I-Phthalimide Potassium Salt CAS 1074-82-4 Ukuhlanzeka >99.0% (HPLC)

3. Indlela yokuhlola
3.1 Ukulahlekelwa Ekumisweni (W/W)
3.1.1 Izimpahla namathuluzi
Ibhalansi ye-elekthronikhi engaphezu kwezinkulungwane eziyishumi, ihhavini yokomisa i-thermostatic kagesi, ibhodlela lesisindo esingu-40*25, isomisi
I-Reagent: i-silica gel
3.1.2 Izindlela
1. Hlanza amabhodlela anesisindo angu-3 40*25.
2, faka kuhhavini eku-105℃ (±2℃) yomile ihora elingu-1.
3. Khipha ibhodlela lokukala elingu-40*25 ulifake ekomeni ukuze liphole imizuzu engu-30.
4, Isisindo esinembile 40*25 ibhodlela lokulinganisa elingenalutho isisindo W0.
5. Sebenzisa ibhodlela lesisindo elingu-40*25 ukuze ukale isampula elixutshwe ngokulinganayo lika-3.0000g (W1), okuyisamba esingu-3.
6, Faka kuhhavini, khumula isivalo sebhodlela, usibeke eduze kwebhodlela lokukala, noma uvule uhhafu isivalo sebhodlela ukuze somiswe, khipha, kufanele sibe nesisindo esihle sebhodlela, lome ku-105℃ (±2℃) ukuze 3 amahora.
7. Khipha ibhodlela lokukala elingu-40*25 ulifake emshinini wokomisa ukuze liphole imizuzu engama-30.
8, Isisindo esinembile ngemva kokumisa 40*25 isisindo sebhodlela W2.
Ifomula yokubala: Ukulahlekelwa Ekomisweni (%) =(W1-W2)/(W1-W0)×100%
3. 4 Ukuzimisela kokuqukethwe
3.4.1 Amathuluzi nezinto zokusebenza
I-LC-UV100 Liquid Chromatograph (Shanghai Wufeng Scientific Instrument Co., LTD.)
10ml ibhodlela levolumu, isipuni sekhoneni lensimbi engagqwali nezinye izinsiza ezihlobene
3.3.2 Izindlela
Indlela yokuhlaziya i-Phthalimide Potassium Salt
3.3.3 Ichromatography ewuketshezi
Isimo seChromatographic
Ikholomu yeChromatographic: HypersilC6H5 (C8 iyatholakala futhi) 4.6*250mm 5um
Ubude begagasi bokutholwa: 210nm
Izinga lokushisa lekholomu: 30℃
Izinga lokugeleza: 1.0ml/min
Ukugxiliswa kwesampula: 0.05mg/ml (i-diluent yisigaba seselula)
Ama-reagents
I-Potassium Phosphate Dibasic (i-analytical pure)
I-Phthalimide Potassium Salt (isampula evamile)
I-Acetonitrile (i-analytical pure)
Amanzi ahlanzekile
Isigaba seselula: i-acetonitrile: i-phosphate buffer (PH:3.5) =40:60
Kala i-1.63g ye-Potassium Phosphate Dibasic bese uncibilikisa emanzini ahlanzekile angu-600ml, lungisa inani le-PH libe ngu-3.5 nge-phosphoric acid, uthele ku-1000ml beaker equkethe i-acetonitrile engu-400ml, hlanganisa kahle, ukuhlunga nge-0.45um exutshwe i-fiber filter kanye ne-vibve isicelo.
3.3.4 Inqubo
1) Isixazululo sokuhlolwa kokucushwa (0.05mg/ml)
Isampula engu-2.5mg ikalwe ngokunembile futhi yafakwa ebhodleleni levolumu engu-50ml.Isigaba seselula sengezwe futhi sahlanjululwa esikalini ngokuqedwa kwe-ultrasonic.
2) Isixazululo esijwayelekile sokucushwa (1.0mg/ml)
Isampula elijwayelekile elingu-2.5mg likalwe ngokunembile lafakwa ebhodleleni levolumu engu-50ml.Isigaba seselula sengezwe futhi sahlanjululwa esikalini ngokuqedwa kwe-ultrasonic.
3) Ukusebenziseka kwesistimu:
(1) Faka ikhanda lesihlungi ku-80% methanol ekuqaleni, vula i-valve yokukhipha umoya bese ukhipha i-3-5min, bese uvala i-valve yokukhipha bese uhlanza i-10-15min.Bese ufaka ikhanda lokuhlunga emanzini ahlanzekile angu-90%, vula i-valve yokukhipha amanzi bese ukhipha i-3-5min, vala i-valve yokukhipha bese uhlanza i-10min.
(2) Bese ushintsha isigaba seselula esilungisiwe, izinga lokugeleza ngu-1.0ml/min, ingcindezi yangaphambili yekholomu ingaphansi kuka-1000Psi, vula umtshina, linda kuze kube yilapho umfutho wangaphambili wekholomu uzinzile, vula indawo yokusebenza yekhompyutha, bese ungena ku-inthanethi.
(3) Ngemuva kokuthi umfutho wangaphambili wekholomu uzinzile, vula umtshina.Qala ngokujova inaliti engu-1 yesigaba seselula, bese ujova inaliti engu-1 yesampula evamile, bese ujova isampula.
(4) Imiphumela yokubala: indlela yokujwayela yendawo
(5) Ngemva kokuqeda umsebenzi wokuhlaziya, vala umtshina kuqala, bese uhlanza ikhanda lokuhlunga emanzini ahlanzekile 10-15min;Ngesikhathi esifanayo, i-valve yomjovo yayihlanjululwa ngamanzi ne-methanol.
(6) Ekugcineni, gqoka i-methanol engu-80%, hlambulula imizuzu engama-30, bese uvala.
4. Ngemva kokuphothula ukuhlola, gcwalisa ishidi lokuhlola nelabhorethri.