Chinyorwa
Kuziva methylene blue murabhoritari: masipekitiramu einfrared nedzimwe nzira dzinotsigira
Fungidzira marabhoritari matatu achigamuchira upfu humwe chete hwebhuruu. Yekutanga inorekodha sipekitiramu yeinfrared yoti upfu hwacho imethylene blue. Yechipiri inoshandisa kromatogirafi yotaura kuti pane 0.4% Azure B. Yechitatu inoshandisa difrakisheni yemwaranzi yeX pamakristaro yodoma fomu yehaidireti. Dzose nhatu dzakarurama, asi hapana yadzo yapindura mimwe mibvunzo miviri. Kuvhiringidzika kunotanga kana mhinduro imwe ikatorwa seyakapindura yose mitatu.
Chinyorwa chino chinopatsanura mibvunzo iyoyo. Kuzivikanwa neinfrared kunosimbisa kuti mamorekuru ndeechinhu chipi nekuenzanisa nemuyero wekureferera. Kromatogirafi inosimbisa kuti chii chirimo. Difrakisheni inosimbisa fomu yechinhu chakasimba. Kupasa bvunzo yekuwirirana pakuzivikanwa hakusi chitupa chehuchena.
Kuzivikanwa neinfrared kunopindura mubvunzo mumwe zvakanaka
Bvunzo yekuziva methylene blue iri mubhuku remitemo yemishonga ndeyekuenzanisa sipekitiramu nemuyero, kwete kutara pamazita enhongonya. Muchiratidziro chemonogirafu yeUSP yemethylene blue, chikamu cheKuzivikanwa A chinotaura ongororo yemasipekitiramu einfrared uchishandisa midziyo yekuona yeATR kana piritsi repotassium bromide. Sipekitiramu yemuyenzaniso inofanira kuwirirana neyeUSP reference standard, muyenzaniso nemuyero zvagadzirirwa uye zvarekodwa mumamiriro akaenzana. Hapana rondedzero yakatarwa yenhamba dzemasaisai dzinoshandiswa pakuziva inopa mutongo. Mutongo unobva pakupindirana kwemasipekitiramu.
Sarudzo iyoyo inobva pamaitiro emasipekitiramu eFTIR emethylene blue. Zvinhu zvinonyanya kuoneka zviri munharaunda inonzi fingerprint. Zvinyorwa zvesainzi zvinowanzobatanidza bhendi guru reringi rine mabhondi anochinjana nenzvimbo iri pedyo ne1590 kusvika 1600 cm-1, panobatana mitowo yekutambanuka kwemabhondi ecarbon-carbon necarbon-nitrogen mumaringi anonzi aromatic. Mamwe mabhendi ari pedyo ne1490 ne1390 cm-1 ane maitiro ekuchinja kwechimiro cheringi, carbon-nitrogen, necarbon-hydrogen. Mabhendi ari pedyo ne1355 ne1330 cm-1 anosanganisira mabhondi ecarbon-nitrogen edimethylamino uye kuchinja kwechimiro chemapoka emethyl. Zvinooneka pedyo ne1225 kusvika 1250 cm-1 ndezvechiumbwa cheheterocyclic, ukuwo mabhendi ari pedyo ne1170 kusvika 1130 ne1066 cm-1 ane maitiro ecarbon-sulfur, uye kukotama kweC-H yeaaromatic kuri pedyo ne880 cm-1. Mitowo yekutambanuka inooneka kumusoro: C-H yeaaromatic pedyo ne3040 cm-1 uye C-H yeN-methyl pakati peanenge 2900 ne3000 cm-1. Tsananguro dzakaburitswa dzinosiyana pane zvimwe nokuti chiumbwa chephenothiazinium chinodedera sechinhu chine zvikamu zvinoshanda pamwe chete; saka tora tafura imwe neimwe inobatanidza mabhendi nemabhondi setsananguro yakataurwa, kwete seyo chete iripo.
