Nciphisa i-HPLC/UHPLC System Baseline Noise kunye noKwandisa ukuSensitivity kunye neNew High-Performance 3D Printed Static Mixer - ngoFebruwari 6, 2017 - uJames C. Steele, uChristopher J. Martineau, uKenneth L. Rubow - Inqaku kwiiSayensi zeBiological News

Umxube omtsha oguquguqukayo we-static we-inline uyilwe ngokukodwa ukuhlangabezana neemfuno ezingqongqo zolwelo lwechromatography (HPLC) kunye ne-ultra high performance liquid chromatography (HPLC kunye ne-UHPLC) iinkqubo.Ukuxuba okungalunganga kwezigaba ezimbini okanye ngaphezulu ezihambayo kunokubangela umlinganiselo ophezulu we-signal-to-noise, onciphisa uvakalelo.Ukuxutywa okulinganayo okumileyo kolwelo ezimbini okanye ngaphezulu ezinomthamo wangaphakathi ophantsi kunye nemilinganiselo yomzimba yomxube ongashukumiyo umele owona mgangatho uphezulu womxube ongashukumiyo ofanelekileyo.Umxubi omtsha we-static ufezekisa oku ngokusebenzisa iteknoloji entsha yoshicilelo lwe-3D ukwenza isakhiwo se-3D esisodwa esibonelela ngokuphuculwa kwe-hydrodynamic static mixing kunye nokunciphisa ipesenti ephezulu kwisiseko samaza e-sine kwiyunithi nganye umthamo wangaphakathi womxube.Ukusebenzisa i-1/3 yomthamo wangaphakathi womxube oqhelekileyo wehlisa i-sine wave nge-98%.Umxubi uqulathe imijelo ye-3D edityanisiweyo eneendawo ezahlukeneyo ezinqamlezayo kunye nobude bendlela njengoko ulwelo lunqumla kwiijometri ze-3D ezinzima.Ukuxuba kunye neendlela ezininzi zokuhamba ezibuhlungu, ezidityaniswe nesiphithiphithi sasekhaya kunye neeeddies, kubangela ukuxubana kwi-micro, meso kunye ne-macro scales.Lo mxubi ukhethekileyo uyilwe kusetyenziswa icomputational fluid dynamics (CFD) ukulinganisa.Idatha yovavanyo ebonakalisiweyo ibonisa ukuba ukuxuba okugqwesileyo kufezekiswa ngomthamo omncinci wangaphakathi.
Ngaphezu kweminyaka engama-30, i-chromatography yolwelo isetyenzisiwe kumashishini amaninzi, kubandakanya amayeza, amayeza okubulala izitshabalalisi, ukhuseleko lokusingqongileyo, i-forensics, kunye nohlalutyo lweekhemikhali.Ukukwazi ukulinganisa iinxalenye ngesigidi okanye ngaphantsi kubalulekile kuphuhliso lobuchwepheshe kulo naliphi na ishishini.Ukungasebenzi kakuhle kokuxubana kukhokelela kumlinganiselo ombi we-signal-to-noise, nto leyo ecaphukisayo kuluntu lwechromatography ngokwemida yokubona kunye novelwano.Xa uxuba izinyibilikisi ezimbini ze-HPLC, ngamanye amaxesha kuyimfuneko ukunyanzela ukuxuba ngeendlela zangaphandle ukwenza i-homogenize izinyibilikisi ezimbini kuba ezinye izinyibilikisi azixubeki kakuhle.Ukuba izinyibilikisi azixutywanga ngokugqibeleleyo, ukuthotywa kwechromatogram ye-HPLC kungenzeka, izibonakalise njengengxolo egqithisileyo yesiseko kunye/okanye ukumila kwencopho embi.Ngokuxutywa kakubi, ingxolo yesiseko iya kubonakala njenge-sine wave (enyukayo kwaye ehla) yesiginali ye-detector ngokuhamba kwexesha.Ngexesha elifanayo, ukuxuba okungahambi kakuhle kunokukhokelela ekwandiseni kunye neencopho ze-asymmetric, ukunciphisa ukusebenza kokuhlalutya, ukubunjwa okuphezulu, kunye nesisombululo esiphezulu.Ishishini liye laqaphela ukuba i-in-line kunye ne-tee static mixers ziyindlela yokuphucula le mida kunye nokuvumela abasebenzisi ukuba bafezekise imida ephantsi yokubona (ubuthathaka).Umxube we-static ofanelekileyo udibanisa inzuzo yokusebenza okuphezulu kokuxuba, umthamo ophantsi ofileyo kunye noxinzelelo oluphantsi loxinzelelo kunye nomthamo omncinci kunye nobuninzi benkqubo yokuphuma.Ukongezelela, njengoko uhlalutyo luba nzima ngakumbi, abahlalutyi kufuneka basebenzise rhoqo i-polar kunye ne-solvents enzima ukuxuba.Oku kuthetha ukuba ukuxubana okungcono kuyimfuneko kuvavanyo lwexesha elizayo, ukwandisa ngakumbi imfuno yoyilo lomxubi oluphezulu kunye nokusebenza.
