Whakaitihia te Haruru Tūāpapa o te Pūnaha HPLC/UHPLC me te Whakanuia te Tairongo mā te Whakaranu Pūmau Tānga 3D Mahi-Tiketike Hou – 6 o Pēpuere, 2017 – James C. Steele, Christopher J. Martineau, Kenneth L. Rubow – Tuhinga i roto i ngā Pūrongo Koiora

Kua whakawhanakehia he mīhini whakaranu hou kua hangaia kia tutuki ai ngā whakaritenga pakari o te chromatography wai mahi teitei (HPLC) me ngā pūnaha chromatography wai mahi tino teitei (HPLC me te UHPLC). Mā te ranunga ngoikore o ngā wāhanga neke e rua, neke atu rānei, ka hua ake he ōwehenga tohu-ki-haruru teitei ake, ka whakaiti i te aro. Ko te ranunga pūmau ōrite o ngā wai e rua, neke atu rānei, me te iti rawa o te rōrahi ā-roto me ngā rahinga ā-tinana o te mīhini whakaranu pūmau te paerewa teitei rawa atu o te mīhini whakaranu pūmau tino pai. Ka tutuki i te mīhini whakaranu pūmau hou tēnei mā te whakamahi i te hangarau tā 3D hou hei hanga i tētahi hanganga 3D ahurei e whakarato ana i te ranunga pūmau waiora pai ake me te ōrau whakaiti teitei rawa atu o te ngaru sine turanga mō ia wae rōrahi ā-roto o te ranunga. Mā te whakamahi i te 1/3 o te rōrahi ā-roto o te mīhini whakaranu tikanga ka whakaiti i te ngaru sine taketake mā te 98%. Kei roto i te mīhini whakaranu ngā hongere rere 3D e hono tahi ana me ngā horahanga whakawhiti-wāhanga me ngā roa ara rerekē i te mea ka whiti te wai i ngā āhuahanga 3D uaua. Mā te whakaranu i ngā ara rere maha, me te aueue ā-rohe me ngā awhiowhio, ka hua ake te whakaranu i ngā tauine moroiti, meso me te macro. Kua hangaia tēnei mīhini whakaranu ahurei mā te whakamahi i ngā whakatauira o ngā pūnaha wai rerehua rorohiko (CFD). E whakaatu ana ngā raraunga whakamātautau e whakaatuhia ana he pai te whakaranu me te iti o te rōrahi o roto.
Neke atu i te 30 tau te roa o te whakamahinga o te chromatography wai i roto i ngā ahumahi maha, tae atu ki ngā rongoā, ngā patu pepeke, te tiaki taiao, te tātaritanga taihara, me te tātari matū. He mea nui te kaha ki te ine ki ngā wāhanga ia miriona, iti iho rānei, ki te whanaketanga hangarau i roto i tētahi ahumahi. Ko te ngoikore o te whai huatanga o te whakaranu ka hua ake te ōwehenga tohu-ki-haruru ngoikore, he mea whakarihariha tēnei ki te hapori chromatography e pā ana ki ngā rohe kitenga me te aro. I te whakaranu i ngā whakarewa HPLC e rua, me akiaki te whakaranu mā ngā tikanga o waho kia ōrite ai ngā whakarewa e rua nā te mea kāore ētahi whakarewa e pai te whakaranu. Mena kāore i tino whakaranua ngā whakarewa, ka puta pea te ngoikore o te chromatogram HPLC, ka puta ko te haruru turanga nui rawa atu me/ranei te āhua tihi ngoikore. Ki te kore e pai te whakaranu, ka puta te haruru turanga hei ngaru sine (te piki me te heke) o te tohu pūoko i roto i te wā. I taua wā anō, ko te whakaranu ngoikore ka hua ake te whānui me te kore taurite o ngā tihi, ka whakaiti i te mahi tātari, te āhua tihi, me te taumira tihi. Kua mōhio te ahumahi ko ngā mīhini whakaranu raina-roto me te tī-pūmau he huarahi hei whakapai ake i ēnei rohe me te tuku i ngā kaiwhakamahi ki te whakatutuki i ngā rohe kitenga iti ake (ngā aro). Ka whakakotahi te mīhini whakaranu pūmau tino pai i ngā painga o te pai o te whakaranu, te iti o te rōrahi mate me te iti o te hekenga pēhanga me te iti o te rōrahi me te nui o te putanga o te pūnaha. Hei tāpiri, i te mea ka uaua haere te tātari, me whakamahi tonu ngā kaitātari i ngā whakarewa pōro me ngā whakarewa uaua ki te whakaranu. Ko te tikanga he mea nui te whakaranu pai ake mō ngā whakamātautau a meake nei, ka nui ake te hiahia mō te hoahoa me te mahi mīhini whakaranu pai ake.