Zvinhu zviviri zvinoitika pakugadzirira zvinoda kutariswa nokuti zvinoshandura masipekitiramu eIR emethylene blue zvisingashanduri dhayi yacho. Chekutanga, zvinhu zvine mvura yakabatana muchiumbwa chazvo zvinoratidza bhendi rakafara reO-H riri panenge pa3300 kusvika 3500 cm-1 pamwe nekukotama kwemvura pedyo ne1630 kusvika 1640 cm-1, uye mafomu akasiyana ehaidireti anochinja nzvimbo dzemabhendi efingerprint nenzira inogona kuyerwa. Chechipiri, zvinhu zveKBr zvinoumba piritsi zvinokweva unyoro: unyoro hwakatorwa hunobudisa mabhendi munzvimbo idzodzo dzemvura uye hunogona kutorwa semvura yehaidireti iri mumuyenzaniso. Kuongorora neATR hakushandisi zvinhu zveKBr izvi, asi kusimba kwezviratidzo zveATR kunoenderana nekudzika kunopinda mwaranzi, uko kunochinja nenhamba yemasaisai; saka sipekitiramu yeATR neyekupfuura kwemwaranzi muupfu humwe chete hazvigoni kungoiswa pamusoro peimwe zvichitarisirwa kupindirana. Mutemo wekushandisa unobva pachinodiwa nebhuku remitemo: enzanisa muyenzaniso nemuyero zvakarekodwa nenzira imwe chete, uye nyora kuti ndeipi yakashandiswa. Kuti unzwisise makemikari ecation, munyu, nemahaidireti ari shure kwemasipekitiramu aya, ona gwaro rekureferera pamusoro pechiumbwa nehunhu hwemethylene blue.
Tafura yekusarudza nzira yekuongorora
Tafura iyi ishoko rinobatsira pakusarudza. Verenga mutsara kubva kuruboshwe kuenda kurudyi kuti uone mubvunzo unopindurwa nenzira imwe neimwe, zvinoratidzwa nemhinduro yapasa, uye zvisati zvaratidzwa.
| Nzira | Mubvunzo wainopindura | Zvinoratidzwa nemhinduro yapasa | Zvaisingagoni kuratidza |
|---|---|---|---|
| FTIR ichienzaniswa nemuyero wekureferera | Chinhu ichi imethylene blue here? | Kuzivikanwa kwemamorekuru kunowirirana nesipekitiramu yekureferera | Huchena, mhando nehuwandu hwezvinosvibisa, fomu yehaidireti yoga, kana kukora kwemushonga wakanyungudutswa |
| Kuyera huwandu neHPLC-UV uye zvinosvibisa zveorganic (koramu yephenyl, 246 nm) | Pane methylene blue yakawanda sei uye Azure B yakawanda sei? | Kuzivikanwa nekromatogirafi kuburikidza nekuwirirana kwenguva yekubuda; huwandu hwechinhu nezvinosvibisa zvakatarwa | Fomu yechinhu chakasimba; kuzivikanwa kwenhongonya dzisingatarisirwi pasina miyero |
| LC-MS/MS ine miyero yakasimbiswa kuti yakakodzera | Ndeapi madhayi akabviswa mapoka emethyl aripo? | Kuparadzaniswa nekuzivikanwa kwezvinhu mumutevedzano weMB, Azure A, Azure B, Azure C, thionine | Kutevedzera bhuku remitemo; iyi inzira yakawedzerwa yakakodzera kutsvakurudza, kwete bvunzo yemonogirafu inogara ichiitwa |
| XRD yeupfu | Ndeipi haidireti ine makristaro iripo? | Fomu yechinhu chakasimba, misanganiswa yemafomu iri pamusoro pemuganhu wekugona kuonekwa, uye kuumbwa kwemakristaro | Kuzivikanwa kwemamorekuru ezvinosvibisa zvisina makristaro; kukora kwemushonga wakanyungudutswa |
| Kutorwa kwemwaranzi yeUV-Vis | Mushonga wakanyungudutswa unotora mwaranzi sezvinotarisirwa here? | Nzvimbo dzinozivikanwa dzekutorwa kwemwaranzi zvakanyanya uye maitiro anoenderana nekukora kwemushonga wakanyungudutswa | Kuzivikanwa kana huchena pachawo |
| Kuzivikanwa kwechloride uye kurasikirwa nehuremu pakuomesa (zvinotsigira) | Ioni inopikisa iripo here; ihuremu hwakawanda sei hunogona kubuda semhute? | Fomu yemunyu nehuremu hunorasika pakuomesa mumamiriro akatarwa | Kuti nderipi morekuru rinopa ruvara |
Nei kuwirirana kweinfrared kusiri chitupa chehuchena
Kuwirirana pakuzivikanwa kunobvisa mukana wekuti idhayi isiri iyo. Hakuratidzi zvose zviri mumuyenzaniso. Pane miganhu mitatu inonyanya kukosha.