I-Mott isanda kuvelisa uluhlu olutsha lwe-patent ye-PerfectPeak TM e-intanethi ye-static mixers enemithamo emithathu yangaphakathi: 30 µl, 60 µl kunye ne-90 µl.Ezi sayizi zigubungela uluhlu lwemithamo kunye neempawu zokuxuba ezifunekayo kwiimvavanyo ezininzi ze-HPLC apho ukuxuba okuphuculweyo kunye nokusabalalisa okuphantsi kuyadingeka.Zontathu iimodeli ziyi-0.5 ″ ububanzi kwaye zihambisa intsebenzo ekhokelayo kwishishini kuyilo olubambeneyo.Zenziwe nge-316L yensimbi engenasici, i-passivated ngenxa ye-inertness, kodwa i-titanium kunye nezinye i-corrosion resistant kunye nee-alloys zetsimbi ezingenazo iikhemikhali nazo ziyafumaneka.Aba baxubi banoxinzelelo oluphezulu lokusebenza ukuya kuthi ga kwi-20,000 psi.Kwikhiwane.I-1a yifoto yomxube we-60 µl we-Mott we-static eyilelwe ukubonelela ngobuchule obukhulu bokuxuba ngelixa usebenzisa umthamo omncinci wangaphakathi kunemixube eqhelekileyo yolu hlobo.Olu yilo lutsha lomxubi omileyo lusebenzisa itekhnoloji entsha yokwenziwa kokongeza ukwenza isakhelo esikhethekileyo se-3D esisebenzisa ukuhamba kancinci kwangaphakathi kunaso nawuphi na umxubi osetyenziswa ngoku kushishino lwechromatography ukuphumeza ukuxubana okumileyo.Abaxubeki abanjalo baquka imijelo edityanisiweyo enemigangatho emithathu eneendawo ezahlukeneyo ezinqamlezayo kunye nobude bendlela eyahlukileyo njengoko ulwelo luwela imiqobo yejometri entsonkothileyo ngaphakathi.Kwikhiwane.Umzobo we-1b ubonisa umzobo oqingqiweyo womxubi omtsha, osebenzisa umgangatho woshishino we-10-32 wofakelo loxinzelelo lwe-HPLC olufakwe kwindawo yokungena kunye nokuphuma, kwaye inemida enombala oluhlaza wezibuko lomxubi langaphakathi elinelungelo elilodwa lomenzi wechiza.Iindawo ezihlukeneyo ezinqamlezileyo zeendlela zokuhamba zangaphakathi kunye notshintsho kwindlela yokuhamba ngaphakathi komthamo wangaphakathi wokuhamba zenza imimandla ye-turbulent kunye ne-laminar flow, ebangela ukuxuba kwi-micro, meso kunye ne-macro scales.Uyilo lwalo mxubi ukhethekileyo lusetyenziselwe ukulinganisa ulwelo lwe-computational (CFD) ukuhlalutya iipateni zokuhamba kunye nokucokisa uyilo ngaphambi kovavanyo lohlalutyo lwangaphakathi kunye novavanyo lwentsimi yabathengi.Imveliso eyongeziweyo yinkqubo yokushicilela amacandelo ejometri ye-3D ngokuthe ngqo kwimizobo ye-CAD ngaphandle kwesidingo somatshini wendabuko (oomatshini bokugaya, i-lathes, njl.).Ezi mixube zitsha ze-static ziyilelwe ukuveliswa kusetyenziswa le nkqubo, apho umzimba womxube wenziwa ukusuka kwimizobo ye-CAD kwaye iinxalenye zenziwe (eziprintiweyo) umaleko zisebenzisa imveliso eyongezelelweyo.Apha, umaleko womgubo wesinyithi malunga nama-microns angama-20 ubukhulu ufakwa, kwaye i-laser elawulwa yikhompyuter inyibilika ngokukhetha kwaye ixube umgubo kwifomu eqinileyo.Faka