Nō nā tata nei, kua whakawhanakehia e Mott tētahi whānuitanga hou o ngā mīhini whakaranu PerfectPeakTM kua patenttia, me ngā rōrahi ā-roto e toru: 30 µl, 60 µl me te 90 µl. Ka kapi i ēnei rahi te whānuitanga o ngā rōrahi me ngā āhuatanga whakaranu e hiahiatia ana mō te nuinga o ngā whakamātautau HPLC e hiahiatia ana te whakaranu pai ake me te iti o te marara. Ko ngā tauira e toru he 0.5″ te whānui, ā, e whakarato ana i te mahi ārahi-umanga i roto i tētahi hoahoa kiato. He mea hanga ēnei ki te maitai kore waikura 316L, kua whakakorehia mō te kore e taea te whakamahi, engari kei te wātea hoki te titanium me ētahi atu koranu whakarewa ātete waikura me te kore e taea te whakamahi matū. He pēhanga mahi mōrahi tō ēnei mīhini whakaranu tae atu ki te 20,000 psi. Kei te pikitia 1a tētahi whakaahua o tētahi mīhini whakaranu Mott 60 µl kua hangaia hei whakarato i te pai o te whakaranu i te wā e whakamahi ana i te rōrahi ā-roto iti ake i ngā mīhini whakaranu paerewa o tēnei momo. Ka whakamahia e tēnei hoahoa mīhini whakaranu hou te hangarau hanga tāpiri hou hei hanga i tētahi hanganga 3D ahurei e whakamahi ana i te iti o te rere o roto i tētahi atu mīhini whakaranu e whakamahia ana i roto i te umanga chromatography hei whakatutuki i te whakaranu tūmau. Ko ēnei mīhini whakaranu he mea hanga mai i ngā awa rere-toru-ahu e hono tahi ana me ngā horahanga whakawhiti-wāhanga rerekē me ngā roa ara rerekē i te mea ka whiti te wai i ngā arai āhuahanga matatini i roto. I te pikitia. E whakaatu ana te Pikitia 1b i tētahi hoahoa kauwhata o te mīhini whakaranu hou, e whakamahi ana i ngā hononga kōpeketanga HPLC miro paerewa ahumahi 10-32 mō te tomokanga me te putanga, ā, he rohe kikorangi atarangi o te tauranga mīhini whakaranu ā-roto kua patenthia. Ko ngā horahanga whakawhiti-wāhanga rerekē o ngā ara rere ā-roto me ngā huringa o te ahunga rere i roto i te rōrahi rere ā-roto ka hanga i ngā rohe o te rere pōrearea me te rere laminar, ka puta ai te ranunga i ngā tauine moroiti, meso me te macro. I whakamahia e te hoahoa o tēnei mīhini whakaranu ahurei ngā whakatauira hihiri wai rorohiko (CFD) hei tātari i ngā tauira rere me te whakapai ake i te hoahoa i mua i te tauira mō te whakamātautau tātari ā-roto me te aromatawai mara kiritaki. Ko te hanga tāpiri ko te tukanga o te tā i ngā wāhanga āhuahanga 3D tika mai i ngā tuhi CAD me te kore e hiahiatia he miihini tuku iho (mīhini mira, mīhini mīhini, me ētahi atu). Kua hangaia ēnei mīhini whakaranu pumau hou kia hangaia mā te whakamahi i tēnei tukanga, ka hangaia te tinana mīhini whakaranu mai i ngā tuhi CAD, ā, ka hangaia (tāia) ngā wāhanga paparanga i te paparanga mā te whakamahi i te hanga tāpiri. I konei, ka whakatakotoria he paparanga paura whakarewa e 20 maikorone te matotoru, ā, ka rewahia te paura e te reera e whakahaerehia ana e te rorohiko hei hanga totoka. Tāpirihia tētahi