Gane shuɗin methylene a dakin gwaje-gwaje: bakunan infrared da hanyoyin taimako

Ka yi tunanin dakunan gwaje-gwaje uku sun karɓi shuɗin foda iri ɗaya. Na farko ya rubuta bakan infrared kuma ya bayyana cewa shuɗin methylene ne. Na biyu ya gudanar da chromatography kuma ya bayar da rahoton 0.4% Azure B. Na uku ya yi amfani da karkatarwar X-ray daga lu'ulu'un kuma ya bayyana siffar hydrate. Dukkansu ukun sun yi daidai, amma babu wanda ya amsa sauran tambayoyin biyu. Ruɗani yana farawa ne idan aka ɗauki sakamako guda a matsayin amsar dukkan ukun.

Wannan makala ta raba waɗannan tambayoyin. Gane sinadari da infrared yana tabbatar da ainihin nau'in ƙwayar sinadari ta hanyar kwatantawa da samfurin ma'auni. Chromatography yana tabbatar da abubuwan da ke cikin samfurin. Karkatarwar haske tana tabbatar da sifarsa a yanayin daskararru. Daidaituwar da ta tsallake gwajin gane sinadari ba takardar shaidar tsarki ba ce.

Gane sinadari da infrared yana amsa tambaya guda da kyau

Gwajin gane shuɗin methylene da ke cikin kundin ƙa'idojin magunguna kwatanta bakan samfurin da na ma'auni ne, ba jerin kololuwar bakan da za a duba ba. A ƙarƙashin samfotin bayanin ƙa'idojin USP na shuɗin methylene, Identification A ya ambaci nazarin infrared ta amfani da tsarin gani na ATR ko ƙwayar potassium bromide da aka matse. Dole bakan samfurin ya yi daidai da bakan samfurin ma'aunin USP, tare da shirya samfurin da ma'aunin da rubuta bakunansu a yanayi masu daidaito. Babu wani ƙayyadadden jerin lambobin igiya na tantancewa da ke yanke hukunci. Daidaituwar bakunan idan an ɗora su kan juna ce ke yin hakan.

Wannan zaɓin tsarin gwaji yana nuna yadda bakunan FTIR na shuɗin methylene ke kasancewa. Alamomin da suka fi ƙarfi suna yankin da ke ɗauke da siffofin musamman na sinadarin. Bayanan da aka wallafa suna danganta babban zangon zoben da ke da tsarin conjugation da yankin kusa da 1590 zuwa 1600 cm-1, inda yanayin miƙewar haɗin carbon-carbon da carbon-nitrogen na zoben aromatic ke haɗuwa. Sauran zanguna kusa da 1490 da 1390 cm-1 suna nuna halayen murɗewar zobe, carbon-nitrogen, da carbon-hydrogen. Zanguna kusa da 1355 da 1330 cm-1 sun shafi haɗin carbon-nitrogen na dimethylamino da murɗewar methyl. Alamomi kusa da 1225 zuwa 1250 cm-1 sun shafi tsarin zoben heterocyclic, yayin da zanguna kusa da 1170 zuwa 1130 da 1066 cm-1 suke nuna halayen carbon-sulfur, tare da lanƙwasawar C-H na aromatic kusa da 880 cm-1. Yanayin miƙewa yana bayyana a lambobin igiya mafi girma: C-H na aromatic kusa da 3040 cm-1 da C-H na N-methyl tsakanin kusan 2900 da 3000 cm-1. Dangantakar da wallafe-wallafe suka bayyana tana bambanta a cikakkun bayanai saboda tsarin phenothiazinium yana girgiza ne a matsayin tsarin da sassansa ke haɗuwa, don haka a ɗauki kowane teburin dangantaka guda a matsayin bayanin da aka bayar, ba matsayin bayani guda tilo da zai yiwu ba.