enye umaleko phezu kolu luhlu kwaye usebenzise i-laser sintering.Phinda le nkqubo de inxalenye igqitywe ngokupheleleyo.Emva koko umgubo uyasuswa kwindawo engeyiyo i-laser eboshiweyo, ushiya inxalenye eprintiweyo ye-3D ehambelana nomzobo we-CAD wokuqala.Imveliso yokugqibela ifana nje nenkqubo ye-microfluidic, umahluko omkhulu kukuba i-microfluidic components zihlala zimbini-dimensional (flat), ngelixa kusetyenziswa ukuveliswa okongeziweyo, iipatheni zokuhamba ezintsonkothileyo zinokudalwa kwijometri ye-dimensional-dimensional.Ezi faucets zikhoyo ngoku njengeenxalenye eziprintiweyo ze-3D kwi-316L yentsimbi engatyiwayo kunye ne-titanium.Uninzi lweealloyi zetsimbi, iipolima kunye nezinye iiseramikhi zingasetyenziselwa ukwenza amacandelo kusetyenziswa le ndlela kwaye ziya kuqwalaselwa kuyilo / kwiimveliso ezizayo.
Irayisi.1. Ifoto (a) kunye nedayagram (b) ye-90 μl ye-Mott static mixer ebonisa icandelo elinqamlezayo lendlela yokuhamba yolwelo lomxubi ofakwe umbala oblowu.
Qhuba i-computational fluid dynamics (CFD) ukulinganisa ukusebenza komxubi omileyo ngexesha lesigaba soyilo ukunceda ukuphuhlisa uyilo olusebenzayo kunye nokunciphisa imifuniselo edla ixesha kunye neendleko zolingo kunye neempazamo.Ukulinganisa kwe-CFD ye-static mixers kunye nemibhobho eqhelekileyo (akukho-mixer simulation) usebenzisa iphakheji yesofthiwe ye-COMSOL Multiphysics.Ukwenza imodeli usebenzisa i-laminar fluid mechanics eqhutywa ngoxinzelelo ukuqonda isantya solwelo kunye noxinzelelo ngaphakathi kwenxalenye.Olu tshintsho lwe-fluid, ludityaniswe nokuthuthwa kweekhemikhali ze-mobile phase compounds, kunceda ukuqonda ukuxutywa kwezinto ezimbini ezahlukeneyo ezixubileyo.Imodeli ifundwa njengomsebenzi wexesha, elilingana nemizuzwana ye-10, ukuze kube lula ukubala ngelixa ukhangela izisombululo ezifaniswayo.Idatha yethiyori ifunyenwe kwisifundo esihambelana nexesha kusetyenziswa isixhobo sokubonisa inqaku, apho inqaku eliphakathi kokuphuma likhethwe ukuqokelelwa kwedatha.Imodeli ye-CFD kunye neemvavanyo zokuvavanya zisebenzise izinyibilikisi ezimbini ezahlukeneyo ngokusebenzisa ivalve yesampulu elinganayo kunye nenkqubo yokumpompa, okukhokelela kwiplagi yokutshintshwa kwi-solvent nganye kumgca wesampulu.Ezi zinyibilikisi ke zixutywa kumxube omileyo.Amanani 2 kunye ne-3 abonisa ukulinganisa ukuhamba ngombhobho oqhelekileyo (akukho mixer) kunye ne-Mott static mixer, ngokulandelanayo.Ukulinganisa kwakuqhutywe kwi-tube echanekileyo 5 cm ubude kunye ne-0.25 mm ye-ID ukubonisa ingcamango yokutshintshisa iiplagi zamanzi kunye ne-acetonitrile ecocekileyo kwi-tube ngokungabikho komxube we-static, njengoko kuboniswe kuMzobo 2. Ukulinganisa kusetyenziswe ubungakanani obuchanekileyo bombhobho kunye nomxube kunye nesantya sokuhamba kwe-0.3 ml / min.