atu paparanga ki runga i tēnei paparanga, ka whakamahia te whakamahana reera. Whakahokia tēnei tukanga kia oti rawa te wāhanga. Kātahi ka tangohia te paura mai i te wāhanga kāore i te herea ki te reera, ka waiho he wāhanga tānga 3D e rite ana ki te tuhi CAD taketake. He rite te hua whakamutunga ki te tukanga moroiti-wai, ko te rerekētanga matua ko ngā wāhanga moroiti-wai he rua-ahu (papatahi), i te whakamahi i te hanga tāpiri, ka taea te hanga i ngā tauira rere matatini i roto i te āhuahanga toru-ahu. Kei te wātea ēnei taputapu i tēnei wā hei wāhanga tānga 3D i roto i te maitai kore waikura 316L me te titanium. Ka taea te whakamahi i te nuinga o ngā koranu whakarewa, ngā pūmua me ētahi uku hei hanga wāhanga mā te whakamahi i tēnei tikanga, ā, ka whakaarohia i roto i ngā hoahoa/hua o muri mai.
Raihi. 1. Whakaahua (a) me te hoahoa (b) o tētahi mīhini whakaranu Mott 90 μl e whakaatu ana i te wāhanga whakawhiti o te ara rere wai o te mīhini whakaranu kua whakamarumaruhia ki te kikorangi.
Whakahaerehia ngā whakatauira CFD mō te mahi a te mīhini whakaranu pūmau i te wā hoahoa hei āwhina i te whakawhanake i ngā hoahoa whai hua me te whakaiti i ngā whakamātautau whakamātautau-me-te-hē e pau ana te wā me te utu nui. Te whakatauira CFD o ngā mīhini whakaranu pūmau me ngā paipa paerewa (whakatauira kore-whakaranu) mā te whakamahi i te kete pūmanawa COMSOL Multiphysics. Te whakatauira mā te whakamahi i te miihini wai laminar pehanga-pehanga hei mārama ki te tere me te pēhanga wai i roto i tētahi wāhanga. Ko tēnei nekehanga wai, me te kawe matū o ngā matū wāhanga neke, ka āwhina ki te mārama ki te whakaranu o ngā wai kukū rerekē e rua. Ka akohia te tauira hei mahi o te wā, he rite ki te 10 hēkona, kia māmā ake ai te tatau i te wā e rapu ana i ngā otinga rite. I whiwhihia ngā raraunga ariā i roto i tētahi rangahau e hono ana ki te wā mā te whakamahi i te taputapu whakaata ira, i reira i whiriwhiria ai tētahi pūwāhi i waenganui o te putanga mō te kohikohinga raraunga. I whakamahia e te tauira CFD me ngā whakamātautau whakamātautau ngā whakarewa rerekē e rua mā roto i tētahi takirere tauira taurite me te pūnaha papu, ka hua ake he mono whakakapinga mō ia whakarewa i roto i te raina tauira. Kātahi ka whakaranua ēnei whakarewa ki roto i tētahi mīhini whakaranu pūmau. E whakaatu ana ngā Pikitia 2 me te 3 i ngā whakatauira rere mā roto i tētahi paipa paerewa (kāore he mīhini whakaranu) me te mā roto i tētahi mīhini whakaranu Mott. I whakahaerehia te whakatauira i runga i tētahi ngongo tika 5 cm te roa me te 0.25 mm ID hei whakaatu i te ariā o te whakauru tauwhitiwhiti i ngā mono wai me te acetonitrile parakore ki roto i te ngongo i te korenga o tētahi mīhini whakaranu tūmau, e whakaaturia ana i te Pikitia 2. I whakamahia e te whakatauira ngā ine tika o te ngongo me te mīhini whakaranu me te tere rere o te 0 .3 ml/min.