Chekutanga, madhayi ane hukama hwepedyo anotaridzika zvakafanana muinfrared. Azure B inosiyana nemethylene blue neboka rimwe chete remethyl, saka sipekitiramu yayo yakafanana zvikuru neyemethylene blue. Musanganiswa une Azure B yezvikamu zvishoma kubva muzana unogona kuramba uchipindirana zvakanaka nemuyero wemethylene blue. Kuona chinosvibisa icho ibasa rekromatogirafi, rinotsanangurwa munhungamiro yezvinosvibisa methylene blue nenzira dzekuzviongorora.
Chechipiri, ongororo yemasipekitiramu einfrared inzira inotarisa zvinhu zvakawanda pamwe chete uye ine muganhu pakugona kuona zvikamu zviri zvishoma. Huwandu hudiki hwemadhayi ane hukama, zvinonyungudutsa zvasara, kana zvisaririra zveinorganic hunovanzwa pasi pemabhendi makuru. Kusavapo kwenhongonya dzakawedzerwa hakusi uchapupu hwakasimba hwekusavapo kwezvinosvibisa.
Chechitatu, muyero wekureferera ndiwo unotonga kuenzanisa kwose. Muyero wakashata, wakachinja nekuda kwehaidireti, kana usina kubatwa zvakanaka unoshandura hwaro hwekutonga. Ndizvo zvinoitikawo kana nzira dzisingaenderani dzikaenzaniswa, zvakadai sekutonga sipekitiramu yemuyenzaniso yeATR uchishandisa muyero weKBr. Rekodha nhamba yebatch yemuyero, nzira yakashandiswa, nemagadzirirwo pamwe chete nemutongo mumwe nomumwe.
Misanganiswa inowedzera imwe yambiro yekupedzisira. Sipekitiramu inonyanya kuwirirana asi iine mapendekete enhongonya kana kusimba kwezviratidzo kusingatarisirwi haisi mhinduro yapasa inongoda mashoko ezasi. Chiratidzo chokuti muyenzaniso unofanira kutanga waparadzaniswa usati wazivikanwa.
Kushandisa nzira dzinotsigirana
HPLC yemethylene blue inopa mhinduro yezviri mumuyenzaniso iyo infrared isingagoni kupa. Nzira yazvino iri mubhuku remitemo inoshandisa koramu yerudzi rwephenyl ine musanganiswa wemvura neacetonitrile une trifluoroacetic acid, uchichinja kuenzana kwezvinonyungudutsa, uye inoona pa246 nm, kwete mubhendi remwaranzi inooneka. Kuzivikanwa kunobva pakuwirirana kwenguva yekubuda mukoramu neyemuyero wekureferera; kuenzanisa kumwe chete ikoko kunopawo chiyero chehuwandu. Bvunzo yezvinosvibisa zveorganic inoziva Azure B ichishandisa zvinhu zvayo zvekureferera, nenguva yekubuda yakaenzaniswa iri pedyo ne0.8 kana methylene blue iri pa1.0, uye inoda kuti nhongonya mbiri idzi dziparadzaniswe zvakajeka zvikuru. Cherechedza kusarudzwa kweurefu hwesaisai: mutevedzano wemadhayi anobviswa mapoka emethyl unotora mwaranzi uchiramba uchienda kudivi dzvuku, kubva pathionine iri pedyo ne600 nm uchipfuura neAzure C, Azure A, neAzure B kusvika pamethylene blue iri pedyo ne670 nm. Saka mudziyo unoona mwaranzi wakatarwa pedyo ne660 nm haupi mhinduro dzakaenzana pamutevedzano wose uye unoratidza huwandu hudiki pane huripo hwedzimwe nhengo dzine hukama. Kana zvichidiwa kuongorora mhando nehuwandu zvemutevedzano wose, zvinofanira kuitwa nenzira yeC18 LC-MS/MS ine miyero yakasimbiswa kuti yakakodzera yechinhu chimwe nechimwe chiri kuyerwa.