Irayisi.2. Ukulinganisa ukuhamba kweCFD kwi-tube ye-5 cm kunye nobubanzi bangaphakathi be-0.25 mm ukumela okwenzekayo kwi-tube ye-HPLC, okt ngokungabikho komxube.Ubomvu obugcweleyo bumele ubukhulu beqhekeza lamanzi.Blue imele ukunqongophala kwamanzi, oko kukuthi iacetonitrile ecocekileyo.Imimandla yosasazo inokubonwa phakathi kweeplagi ezitshintshanayo zolwelo ezimbini ezahlukeneyo.
Irayisi.3. Umxube we-static kunye nomthamo we-30 ml, owenziwe kwiphakheji yesofthiwe ye-COMSOL CFD.Intsomi imele iqhekeza elikhulu lamanzi kumxube.Amanzi acocekileyo aboniswa kwi-acetonitrile ebomvu kunye necocekileyo eluhlaza okwesibhakabhaka.Utshintsho kwiqhekeza lobuninzi bamanzi afanisiweyo lumelwe ngotshintsho kumbala wokuxutywa kwee-liquids ezimbini.
Kwikhiwane.I-4 ibonisa isifundo sokuqinisekisa imodeli yokulungelelanisa phakathi kokusebenza kakuhle kokuxuba kunye nomthamo wokuxuba.Njengoko umthamo wokuxuba ukhula, ukudibanisa ukudibanisa kuya kwanda.Kulwazi lwababhali, amanye amandla omzimba antsonkothileyo asebenza ngaphakathi kumxubi akanakubalwa kule modeli yeCFD, ekhokelela ekusebenzeni okuphezulu kokuxuba kwiimvavanyo zovavanyo.Ukusebenza kokuxubana kovavanyo kulinganiswe njengepesenti yokunciphisa isiseko se-sinusoid.Ukongezelela, ukunyuka kwengcinezelo yomva ngokuqhelekileyo kubangela amanqanaba aphezulu okuxuba, angathathelwa ngqalelo kwi-simulation.
Ezi meko zilandelayo ze-HPLC kunye nokuseta uvavanyo zisetyenziselwe ukulinganisa amaza e-sine ekrwada ukuthelekisa ukusebenza okuhambelanayo nabaxube abamileyo abahlukeneyo.Umzobo kwi-Figure 5 ubonisa i-HPLC / UHPLC yenkqubo yoyilo lwenkqubo.Umxube we-static wavavanywa ngokubeka umxube ngokuthe ngqo emva kompompo naphambi kwe-injector kunye nekholomu yokwahlula.Uninzi lwemilinganiselo ye-sinusoidal yangasemva yenziwa ngokudlula i-injector kunye nekholamu ye-capillary phakathi kwe-static mixer kunye ne-UV detector.Xa uvavanya umlinganiselo wesignali ukuya kwingxolo kunye/okanye uhlalutya ubume bencopho, ukucwangciswa kwenkqubo kuboniswe kuMfanekiso 5.
Umzobo 4. Iploti yokudibanisa ukusebenza ngokufanelekileyo ngokuchasene nomthamo wokuxuba uluhlu lwabaxube be-static.Ukungahlambuluki kwethiyori kulandela umkhwa ofanayo njengedatha yokulinga yokungcola eqinisekisa ukunyaniseka kwe-CFD yokulinganisa.