Raihi. 2. Te whakatauira i te rere o te CFD i roto i tētahi ngongo 5 cm te whānui me te diameter o roto o te 0.25 mm hei tohu i ngā mea ka tupu i roto i tētahi ngongo HPLC, arā, i te korenga o tētahi mīhini whakaranu. Ko te whero katoa e tohu ana i te wāhanga papatipu o te wai. Ko te kikorangi e tohu ana i te korenga o te wai, arā, te acetonitrile parakore. Ka kitea ngā rohe horapa i waenga i ngā mono whakawhiti o ngā wai rerekē e rua.
Raihi. 3. He mīhini whakaranu pūmau me te rōrahi o te 30 ml, i tauirahia i roto i te kete pūmanawa COMSOL CFD. Ko te tohu e tohu ana i te wāhanga papatipu o te wai i roto i te mīhini whakaranu. E whakaaturia ana te wai parakore i te whero me te acetonitrile parakore i te kikorangi. Ko te huringa o te wāhanga papatipu o te wai whakaata e tohuhia ana e te huringa o te tae o te ranunga o ngā wai e rua.
Kei te pikitia 4 te whakaaturanga o tētahi rangahau whakamana o te tauira hononga i waenga i te pai o te whakaranu me te rōrahi whakaranu. I te pikinga ake o te rōrahi whakaranu, ka piki ake te pai o te whakaranu. Ki te mōhio o ngā kaituhi, kāore e taea te whakaaro ki ētahi atu kaha ā-tinana uaua e mahi ana i roto i te whakaranu i roto i tēnei tauira CFD, ka hua ake he pai ake te whakaranu i roto i ngā whakamātautau whakamātautau. I inehia te pai o te whakaranu whakamātautau hei ōrau whakahekenga i roto i te sinusoid turanga. Hei tāpiri, ko te pikinga o te pēhanga whakamuri ka hua ake he taumata whakaranu teitei ake, kāore e whakaarohia i roto i te whakatauira.
I whakamahia ngā tikanga HPLC me te whakatakotoranga whakamātautau e whai ake nei hei ine i ngā ngaru sine mata hei whakataurite i te mahi whanaunga o ngā mīhini whakaranu pūmau rerekē. E whakaatu ana te hoahoa i te Pikitia 5 i tētahi tahora pūnaha HPLC/UHPLC noa. I whakamatautauria te mīhini whakaranu pūmau mā te whakanoho i te mīhini whakaranu i muri tonu i te papu me mua i te pou werowero me te pou wehewehe. Ko te nuinga o ngā inenga sinusoidal papamuri ka mahia mā te karo i te pou werowero me te pou capillary i waenganui i te mīhini whakaranu pūmau me te pūoko UV. I te aromatawai i te ōwehenga tohu-ki-haruru me/te tātari rānei i te āhua tihi, ka whakaaturia te whirihoranga pūnaha i te Pikitia 5.
Pikitia 4. Kauwhata o te pai o te whakaranu me te rōrahi whakaranu mō te whānuitanga o ngā whakaranu pūmau. Ko te poke ariā e whai ana i te ia o te poke whakamātautau e whakaū ana i te mana o ngā whakatauira CFD.
