Fmoc-Ser(tBu)-OH CAS 71989-33-8 Fmoc-O-tert-Butyl-L-Serine Purity>98.5% (HPLC)

Njira zoyendera
1. Maonekedwe
-- Kuwunika kowoneka
2. Purity (HPLC)
2.1 Chida
High performance liquid chromatography, PDA chowunikira.
Electronic analytical balance
2.2 Reagent
Acetonitrile (chromatographic grade), trifluoroacetic acid (chromatographic grade)
2.3 Mikhalidwe ya Chromatographic
2.3.1 Mzere: YMC-ODS-AM, 5 μl, 250x4.6 mm
2.3.2 Kutalika kwa mawonekedwe: INC220nm
Kuthamanga: 1.0mL / min
Kukula kwachitsanzo: 10 μl (reference)
Zosakaniza: acetonitrile
Nthawi yosonkhanitsa deta: 25.00min
2.4 Kukonzekera gawo la mafoni
Mobile gawo A (0.1% trifluoroacetic acid madzi): mwatsatanetsatane mayamwidwe 2. Sungunulani Oml trifluoroacetic asidi ndi madzi 2000m1, sakanizani bwino, ndi degassing;
Mobile gawo B (0.1% acetonitrile trifluoroacetic acid): yeniyeni mayamwidwe 2.0ml trifluoroacetic asidi anali kuchepetsedwa kuti 2000m1 ndi acetonitrile, wosakaniza ndi degassing;
Pulogalamu ya 2.5 Gradient ya gawo la mafoni
Nthawi (mphindi) A% B%
0.00 90 10
13.00 10 90
18.00 10 90
18.01 90 10
23.00 90 10
2.6 Kukonzekera chitsanzo cha yankho
Yesani ndi kusungunula chitsanzo cha 0.1g ndi acetonitrile ndi kuchepetsa mpaka 100ml, gwedezani bwino kuti mugwiritse ntchito, kapena ndende yomweyo.Konzani zitsanzo ziwiri zofanana.
2.7 Kutsimikiza Kwachitsanzo
Sankhulani chitsanzocho motsatira njira zotsatirazi:
Kupitilira 1 jekeseni wopanda kanthu
1 Stitch chitsanzo yankho 1#
1 Stitch chitsanzo yankho 2#
2.8 Kuwerengera zotsatira
2.8.1 Njira yokhazikika yamalo okhazikika idagwiritsidwa ntchito kuwerengera chiyero cha HPLC pochotsa malo opanda kanthu.
2.8.2 Chibale chikutanthauza kupatuka kwa chiyero cha singano ziwiri sikuyenera kukhala wamkulu kuposa 1%
2.8.3 Ngati zotsatira za majekeseni onsewa zikugwirizana ndi zovomerezeka, chiyero chapakati chimatengedwa ngati chotsatira chomaliza.
3, Malo osungunuka -- RY-1 chida chosungunuka
4. Kutaya pa kuyanika njira kuzindikira
4.1 Zida:
Magetsi thermostatic kuyanika uvuni, chimodzi mwa zikwi khumi bwino.
4.2 Ndondomeko:
Mu botolo lathyathyathya lokhala ndi chivundikiro chapansi pakamwa ndi kulemera kosalekeza ndi kuyanika mopitirira muyeso, yezani 1 gramu ya zitsanzo (zolondola mpaka 0.0001 gramu).Zitsanzo ziyenera kufalikira pansi pa botolo lolemera ndi makulidwe osapitirira 10mm, kuyika mu uvuni woyanika nthawi zonse, wouma pa 105-110 ℃ kwa maola atatu, kenako ndikulowa m'chipinda chowumitsira, ozizira. kutentha kwa chipinda ndi kulemera.
Kuwerengera: Kutaya kuwonda %= (M1-M2) ÷M×100
Kumene: M1: kuchuluka kwa zitsanzo ndi botolo loyezera lisanawumitsidwe, g
M2: Unyinji wa zitsanzo ndi botolo loyezera pambuyo poyanika, g
M: Zitsanzo za kulemera, gramu
5. Kuzungulira kwachindunji
-- Kuzungulira kwachindunji kumayesedwa molingana ndi GB/T613-1988
Kukonzekera kwachitsanzo: 0.5000g ya chitsanzo inayesedwa molondola ndikusamutsidwa ku botolo loyera ndi louma la 50ml volumetric ndi 20ml Ethyl acetate.Botolo lidakhomeredwa ndikugwedezeka kuti lisungunuke Ethyl acetate.
Mayeso: Sinthani ziro ya gyroscope mayeso asanayesedwe, kenako lembani chubu choyesera ndi yankho lachitsanzo, lembani njira yosinthira yozungulira, ndikuwerengera kuzungulira kwachitsanzo pogwiritsa ntchito njira iyi.
[α]20/D= (r×50) ÷(L×W)
Kumene:
[α] 20/D: Kusinthasintha kwachindunji kwa yankho lachitsanzo pa 25 ℃
R: Kuzungulira komwe kumawonedwa pa 25 ℃ kuti mupeze yankho lachitsanzo
50: Konzani voliyumu ya yankho lachitsanzo (ml)
w: kulemera kwachitsanzo (g)
L: Kutalika kwa chubu (dm)
6. Kusanthula kwa TCL
Kukonzekera kwachitsanzo: chitsanzo cha 0.5000g chinayesedwa molondola ndikusunthira ku botolo loyera ndi louma la 50ml volumetric, 40ml EtoH inawonjezeredwa, botolo linatsekedwa ndikugwedezeka kuti lisungunuke, ndiyeno limachepetsedwa ku sikelo ndi EtoH.
Kukonzekera kwa chitsanzo chowongolera: 0.5000g chitsanzo chinayesedwa bwino ndikusunthira ku botolo laukhondo ndi louma la 50ml volumetric, madzi 40ml ndi madontho 2 a 6N hydrochloric acid anawonjezeredwa, botolo linatsekedwa ndikugwedezeka kuti lisungunuke, ndiyeno kuchepetsedwa ku sikelo ndi madzi.Ndiye kutenga 0,5 wa pamwamba madzi ndi kuchepetsa ndi Mowa mu 100ml voliyumu botolo kuti Buku chitsanzo ndi 1.0% amino asidi zotsalira sikelo.
Zitsanzo za 10 za microliter zinatengedwa ndi syringe ya microsampling, ndipo zitsanzozo zinayikidwa pa mbale ya GF254 silikoni.5 microliter, 10 microliter ndi 15 microliter point plates anatengedwa kuti afananize mfundo, motero.
Wopanga: n-butanol: glacial acetic acid: madzi =4:1:1.
Wopanga utoto: 5% yankho la ninhydrin methanol.
Ntchito yokulitsa utoto: choyamba, gwiritsani ntchito chowumitsira tsitsi kuti muumitse mbale ya silika yopangidwa ndi gel osakaniza, kenaka muyiwike mu 5% ninhydrin methanol solution, kenako muwume, ndikuwotcha kutentha kwambiri mu ng'anjo yamagetsi kuti mupange utoto.
Chiweruzo: Yang'anani pa nthawi ya mtundu wa mankhwala, kukula kwa malo, ndende ya mtundu ndi kufananiza ndi mankhwala olamulira, weruzani kuti ali mumtundu umenewo.