Inkqubo ye-HPLC esetyenziselwa olu vavanyo yayiyi-Agilent 1100 Series HPLC ene-UV detector elawulwa yi-PC eqhuba isofthiwe ye-Chemstation.Itheyibhile yoku-1 ibonisa iimeko eziqhelekileyo zokulungelelanisa ukulinganisa ukusebenza kakuhle komxube ngokubeka iliso kwii-sinusoids ezisisiseko kwizifundo ezimbini.Uvavanyo lovavanyo lwenziwa kwimizekelo emibini eyahlukeneyo yezinyibilikisi.Izinyibilikisi ezibini ezixutywe kwimeko ye-1 yayiyi-solvent A (20 mM ammonium acetate kumanzi adibeneyo) kunye ne-solvent B (80% ye-acetonitrile (ACN) / 20% yamanzi e-deionized).Kwi-Case 2, i-solvent A yayiyisisombululo se-0.05% ye-acetone (ileyibhile) emanzini adibeneyo.I-Solvent B ngumxube we-80/20% ye-methanol kunye namanzi.Kwimeko ye-1, ipompo ibekwe kwinqanaba lokuhamba kwe-0.25 ml / min ukuya kwi-1.0 ml / min, kwaye kwimeko ye-2, ipompo ibekwe kwinqanaba lokuhamba rhoqo le-1 ml / min.Kuzo zombini iimeko, umlinganiselo womxube we-solvents A kunye no-B wawuyi-20% A / 80% B. I-detector imiselwe kwi-220 nm kwimeko ye-1, kwaye ubuninzi bokuxutywa kwe-acetone kwimeko ye-2 yayibekwe kwi-wavelength ye-265 nm.
Itheyibhile 1. Ulungelelwaniso lwe-HPLC kuMatyala 1 kunye ne-2 I-Case 1 Case 2 Pump Speed ​​​​0.25 ml / min ukuya kwi-1.0 ml / min 1.0 ml / min I-Solvent A 20 mM i-acetate ye-ammonium emanzini e-deionized 0.05% I-Acetone kumanzi adibeneyo I-Solvent B 80% 2% ye-Acetol 2% ye-Acetol 0lno% ye-Aceto 80% I-20% yomlinganiselo wokunyibilikisa wamanzi angama-20% A / 80% B 20% A / 80% B Isitshini 220 nm 265 nm
Irayisi.6. Iiplati zamaza e-sine axubeneyo alinganiswe ngaphambi nasemva kokufaka isihluzo esisezantsi ukuze kususwe amacandelo asisiseko sokukhukuliseka kophawu.
Umzobo we-6 ngumzekelo oqhelekileyo wengxolo yesiseko edibeneyo kwi-Case 1, eboniswe njengephethini ephindaphindiweyo ye-sinusoidal ebekwe phezulu kwi-baseline drift.I-Baseline drift kukunyuka okucothayo okanye ukwehla kumqondiso ongasemva.Ukuba inkqubo ayivunyelwanga ukuba ilingane ixesha elide ngokwaneleyo, iya kuwa, kodwa iya kukhukuliseka ngokungahambi kakuhle naxa inkqubo izinzile ngokupheleleyo.Le siseko idla ngokunyuka xa isixokelelwano sisebenza kumnqantsa okanye iimeko zoxinzelelo oluphezulu.Xa oku kuqhutywa kwesiseko kukho, kunokuba nzima ukuthelekisa iziphumo ukusuka kwisampulu ukuya kwisampulu, enokuthi yoyiswe ngokufaka isihluzo sokupasa esisezantsi kwidatha ekrwada ukuhluza ezi zantlukwano ze-frequency ephantsi, ngaloo ndlela ibonelela ngeploti ye-oscillation enesiseko esicaba.Kwikhiwane.Umzobo wesi-6 ubonisa icebo lengxolo yesiseko somxube emva kokufaka isihluzo esisezantsi.