Ko te pūnaha HPLC i whakamahia mō tēnei whakamātautau he Agilent 1100 Series HPLC me te pūoko UV e whakahaeretia ana e te PC e whakahaere ana i te pūmanawa Chemstation. E whakaatu ana te Ripanga 1 i ngā tikanga whakahāngai noa mō te ine i te pai o te whakaranu mā te aroturuki i ngā sinusoid taketake i roto i ngā rangahau take e rua. I whakahaerehia ngā whakamātautau whakamātautau ki runga i ngā tauira rerekē e rua o ngā whakarewa. Ko ngā whakarewa e rua i konatunatua i te take 1 ko te whakarewa A (20 mM ammonium acetate i roto i te wai whakakore ion) me te whakarewa B (80% acetonitrile (ACN)/20% wai whakakore ion). I te Take 2, ko te whakarewa A he otinga o te 0.05% acetone (tapanga) i roto i te wai whakakore ion. Ko te whakarewa B he ranunga o te 80/20% methanol me te wai. I te take 1, i whakatakotoria te papu ki te tere rere o te 0.25 ml/min ki te 1.0 ml/min, ā, i te take 2, i whakatakotoria te papu ki te tere rere pumau o te 1 ml/min. I ngā take e rua, ko te ōwehenga o te ranunga o ngā whakarewa A me B he 20% A/80% B. I whakatakotoria te pūoko ki te 220 nm i te take 1, ā, ko te mimiti mōrahi o te acetone i te take 2 i whakatakotoria ki te roanga ngaru o te 265 nm.
Ripanga 1. Ngā Whirihoranga HPLC mō ngā Take 1 me te 2 Take 1 Take 2 Tere o te Papu 0.25 ml/min ki te 1.0 ml/min 1.0 ml/min Whakarewa A 20 mM ammonium acetate i roto i te wai whakakore ion 0.05% Acetone i roto i te wai whakakore ion Whakarewa B 80% Acetonitrile (ACN) / 20% wai whakakore ion 80% methanol / 20% wai whakakore ion Ōwehenga whakarewa 20% A / 80% B 20% A / 80% B Pūoko 220 nm 265 nm
Raihi. 6. Ngā kauwhata o ngā ngaru sine whakauru i inehia i mua atu, ā, i muri i te whakamahinga o te tātari pā-iti hei tango i ngā wāhanga nekenekehanga o te tohu.
Ko te Pikitia 6 tētahi tauira noa o te haruru turanga whakauru i roto i te Take 1, e whakaaturia ana hei tauira sinusoidal e tāruaruatia ana i runga i te nekehanga turanga. Ko te nekehanga turanga he pikinga puhoi, he hekenga puhoi rānei i roto i te tohu papamuri. Mena kāore te pūnaha e whakaaetia kia taurite mō te wā roa, ka hinga tonu, engari ka neke haere tonu ahakoa he tino pumau te pūnaha. Ka piki ake tēnei nekehanga turanga ina whakahaerehia te pūnaha i roto i ngā āhuatanga pikinga pari, teitei rānei o te pēhanga whakamuri. Ina kitea tēnei nekehanga turanga, ka uaua pea te whakataurite i ngā hua mai i tētahi tauira ki tētahi tauira, ka taea te wikitoria mā te whakamahi i tētahi tātari iti-haere ki ngā raraunga mata hei tātari i ēnei rerekētanga auau iti, ā, mā reira ka whakaratohia he kauwhata oscillation me tētahi turanga papatahi. I te pikitia. E whakaatu ana hoki te Pikitia 6 i tētahi kauwhata o te haruru turanga o te whakaranu i muri i te whakamahi i tētahi tātari iti-haere.
