I-Phthalimide Potassium yeTyuwa CAS 1074-82-4 Ubunyulu > 99.0% (HPLC)

3. Indlela yokuvavanya
3.1 Ilahleko ekomisweni (W/W)
3.1.1 Izixhobo kunye nezixhobo
Enye ngaphezulu kwamawaka alishumi ebhalansi ye-elektroniki, i-oveni yombane ye-thermostatic, 40 * 25 ibhotile enobunzima, isomisi
I-Reagent: i-silica gel
3.1.2 Iindlela
1. Coca iibhotile zokukala eziyi-3 40*25.
2, faka kwi-oven kwi-105 ℃ (± 2℃) yomile ngeyure enye.
3. Khupha ibhotile ye-40 * 25 kwaye uyibeke kwi-dryer ukuze ipholile i-30min.
4, Ubunzima obuchanekileyo 40 * 25 ibhotile yokulinganisa engenanto ubunzima W0.
5. Sebenzisa ibhotile yokulinganisa i-40 * 25 ukulinganisa isampuli edibeneyo edibeneyo ye-3.0000g (W1), i-3 iyonke.
6, faka i-oveni, khulula ikepusi yebhotile, uyibeke ecaleni kwebhotile yokulinganisa, okanye uvule isiqingatha sebhotile ukuze yomiswe, khupha, kufuneka ibeyiyo ibhotile yokulinganisa kakuhle, yome kwi-105 ℃ (±2℃) iiyure ezi-3.
7. Thatha ibhotile ye-40 * 25 kwaye uyibeke kwisixhobo sokumisa ukupholisa i-30min.
8, Ubunzima obuchanekileyo emva kokumisa 40 * 25 ubunzima bebhotile W2.
Ifomula yokubala: Ilahleko ekomisweni (%) =(W1-W2)/(W1-W0)×100%
3. 4 Ukuzimisela komxholo
3.4.1 Izixhobo kunye nezixhobo
I-LC-UV100 Liquid Chromatograph (i-Shanghai Wufeng Scientific Instrument Co., LTD.)
I-10ml ibhotile ye-volumetric, i-stainless steel corner spoon kunye nezinye izibonelelo ezinxulumene nazo
3.3.2 Iindlela
Indlela yohlalutyo lweTyuwa yePhthalimide Potassium
3.3.3 Ichromatography elulwelo
Imeko yeChromatographic
Ikholamu yeChromatographic: HypersilC6H5 (C8 iyafumaneka) 4.6*250mm 5um
Ukubona ubude bobude: 210nm
Ubushushu bekholamu: 30℃
Izinga lokuhamba: 1.0ml / min
Isampulu yoxinaniso: 0.05mg/ml (i-diluent sisigaba esihambayo)
Iireagents
I-Potassium Phosphate Dibasic (uhlalutyo olusulungekileyo)
Ityuwa yePotassium yePhthalimide (isampulu eqhelekileyo)
I-acetonitrile (uhlalutyo olusulungekileyo)
Amanzi acocekileyo
Isigaba seselula: i-acetonitrile: i-phosphate buffer (PH: 3.5) =40:60
Ukulinganisa i-1.63g ye-Potassium Phosphate Dibasic kwaye ichithe kwi-600ml yamanzi acocekileyo, lungisa ixabiso le-PH ukuya kwi-3.5 nge-phosphoric acid, uthele kwi-1000ml beaker equkethe i-400ml i-acetonitrile, xuba kakuhle, ukucoca nge-0.45um edibeneyo ye-fiber fibre kunye ne-fiber fibre standby, dissolve ultrasonic membrane isicelo.
3.3.4 Inkqubo
1) Isisombululo sovavanyo loqwalaselo (0.05mg/ml)
Isampuli ye-2.5mg ilinganiswe ngokuchanekileyo kwaye ifakwe kwibhotile ye-volumetric ye-50ml.Isigaba seselula songezwa kwaye sihlanjululwe kwisikali ngokuchithwa kwe-ultrasonic.
2) Isisombululo somgangatho woqwalaselo (1.0mg/ml)
Isampula esiqhelekileyo se-2.5mg silinganiswe ngokuchanekileyo kwaye sifakwe kwibhotile ye-volumetric ye-50ml.Isigaba seselula songezwa kwaye sihlanjululwe kwisikali ngokuchithwa kwe-ultrasonic.
3) Ukusetyenziswa kwenkqubo:
(1) Faka intloko yokucoca kwi-80% ye-methanol ekuqaliseni, vula i-valve yokukhupha kwaye ukhuphe i-3-5min, kwaye uvale i-valve yokukhupha kwaye uhlanza i-10-15min.Emva koko faka intloko yokucoca kwi-90% yamanzi acocekileyo, vula i-valve yokukhupha kwaye ukhuphe i-3-5min, vala i-valve yokukhupha kwaye uhlanza i-10min.
(2) Emva koko utshintshe isigaba seselula esilungisiweyo, izinga lokuhamba ngu-1.0ml / min, uxinzelelo lwangaphambili lwekholomu lungaphantsi kwe-1000Psi, vula i-detector, linda de ikholomu yangaphambili igxininise, vula indawo yokusebenza yekhompyutheni, kwaye ungene kwi-intanethi.
(3) Emva kokuba uxinzelelo lwangaphambili lwekholamu luzinzile, vula i-detector.Okokuqala ujove inaliti ye-1 yesigaba esihambayo, emva koko ujobe inaliti ye-1 yesampuli eqhelekileyo, kwaye ekugqibeleni ujobe isampuli.
(4) Iziphumo zokubala: indlela yokulungelelanisa indawo
(5) Emva kokugqiba umsebenzi wokuhlalutya, vala i-detector kuqala, uze uhlambe intloko yokucoca emanzini ahlambulukileyo kwi-10-15min;Ngelo xesha, i-valve yokutofa yahlanjululwa ngamanzi kunye ne-methanol.
(6) Ekugqibeleni, faka i-80% ye-methanol, uhlambulule i-30min, kwaye uvale.
4. Emva kokugqitywa kokuhlolwa, gcwalisa iphepha lokuhlola kunye nelebhu.