangavanze ingano, hari ukwiyongera gato k’umuvuduko wa sinusoidal uko umuvuduko w’amazi ugabanuka, ibi bikaba byitezwe bitewe n’igihe cyo kuba cyiyongereye cy’umuvuduko mu mashini zivangavanze, bigatuma habaho kwiyongera k’umuvuduko w’amazi. Biteganijwe ko gukuramo umuraba wa sine biziyongera uko umuvuduko w’amazi ugabanuka kurushaho. Ariko, ku ngano nini y’imashini zivangavanze ifite umuvuduko mwinshi w’umuraba wa sine, umuvuduko w’umuraba wa sine wakomeje kugabanuka cyane (muri urwo rugero rw’igerageza rutari rwumvikana), aho agaciro kari hagati ya 95% na 98%. Umuceri. 10. Kugabanya umuvuduko w'amazi ugereranyije n'umuvuduko w'amazi mu gihe cya 1. Ikizamini cyakozwe mu bihe bisa n'ikizamini cya sine gifite umuvuduko uhindagurika w'amazi, hashyirwamo 80% by'uruvange rwa 80/20 rwa acetonitrile n'amazi na 20% bya acetate ya ammonium ya 20 mM.
Ubwoko bushya bwa PerfectPeakTM inline static mixers bufite patente hamwe n'ingano eshatu z'imbere: 30 µl, 60 µl na 90 µl bukubiyemo ingano n'imikorere yo kuvanga ikenewe mu isesengura rya HPLC risaba kunoza imvange n'ubuso buke bwo gutatanya. Iyi mvange nshya ihoraho ibigeraho ikoresheje ikoranabuhanga rishya rya 3D kugira ngo ikore imiterere yihariye ya 3D itanga uburyo bwiza bwo kuvanga static hydrodynamic hamwe n'igabanuka ryinshi ry'urusaku rw'ibanze kuri buri gice cy'ingano y'imvange y'imbere. Gukoresha 1/3 cy'ingano y'imbere y'iyi mvange isanzwe bigabanya urusaku rw'ibanze ho 98%. Izi mvange zigizwe n'imiyoboro y'amazi ifite imiterere itatu ihujwe hamwe n'ahantu hatandukanye hamwe n'uburebure butandukanye bw'inzira uko amazi yambukiranya inzitizi zikomeye z'imiterere y'imbere. Umuryango mushya w'imvange zihoraho utanga imikorere myiza ugereranije n'imvange zihanganye, ariko hamwe n'ingano nto y'imbere, bigatuma habaho ikigereranyo cyiza cy'urusaku hagati y'ibimenyetso n'ingano nke, ndetse no kunoza imiterere y'ubuhanga, imikorere myiza n'ubushobozi bwo kugaragaza ubushobozi bwo kumva ibintu neza.
Muri iki kinyamakuru, Chromatography – RP-HPLC irinda ibidukikije – Gukoresha chromatography y’ingufu kugira ngo isimbuze acetonitrile na isopropanol mu gusesengura no gutunganya – Chromatography nshya ya gaze kuri…
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Igihe cyo kohereza: Ugushyingo-15-2022