I muri i te otinga o ngā whakatauira CFD me ngā whakamātautau whakamātautau tuatahi, i whakawhanakehia ētahi mīhini whakaranu pūmau motuhake e toru mā te whakamahi i ngā wāhanga o roto kua whakaahuatia i runga ake nei me ngā rōrahi o roto e toru: 30 µl, 60 µl me te 90 µl. Ka hipokina e tēnei whānuitanga te whānuitanga o ngā rōrahi me te mahi whakaranu e hiahiatia ana mō ngā tono HPLC iti-tātari e hiahiatia ana te whakaranu pai ake me te marara iti hei whakaputa i ngā turanga whānui iti. I te pikitia 7 e whakaatu ana i ngā inenga ngaru sine taketake i whiwhihia i runga i te pūnaha whakamātautau o te Tauira 1 (acetonitrile me te ammonium acetate hei tohu) me ngā rōrahi e toru o ngā mīhini whakaranu pūmau, ā, kāore he mīhini whakaranu i tāutahia. Ko ngā tikanga whakamātautau whakamātautau mō ngā hua i whakaaturia i te Pikitia 7 i puritia kia rite tonu puta noa i ngā whakamātautau e 4 e ai ki te tikanga i whakatakotoria i roto i te Ripanga 1 i te tere rere o te whakarewa o te 0.5 ml/min. Whakamahia he uara taupatupatu ki ngā huinga raraunga kia taea ai te whakaatu taha ki taha me te kore e taupatupatu tohu. Kāore te taupatupatu e pā ki te whānui o te tohu i whakamahia hei aromatawai i te taumata mahi o te mīhini whakaranu. Ko te kaha o te oro sinusoidal toharite i waho o te mīhini whakaranu he 0.221 mAi, ko te kaha o ngā mīhini whakaranu Mott tūmau i te 30 µl, 60 µl, me te 90 µl i heke ki te 0.077, 0.017, me te 0.004 mAi.
Pikitia 7. Te Whakakorenga Tohu o te Pūoko UV HPLC vs. Te Wā mō te Take 1 (acetonitrile me te tohu ammonium acetate) e whakaatu ana i te whakaranu whakarewa me te kore he whakaranu, 30 µl, 60 µl me te 90 µl ngā whakaranu Mott e whakaatu ana i te whakaranu pai ake (he iti ake te kaha o te tohu) i te pikinga o te rōrahi o te whakaranu tūmau. (ngā whakakorenga raraunga tūturu: 0.13 (kāore he whakaranu), 0.32, 0.4, 0.45mA mō te whakaaturanga pai ake).
Ko ngā raraunga e whakaaturia ana i te pikitia 8 he rite tonu ki te pikitia 7, engari i tēnei wā kei roto ko ngā hua o ngā mīhini whakaranu HPLC pūmau e toru e whakamahia whānuitia ana me ngā rōrahi o roto o te 50 µl, 150 µl me te 250 µl. Rice. Pikitia 8. Tauwehenga Tohu Pūoko HPLC UV me te Kauwhata Wā mō te Take 1 (Acetonitrile me te Ammonium Acetate hei tohu) e whakaatu ana i te whakaranu o te whakarewa me te kore mīhini whakaranu pūmau, te raupapa hou o ngā mīhini whakaranu pūmau Mott, me ngā mīhini whakaranu tikanga e toru (ko te tauwehenga raraunga tūturu ko te 0.1 (me te kore mīhini whakaranu), 0.32, 0.48, 0.6, 0.7, 0.8, 0.9 mA ia mō te pānga whakaatu pai ake). Ka tatauhia te ōrau whakahekenga o te ngaru sine turanga mā te ōwehenga o te kaha o te ngaru sine ki te kaha me te kore te mīhini whakaranu i tāutahia. Ko ngā ōrau whakaiti ngaru sine i inehia mō ngā Take 1 me te 2 kua whakarārangihia ki te Ripanga 2, me ngā rōrahi ā-roto o tētahi mīhini whakaranu pūmau hou me ngā mīhini whakaranu paerewa e whitu e whakamahia whānuitia ana i roto i te umanga. Ko ngā raraunga i roto i ngā Pikitia 8 me te 9, me ngā tātaitanga i whakaaturia i roto i te Ripanga 2, e whakaatu ana ka taea e te Mīhini Whakaranu Pūmau Mott te whakarato i te whakaiti ngaru sine tae atu ki te 98.1%, he nui atu i te mahi a tētahi mīhini whakaranu HPLC tikanga i raro i ēnei tikanga whakamātautau. Pikitia 9. Te tauwehenga tohu pūoko UV HPLC me te kauwhata wā mō te take 2 (methanol me te acetone hei tohu) e whakaatu ana i te kore mīhini whakaranu pūmau (whakakotahi), he raupapa hou o ngā mīhini whakaranu pūmau Mott me ngā mīhini whakaranu tikanga e rua (ko ngā tauwehenga raraunga tūturu ko te 0, 11 (kāore he mīhini whakaranu. ), 0.22, 0.3, 0.35 mA me te whakaatu pai ake). E whitu ngā mīhini whakaranu e whakamahia whānuitia ana i roto i te umanga i arotakengia hoki. Kei roto i ēnei ko ngā mīhini whakaranu me ngā rahinga ā-roto e toru rerekē mai i te kamupene A (ko te Kaiwhakaranu A1, A2 me te A3) me te kamupene B (ko te Kaiwhakaranu B1, B2 me te B3) . Kotahi te rahi i whakatauhia e te Kamupene C.