Tasirin shirye-shirye guda biyu suna buƙatar kulawa saboda suna sauya bakunan IR na shuɗin methylene ba tare da sauya rinin ba. Na farko, sinadarin da ke ɗauke da ruwan hydrate yana nuna faɗaɗɗen zangon O-H kusa da 3300 zuwa 3500 cm-1 tare da lanƙwasawar ruwa kusa da 1630 zuwa 1640 cm-1, kuma siffofin hydrate dabam-dabam suna sauya matsayin zangunan musamman na sinadarin da adadin da za a iya aunawa. Na biyu, kayan KBr da aka matse suna jan danshi: danshin da suka sha yana samar da zanguna a daidai waɗannan yankunan ruwa, kuma yana iya zama kamar ruwan hydrate ne daga samfurin. Gwaji da ATR yana kauce wa kayan KBr, amma ƙarfin alamomin ATR yana canzawa bisa zurfin shigar hasken da ya dogara da lambar igiya; saboda haka ba za a iya ɗora bakan ATR da bakan wucewar haske na foda ɗaya kai tsaye kan juna ba. Ƙa'idar aiki ta biyo bayan buƙatar kundin ƙa'idoji: a kwatanta samfurin da ma'aunin da aka rubuta ta hanya ɗaya, kuma a rubuta hanyar da aka yi amfani da ita. Don fahimtar tushen ilimin sinadaran cation, gishiri, da hydrates da ke bayan waɗannan bakuna, duba bayani kan tsarin shuɗin methylene da halayensa.

Teburin zaɓen hanyar nazari

Wannan tebur kayan zaɓe ne. Karanta kowace jere daga gefe zuwa gefe don gano tambayar da hanyar ke amsawa, abin da sakamakon da ya tsallake gwaji ke tabbatarwa, da abin da bai samu tabbaci ba.

Dalilin da ya sa daidaituwar infrared ba takardar shaidar tsarki ba ce

Daidaituwar gane sinadari tana kawar da yiwuwar rinin da ba daidai ba. Ba ta lissafa duk abin da ke cikin samfurin. Iyakoki guda uku ne suka fi muhimmanci.

Na farko, sinadarai masu kusancin tsari suna kama da juna a infrared. Azure B ya bambanta da shuɗin methylene da rukunin methyl guda ɗaya, don haka bakansa yana kama sosai da na shuɗin methylene. Gaurayen da ke ɗauke da wasu 'yan kaso na Azure B har yanzu zai iya yin daidaito sosai idan an ɗora bakansa kan na ma'aunin shuɗin methylene. Gano wannan ƙazantar aikin chromatography ne, wanda aka tattauna a jagorar ƙazantun shuɗin methylene da hanyoyin gwaji.

Na biyu, nazarin infrared hanya ce da ke duba samfurin gaba ɗaya, amma ƙarfinta na gano abubuwan da suke kaɗan yana da iyaka. Ƙananan adadin rinuka masu alaƙa, ragowar abubuwan narkarwa, ko ragowar sinadaran da ba na halitta ba suna ɓoyuwa ƙarƙashin manyan zanguna. Rashin ƙarin kololuwa shaida ce mai rauni ta rashin ƙazantu.

Na uku, samfurin ma'auni ne ke jagorantar kwatantawar gaba ɗaya. Ma'aunin da ya lalace, wanda kasancewar hydrate ta sauya bakansa, ko wanda aka sarrafa ba daidai ba yana sauya tushen yanke hukunci. Haka ma haɗa hanyoyin gwaji marasa daidaito, kamar kwatanta bakan samfurin ATR da ma'aunin KBr. A rubuta rukunin samarwar ma'aunin, hanyar gwaji, da yadda aka shirya shi tare da kowane hukunci.

Gauraye suna ƙara wani gargaɗi na ƙarshe. Bakan da ya fi yawa ya yi daidai, amma yana da ƙarin kumburi a gefen kololuwa ko ƙarfin alamomi da bai saba ba, ba sakamakon da ya tsallake gwaji ne tare da bayanan ƙasa ba. Alama ce ta cewa a fara rarraba abubuwan samfurin kafin gano su.

Hanyoyin taimako a aikace

HPLC na shuɗin methylene yana bayar da amsar abubuwan da ke cikin samfurin da infrared ba zai iya bayarwa ba. Hanyar da ke cikin kundin ƙa'idoji na yanzu tana amfani da ginshiƙi irin na phenyl tare da gaurayen ruwa da acetonitrile wanda rabonsu ke sauyawa kuma yake ɗauke da trifluoroacetic acid, tana kuma gano sinadarai a 246 nm, ba a zangon hasken da ake gani ba. Ana gane sinadarin ta daidaituwar lokacin riƙewarsa da na samfurin ma'auni; wannan kwatantawar ce kuma ke bayar da adadinsa. Gwajin ƙazantun halitta yana gano Azure B da nasa samfurin ma'auni, da lokacin riƙewa na dangi kusa da 0.8 idan aka kwatanta da shuɗin methylene a 1.0, kuma yana buƙatar babban matakin rarrabewa tsakanin kololuwar biyu. A lura da zaɓin tsawon igiya: jerin sinadaran da aka cire wa methyl yana shan haske a tsawon igiya da ke ƙara matsawa zuwa ja, daga thionine kusa da 600 nm, ta Azure C, Azure A, da Azure B, har zuwa shuɗin methylene kusa da 670 nm. Saboda haka na'urar ganowa da aka saita kusa da 660 nm ba ta amsawa daidai ga dukkan sinadaran jerin ba, kuma tana nuna wasu sinadarai masu kusancin tsari a ƙasa da ainihin adadinsu. Idan ana buƙatar cikakken bayanin jerin gaba ɗaya, ya kamata a yi shi da hanyar C18 LC-MS/MS tare da ingantattun samfuran ma'auni na kowane sinadarin da ake nazarta.