Difrakisheni yeupfu inopindura mubvunzo wefomu yechinhu chakasimba iyo nzira mbiri dziri pamusoro dzinoparadza kana kufuratira: kunyungudutsa upfu kuti uitise kromatogirafi kunobvisa ruzivo rwemakristaro, uye kudedera kwemamorekuru kunoratidza mabhondi kwete marongerwo azvo anoramba achidzokororwa achienda kure. Mapatani edifrakisheni anosiyanisa mafomu ehaidireti nekuumbwa kwemakristaro, uye methylene blue inoda kunyatsoongororwa uku kupfuura zvinhu zvizhinji. Tsvakurudzo yaRager nevamwe pamusoro pechinhu chakasimba yakawana zviumbwa zvishanu zvakasiyana zvehaidireti, kusanganisira pentahaidireti, dhaihaidireti mbiri, monohaidireti, nehaidireti yepakati, uye haina kuwana trihydrate chaiyo pakati pemafomu akaongororwa. Mabatiro emurabhoritari akakosha pano: unyoro netembiricha zvinoshandura kugadzikana kwehaidireti, uye kukuya zvakanyanya kunogona kuchinja fomu kana kukanganisa kuumbwa kwemakristaro; saka dzora uye nyora mwero weunyoro hwemhepo netembiricha, uye deredza kukuya. Kuisa mazita ehaidireti nezvakunoita pahuremu hunoyerwa zvinokurukurwa zvakare mumafomu ehaidireti emethylene blue nekuiswa kwemazita.
Kutorwa kwemwaranzi yeUV-Vis kunoshanda senzira inotsigira. Nzvimbo dzinozivikanwa dzekutorwa kwemwaranzi zvakanyanya dzinosimbisa maitiro anotarisirwa emushonga wakanyungudutswa uye dzinobatsira pakuyera kukora kwawo, asi mushonga webhuruu unotora mwaranzi paurefu hwesaisai hunotarisirwa unowirirana nemethylene blue usina kuratidza zvakasimba kuti ndiyo, nokuti madhayi ane hukama anotora mwaranzi panzvimbo dziri pedyo.
Zvokubvunza usati watenga
Shandura misiyano iyi kuita mibvunzo yekutenga. Bvunza kuti ndeipi batch yakaongororwa, ndeipi nzira yakasimbisa kuzivikanwa, kana bvunzo yeHPLC yezvinosvibisa yakashandisa zvinhu zvekureferera zveAzure B, uye kana fomu yehaidireti yakaongororwa kana kungofungidzirwa. Kupfuura zvose, bvunza kana chitupa chichifukidza zvose zvinodiwa kana bvunzo dzakasarudzwa chete. Vatengesi vazhinji vanoti vanotevedzera bhuku remitemo vanongoongorora simbi dzinorema chete, zvichisiya mibvunzo yekuzivikanwa, huwandu, zvinosvibisa zveorganic, zvinonyungudutsa, uye tupukanana tusina kupindurwa.
Blupreme inoongorora zvose zvinodiwa neUSP, kusanganisira kuzivikanwa, huchena, zvinosvibisa zveorganic, zvinonyungudutsa zvasara, zvinosvibisa zvemaelementi, zvisaririra mushure mekupisa, miganhu yetupukanana, uye maendotoxin emabhakitiriya, ichishanda pamwe chete nemugadziri wemethylene blue yemishonga. Chitupa chekuongorora chebatch imwe neimwe chinowanikwa nevanhu vose chinoburitswa pakuongororwa kwemhando neBlupreme, saka hwaro hwekuyera huwandu nemhinduro dzezvinosvibisa zvinogona kuverengwa zvakananga pane kungofungidzirwa. Mhinduro dziri pedyo ne100% dzichiri kuda kuti hwaro hwadzo hwekuverenga hutsanangurwe, sezvinotsanangurwa nenhungamiro yehuwandu hunopfuura zvikamu 100 kubva muzana. Kuwirirana pakuzivikanwa kunotanga ongororo. Zvinyorwa zvizere zvinoipedzisa.