Emva kokugqiba ukulinganisa kweCFD kunye novavanyo lokuqala lovavanyo, abaxube abathathu abahlukeneyo be-static baphuhliswa emva koko kusetyenziswa amacandelo angaphakathi achazwe ngasentla kunye nemiqulu emithathu yangaphakathi: 30 µl, 60 µl kunye ne-90 µl.Olu luhlu lubandakanya uluhlu lwemiqulu kunye nokusebenza kokuxuba okufunekayo kuhlalutyi oluphantsi lwezicelo ze-HPLC apho ukuxuba okuphuculweyo kunye nokusabalalisa okuphantsi kuyadingeka ukuvelisa iziseko ze-amplitude ephantsi.Kwikhiwane.I-7 ibonisa imilinganiselo esisiseko yamaza e-sine efunyenwe kwinkqubo yovavanyo yoMzekelo 1 (i-acetonitrile kunye ne-acetate ye-ammonium njenge-tracers) kunye nemiqulu emithathu ye-static mixers kwaye akukho mixube efakiweyo.Iimeko zokuvavanya iziphumo eziboniswe kwi-Figure 7 zigcinwe rhoqo kuzo zonke iimvavanyo ze-4 ngokwenkqubo echazwe kwiThebhile 1 kwinqanaba lokuhamba kwe-solvent ye-0.5 ml / min.Faka ixabiso le-offset kwiiseti zedatha ukuze ziboniswe ecaleni ngaphandle kokudibana komqondiso.I-Offset ayichaphazeli i-amplitude yesiginali esetyenziselwa ukugweba inqanaba lokusebenza lomxube.Umyinge we-amplitude ye-sinusoidal ngaphandle komxube wawuyi-0.221 mAi, ngelixa i-amplitudes ye-static Mott mixers kwi-30 µl, 60 µl, kunye ne-90 µl yehla ukuya kwi-0.077, 0.017, kunye ne-0.004 mAi, ngokulandelanayo.
Umzobo 7. I-HPLC UV Detector Signal Offset vs. Ixesha le-Case 1 (i-acetonitrile ene-ammonium acetate indicator) ebonisa ukuxutywa kwe-solvent ngaphandle komxube, i-30 µl, i-60 µl kunye ne-90 µl abaxube be-Mott ababonisa ukuxuba okuphuculweyo (i-acetonitrile ene-ammonium acetate indicator) njengomthamo womxube we-static kwandisa umthamo.(i-offsets data real: 0.13 (akukho mixer), 0.32, 0.4, 0.45mA yokubonisa okungcono).
Idatha eboniswe kwifig.Ezisi-8 ziyafana nakuFig. 7, kodwa ngeli xesha zibandakanya iziphumo zemixube emile ye-HPLC esetyenziswa ngokuqhelekileyo enemithamo yangaphakathi eyi-50 µl, 150 µl kunye ne-250 µl.Irayisi.Umzobo 8. I-HPLC ye-UV ye-UV Detector Signal Offset kunye ne-Time Plot ye-Case 1 (i-Acetonitrile kunye ne-Acetate ye-Acetate njengezibonakaliso) ebonisa ukuxutywa kwe-solvent ngaphandle komxube we-static, uchungechunge olutsha lwe-Mott static mixers, kunye nabaxube abathathu abaqhelekileyo (i-data real data offset yi-0.1 (ngaphandle kwe-mixer), 0.0.0.8, 0.0.8, 0.0. 9 mA ngokulandelelanayo kwisiphumo esingcono sokubonisa).Ipesenti yokunciphisa i-sine wave ibalwa ngomlinganiselo we-amplitude ye-sine wave ukuya kwi-amplitude ngaphandle komxube ofakiweyo.Iipesenti ezilinganiselweyo zokuthomalalisa amaza e-sine kwi-Case 1 kunye ne-2 zidweliswe kwiThebhile 2, kunye nomthamo wangaphakathi womxube omtsha omileyo kunye nabaxube abasixhenxe abaqhelekileyo abasetyenziswa kushishino.Idatha kwi-Figure 8 kunye ne-9, kunye nezibalo ezichazwe kwiThebhile 2, zibonisa ukuba i-Mott Static Mixer inokubonelela ukuya kwi-98.1% ye-sine wave attenuation, igqithise kakhulu ukusebenza komxube we-HPLC oqhelekileyo phantsi kwezi meko zovavanyo.Umzobo 9. I-HPLC ye-UV ye-detector ye-conset ye-offset kunye nexesha lexesha le-2 (i-methanol kunye ne-acetone njenge-tracers) ebonisa ukuba akukho mixer static (edibeneyo), uchungechunge olutsha lwe-mott static mixers kunye nee-mixers ezimbini eziqhelekileyo (i-data yokwenene i-offsets yi-0, i-11 (ngaphandle komxube. ), i-0.22, i-0.3, kunye ne-0.3 ukubonisa ngcono.Imixube esixhenxe esetyenziswa ngokuqhelekileyo kushishino nayo yavavanywa.Ezi ziquka abaxube abaneemitha ezintathu ezahlukeneyo zangaphakathi ukusuka kwinkampani A (i-Mixer A1 ekhethiweyo, i-A2 kunye ne-A3) kunye nenkampani B (i-Mixer ekhethiweyo B1, i-B2 kunye ne-B3).Inkampani C ilinganise ubungakanani obunye kuphela.