Karkatarwar haske ta foda tana amsa tambayar yanayin daskararru da hanyoyin biyu da ke sama suke lalata bayananta ko watsi da su: narkar da fodar don chromatography yana share bayanan tsarin lu'ulu'u, kuma girgizar ƙwayoyin sinadari tana bayyana haɗe-haɗen sinadari maimakon yadda ƙwayoyin suka jera a faɗin tsarin. Tsarin karkatarwar haske yana bambanta siffofin hydrate da matakin tsarin lu'ulu'u, kuma shuɗin methylene yana buƙatar wannan binciken fiye da yawancin sinadarai. Binciken yanayin daskararru da Rager da abokan aikinsa suka yi ya gano tsarin hydrate biyar dabam-dabam, ciki har da pentahydrate, dihydrate biyu, monohydrate, da hydrate mai matsakaicin adadin ruwa, kuma bai gano ainihin trihydrate a cikin siffofin da aka tantance ba. Yadda ake sarrafa samfurin a dakin gwaje-gwaje yana da muhimmanci a nan: danshi da zafin jiki suna sauya ɗorewar hydrate, kuma niƙa mai tsanani na iya sauya siffarsa ko rage tsarin lu'ulu'unsa, don haka a sarrafa kuma a rubuta danshin dangi da zafin jiki, sannan a rage niƙa gwargwadon yiwuwa. An ƙara tattauna sanya bayanin hydrate a lakabi da tasirinsa kan nauyin da aka auna a siffofin hydrate na shuɗin methylene da bayanan lakabi.

Shayar hasken UV-Vis yana taka rawar taimako. Sanannun kololuwar shayar haske suna tabbatar da halayen ruwan bayani da ake tsammani kuma suna ba da damar auna taron sinadari, amma shuɗin ruwan bayani da ke shan haske a tsawon igiyar da ake tsammani yana dacewa da shuɗin methylene ne ba tare da tabbatar da shi ba, domin rinuka masu alaƙa suna shan haske a kusa.

Abin da za a tambaya kafin saya

A mayar da waɗannan bambance-bambancen zuwa tambayoyin saye. A tambayi wane rukunin samarwa aka gwada, wace hanya ce ta tabbatar da ainihin nau'in sinadari, ko gwajin ƙazantu na HPLC ya yi amfani da samfurin ma'aunin Azure B, da ko an tantance siffar hydrate ko an ɗauka kawai. Fiye da komai, a tambayi ko takardar shaidar ta ƙunshi dukkan ƙa'idojin inganci ko wasu gwaje-gwaje da aka zaɓa kawai. Masu sayarwa da yawa da suke iƙirarin bin kundin ƙa'idoji suna gwada ƙarafa masu nauyi kawai, wanda ke barin tambayoyin ainihin nau'in sinadari, adadinsa, ƙazantun halitta, abubuwan narkarwa, da ƙwayoyin halitta marasa amsa.

Blupreme yana gwada dukkan ƙa'idojin USP, ciki har da ainihin nau'in sinadari, tsarki, ƙazantun halitta, ragowar abubuwan narkarwa, ƙazantun abubuwan sinadarai, ragowar da ke bayan ƙonawa, iyakokin ƙwayoyin halitta, da endotoxins na ƙwayoyin cuta, tare da haɗin gwiwar kamfanin magunguna da ke samar da shuɗin methylene. Ana wallafa takardar shaidar nazari ta kowane rukuni don jama'a a gwajin inganci na Blupreme, don haka ana iya karanta tushen lissafin adadin sinadari da sakamakon ƙazantu kai tsaye maimakon yin hasashe. Har yanzu sakamakon da ke kusa da 100% yana buƙatar bayyana tushen lissafinsa, kamar yadda jagorar adadin sinadari da ya zarce kashi 100 cikin ɗari ta bayyana. Daidaituwar gane sinadari tana buɗe binciken. Cikakken bayanan gwaje-gwaje ne ke kammala shi.