Ripanga 2. Ngā Āhuatanga Whakaoho o te Ranu Pūmau me te Rōrahi ā-Roto Ranu Pūmau Take 1 Whakaora Sinusoidal: Whakamātautau Acetonitrile (Paitake) Take 2 Whakaora Sinusoidal: Whakamātautau Methanol Wai (Paitake) Rōrahi ā-Roto (µl) Kāore he Ranu – - 0 Mott 30 65% 67.2% 30 Mott 60 92.2% 91.3% 60 Mott 90 98.1% 97.5% 90 Ranu A1 66.4% 73.7% 50 Ranu A2 89.8% 91.6% 150 Ranu A3 92.2% 94.5% 250 Ranu B1 44.8% 45.7% 9 35 Ranu B2 845.% 96.2% 370 Ranu C 97.2% 97.4% 250
E whakaatu ana te tātari i ngā hua i te Pikitia 8 me te Ripanga 2 he rite tonu te pai o te whakaranu a te mīhini whakaranu Mott pūmau 30 µl ki te mīhini whakaranu A1, arā, 50 µl, heoi, he 30% te iti iho o te rōrahi o roto o te mīhini Mott 30 µl. I te whakataurite i te mīhini whakaranu Mott 60 µl ki te mīhini whakaranu rōrahi o roto 150 µl A2, he iti ake te pai o te whakaranu o te 92% ki te 89%, engari he mea nui ake, i tutuki tēnei taumata whakaranu teitei ake i te 1/3 o te rōrahi o te mīhini whakaranu. He rite tonu te mahi a te mīhini whakaranu Mott 90 µl ki te mīhini whakaranu A3 me te rōrahi o roto o te 250 µl. I kitea hoki ngā whakapainga o te mahi whakaranu o te 98% me te 92% me te whakahekenga o te rōrahi o roto e 3 ngā wā. I whiwhihia ngā hua me ngā whakataurite ōrite mō ngā mīhini whakaranu B me C. Nō reira, ko te raupapa hou o ngā mīhini whakaranu pūmau Mott PerfectPeakTM e whakarato ana i te pai o te whakaranu i ngā mīhini whakaranu whakataetae rite, engari he iti ake te rōrahi o roto, e whakarato ana i te haruru papamuri pai ake me te ōwehenga tohu-ki-haruru pai ake, te tairongo pai ake o te Analyte, te āhua tihi me te taumira tihi. I kitea ngā au rite o te pai o te whakaranu i roto i ngā rangahau Take 1 me Take 2. Mō te Take 2, i whakahaerehia ngā whakamātautau mā te whakamahi i (methanol me te acetone hei tohu) hei whakataurite i te pai o te whakaranu o te 60 ml Mott, he mīhini whakaranu rite A1 (rōrahi o roto 50 µl) me te mīhini whakaranu rite B1 (rōrahi o roto 35 µl). , he ngoikore te mahi me te kore he mīhini whakaranu i tāutahia, engari i whakamahia mō te tātaritanga turanga. Ko te mīhini whakaranu Mott 60 ml te mīhini whakaranu pai rawa atu i roto i te rōpū whakamātautau, e whakarato ana i te pikinga 90% o te pai o te whakaranu. I kite te mīhini whakaranu rite A1 i te whakapainga 75% o te pai o te whakaranu, ā, i muri mai ko te whakapainga 45% i roto i te mīhini whakaranu rite B1. I whakahaerehia he whakamātautau whakaiti ngaru sine taketake me te tere rere i runga i tētahi raupapa o ngā mīhini whakaranu i raro i ngā āhuatanga ōrite ki te whakamātautau pihi sine i te Take 1, ko te tere rere