Itheyibhile 2. Iimpawu ze-Static Mixer ezivuselelayo kunye ne-Internal Volume Static Mixer Case 1 Ukubuyisela i-Sinusoidal: Uvavanyo lwe-Acetonitrile (Ukusebenza) I-Case 2 yoBuyiselo lwe-Sinusoidal: Uvavanyo lwamanzi e-Methanol (Ukusebenza) Umthamo wangaphakathi (µl) Akukho Umxube - - 0% 5% 60 69 Mott% 30 69. 1.3%. 370 Umxube C 97.2% 97.4% 250
Uhlalutyo lweziphumo kuMfanekiso 8 nakwiTheyibhile 2 lubonisa ukuba i-30 µl Mott static mixer inomxube osebenza ngokufanelekileyo njengomxube we-A1, okt 50 µl, nangona kunjalo, i-30 µl Mott ine-30% yevolyum yangaphakathi ngaphantsi.Xa uthelekisa i-60 µl Mott mixer kunye ne-150 µl umthamo wangaphakathi we-A2 mixer, kukho uphuculo oluncinci ekuxubeni okusebenzayo kwe-92% kunye ne-89%, kodwa okona kubaluleke kakhulu, eli nqanaba eliphezulu lokuxuba liphunyezwe kwi-1/3 yomthamo womxube.umxhubi ofanayo A2.Ukusebenza komxube we-90 µl Mott kulandele intsingiselo efanayo ne-A3 yomxubi enomthamo wangaphakathi wama-250 µl.Ukuphuculwa kokuxuba ukusebenza kwe-98% kunye ne-92% kwakhona kwabonwa kunye nokunciphisa i-3-fold in volume yangaphakathi.Iziphumo ezifanayo kunye nokuthelekiswa kwafunyanwa kubaxube B kunye no-C. Ngenxa yoko, uchungechunge olutsha lwabaxube be-static i-Mott PerfectPeak TM lubonelela ngokusebenza kakuhle kokuxubana kunabaxube abakhuphisana nabo, kodwa kunye nomthamo wangaphakathi ongaphantsi, ukubonelela ngengxolo yemvelaphi engcono kunye nomlinganiselo ongcono we-signal-to-noise, i-Analyte engcono yokuqonda, i-peak shape kunye nesisombululo esiphezulu.Iindlela ezifanayo ekuxubeni okusebenzayo zabonwa kuzo zombini i-Case 1 kunye ne-Case 2 izifundo.Kwi-Case 2, iimvavanyo zenziwa kusetyenziswa (i-methanol kunye ne-acetone njengezibonakaliso) ukuthelekisa ukusebenza kakuhle kokuxuba kwe-60 ml ye-Mott, i-mixer ehambelanayo ne-A1 (ivolumu yangaphakathi 50 µl) kunye nomxube ohambelanayo we-B1 (umthamo wangaphakathi 35 µl)., ukusebenza kwakungalunganga ngaphandle komxube ofakwe, kodwa wawusetyenziselwa uhlalutyo olusisiseko.Umxube we-60 ml we-Mott ubonakalise ukuba ngoyena mxubi kwiqela lovavanyo, ebonelela ngokunyuka kwe-90% ekusebenzeni kokuxuba.I-Mixer A1 ethelekisayo ibone ukuphuculwa kwe-75% ekusebenzeni kokuxuba okulandelwa yi-45% yokuphucula kwi-B1 ehambelanayo.Uvavanyo olusisiseko lokuncitshiswa kwamaza e-sine kunye nesantya sokuhamba luye lwaqhutywa kuthotho lwabaxubi phantsi kweemeko ezifanayo novavanyo lwe-sine curve kwi-Case 1, kunye nesantya sokuhamba kuphela esitshintshileyo.Idatha ibonise ukuba kuluhlu lweereyithi zokuhamba ukusuka kwi-0.25 ukuya kwi-1 ml / min, ukuhla kokuqala kwi-sine wave kwahlala kuthe gqolo kuyo yonke imiqulu emithathu yomxube.Kwimixube emibini emincinci yomthamo, kukho ukunyuka okuncinci kwi-contraction ye-sinusoidal njengoko izinga lokuhamba liyancipha, elilindeleke ngenxa yokunyuka kwexesha lokuhlala kwe-solvent kwi-mixer, okuvumela ukwanda kokuxuba.Ukuthatyathwa kwe-sine wave kulindeleke ukuba kunyuke njengoko ukuhamba kuncipha ngakumbi.Nangona kunjalo, owona mthamo mkhulu womxube onesona siseko siphezulu sokuthomalalisa i-sine wave, isiseko se-sine wave sihlala singatshintshi (ngaphakathi koluhlu lokungaqiniseki kovavanyo), ngamaxabiso aqala ukusuka kwi-95% ukuya kwi-98%.Irayisi.10. Ukunciphisa okusisiseko kwe-sine wave ngokuchasene nesantya sokuhamba kwimeko ye-1. Uvavanyo lwenziwe phantsi kweemeko ezifana novavanyo lwe-sine kunye nesantya sokuhamba okuguquguqukayo, ukujova i-80% yomxube we-80/20 we-acetonitrile kunye namanzi kunye ne-20% ye-20 mM ammonium acetate.
Uluhlu olutsha oluphuhlisiwe lwe-patent ye-PerfectPeak TM e-inline imixube ye-static enemithamo emithathu yangaphakathi: i-30 µl, i-60 µl kunye ne-90 µl igubungela umthamo kunye noluhlu lokusebenza lokuxuba olufunekayo kuninzi lwe-HPLC luhlalutya olufuna ukuxutywa okuphuculweyo kunye nemigangatho ephantsi yokusasazwa.Umxube omtsha we-static ufezekisa oku ngokusebenzisa iteknoloji entsha yoshicilelo lwe-3D ukwenza isakhiwo se-3D esisodwa esibonelela ngokuphuculwa kwe-hydrodynamic static mixing kunye nokunciphisa ipesenti ephezulu kwingxolo yesiseko kwiyunithi nganye umthamo womxube wangaphakathi.Ukusebenzisa i-1/3 yomthamo wangaphakathi womxube oqhelekileyo unciphisa ingxolo yesiseko ngama-98%.Abaxubeki abanjalo baquka imijelo edityanisiweyo enemigangatho emithathu eneendawo ezahlukeneyo ezinqamlezayo kunye nobude bendlela eyahlukileyo njengoko ulwelo luwela imiqobo yejometri entsonkothileyo ngaphakathi.Intsapho entsha yabaxube be-static ibonelela ngokusebenza okuphuculweyo ngaphezu kwabaxube abakhuphisanayo, kodwa ngomthamo wangaphakathi ongaphantsi, obangela umlinganiselo ongcono wesignali ukuya kwingxolo kunye nemida ephantsi yobungakanani, kunye nokuphuculwa komgangatho ophezulu, ukusebenza kakuhle kunye nesisombululo sovakalelo oluphezulu.
Kulo shicilelo I-Chromatography - i-RP-HPLC ehambelana nokusiNgqongileyo - Ukusetyenziswa kwe-chromatography ye-core-shell ukutshintsha i-acetonitrile nge-isopropanol kuhlalutyo kunye nokucoca - I-chromatograph yegesi entsha ye...
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Ixesha lokuposa: Nov-15-2022