anake i rerekē. I whakaatuhia e ngā raraunga i roto i te awhe o ngā tere rere mai i te 0.25 ki te 1 ml/min, i noho tonu te hekenga tuatahi o te ngaru sine mō ngā rōrahi mīhini whakaranu e toru. Mō ngā mīhini whakaranu rōrahi iti e rua, he pikinga iti o te whakahekenga sinusoidal i te hekenga o te tere rere, e matapaetia ana nā te pikinga o te wā noho o te whakarewa i roto i te mīhini whakaranu, e āhei ai te pikinga o te ranunga horapa. E matapaetia ana ka piki ake te tangohanga o te ngaru sine i te hekenga tonu o te rere. Heoi, mō te rōrahi mīhini whakaranu nui rawa atu me te whakaiti turanga ngaru sine teitei rawa atu, i noho tonu te whakaiti turanga ngaru sine (i roto i te awhe o te koretake whakamātautau), me ngā uara mai i te 95% ki te 98%. Rice. 10. Te whakaiti taketake o te ngaru sine me te tere rere i te take 1. I whakahaerehia te whakamātautau i raro i ngā āhuatanga rite ki te whakamātautau sine me te tere rere rerekē, me te werohanga i te 80% o te ranunga 80/20 o te acetonitrile me te wai me te 20% o te 20 mM ammonium acetate.
Ko te whānuitanga hou o ngā mīhini whakaranu ā-roto PerfectPeakTM kua patenthia me ngā rōrahi ā-roto e toru: 30 µl, 60 µl me te 90 µl e kapi ana i te whānuitanga rōrahi me te mahi whakaranu e hiahiatia ana mō te nuinga o ngā tātari HPLC e hiahia ana kia pai ake te whakaranu me ngā papa marara iti. Ka tutuki i te mīhini whakaranu ā-roto hou tēnei mā te whakamahi i te hangarau tā 3D hou hei hanga i tētahi hanganga 3D ahurei e whakarato ana i te whakaranu ā-roto waiora pai ake me te ōrau teitei o te whakaiti i te haruru turanga mō ia rōrahi o te ranunga ā-roto. Mā te whakamahi i te 1/3 o te rōrahi ā-roto o te mīhini whakaranu tikanga ka whakaiti i te haruru turanga mā te 98%. Ko ēnei mīhini whakaranu he hongere rere toru-ahu e hono tahi ana me ngā horahanga whakawhiti-wāhanga rerekē me ngā roa ara rerekē i te mea ka whiti te wai i ngā arai āhuahanga matatini i roto. Ka whakaratohia e te whānau hou o ngā mīhini whakaranu ā-roto he mahi pai ake i ngā mīhini whakaranu whakataetae, engari he iti ake te rōrahi ā-roto, ka hua ake he ōwehenga tohu-ki-haruru pai ake me ngā rohe rahinga iti ake, me te whakapai ake i te āhua tihi, te whai huatanga me te taumira mō te aro nui ake.
I tēnei putanga Chromatography – RP-HPLC hoa-taiao – Te whakamahinga o te chromatography anga-matua hei whakakapi i te acetonitrile ki te isopropanol i roto i te tātari me te purenga – He chromatography hau hou mō…
Pokapū Pakihi o te Ao Labmate Limited Oak Court Sandridge Park, Porters Wood St Albans Hertfordshire AL3 6PH United Kingdom


Wā tuku: Whiringa-ā-rangi 15-2022