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

Iinkqubo zokuhlola
1. Imbonakalo
-- Ukuhlolwa okubonakalayo
2. Ubunyulu (HPLC)
2.1 Isixhobo
Ukusebenza okuphezulu kwechromatography yolwelo, umtshina wePDA.
Ibhalansi yohlalutyo lwe-elektroniki
2.2 I-Reagent
I-Acetonitrile (ibakala le-chromatographic), i-trifluoroacetic acid (ibakala le-chromatographic)
2.3 Iimeko zeChromatographic
2.3.1 Umhlathi: YMC-ODS-AM, 5 μl, 250x4.6 mm
2.3.2 Ubungakanani bewavenge: INC220nm
Izinga lokuhamba: 1.0mL / min
Ubungakanani besampulu:10 μl (isalathisi)
Ukunciphisa: i-acetonitrile
Ixesha lokuqokelela idatha: 25.00min
2.4 Ukulungiswa kwesigaba esiphathwayo
Isigaba se-Mobile A (i-0.1% yamanzi e-trifluoroacetic acid): ukuxutywa ngokuchanekileyo 2. Nciphisa i-Oml trifluoroacetic acid ngamanzi ukuya kwi-2000m1, xuba kakuhle, kunye ne-degassing;
I-Mobile phase B (0.1% i-acetonitrile trifluoroacetic acid): i-absorption echanekileyo 2.0ml i-trifluoroacetic acid yahlanjululwa kwi-2000m1 nge-acetonitrile, ixutywe kunye ne-degassing;
2.5 Iprogram yegradient yesigaba esihambayo
Ixesha (umzu) A% B%
0.00 90 10
13.00 10 90
18.00 10 90
18.01 90 10
23.00 90 10
2.6 Ukulungiswa kwesisombululo sesampuli
Ubunzima kwaye uchithe isampuli ye-0.1g kunye ne-acetonitrile kwaye udibanise kwi-100ml, xubha kakuhle ukusetyenziswa, okanye ugxininiso olufanayo.Lungiselela iisampuli ezimbini ngokuhambelanayo.
2.7 Ukumiselwa kweSampuli
Hlalutya isampuli ngokwenkqubo yesampulu ilandelayo:
Ngaphezulu kwesitofu esinye sesisombululo esingenanto
1 isititshi isisombululo sesampulu 1#
1 isititshi isisombululo sesampulu 2#
2.8 Ubalo lweziphumo
2.8.1 Indlela yokulinganisa indawo eyincopho yasetyenziselwa ukubala ukucoceka kweHPLC ngokutsala indawo engenanto.
2.8.2 Uphambuko olunxulumene nococeko lweenaliti ezimbini aluyi kuba lukhulu kune-1%
2.8.3 Ukuba iziphumo zazo zombini iinaliti ziyahlangabezana nemilinganiselo yokwamkelwa, ucoceko oluqhelekileyo luthathwa njengesiphumo sokugqibela.
3, Indawo yokunyibilika -- RY-1 isixhobo sendawo yokunyibilika
4. Ilahleko kwindlela yokubona ukomisa
4.1 Izixhobo:
I-oven yokumisa i-thermostatic yombane, enye kwi-balance yamawaka alishumi.
4.2 Inkqubo:
Kwibhotile yokulinganisa i-flat kunye nekhava yomlomo womhlaba kunye nobunzima obuqhubekayo kunye nokumisa ngokugqithiseleyo, ulinganise i-1 gram yesampuli (echanekileyo kwi-0.0001 gram).Isampulu kufuneka isasazwe ngokulinganayo emazantsi ebhotile yokulinganisa ngobunzima obungekho ngaphezu kwe-10mm, ifakwe kwi-oven yokushisa yombane eqhubekayo, yome kwi-105-110 ℃ iiyure ezi-3, emva koko ungene kwigumbi lokumisa, upholile. kwiqondo lobushushu begumbi kunye nobunzima.
Ukubala: Ukuncipha kobunzima %= (M1-M2) ÷M×100
Apho: M1: ubunzima besampulu kunye nebhotile yokuwayisha phambi kokuba yomiswe, g
M2: Ubunzima besampulu kunye nebhotile yokulinganisa emva kokumiswa, g
M: Ubunzima besampulu, igram
5. Ukujikeleza okuthe ngqo
-- Ukujikeleza okuthe ngqo kulinganiswa ngokuhambelana ne-GB/T613-1988
Ukulungiswa kwesampuli: i-0.5000g yesampuli ilinganiswe ngokuchanekileyo kwaye idluliselwe kwibhotile ecocekileyo neyomileyo ye-50ml ye-volumetric kunye ne-20ml ye-Ethyl acetate.Ibhotile yayibotshelelwe yaza yashukunyiswa ukunyibilikisa i-acetate ye-Ethyl.
Uvavanyo: Lungisa i-zero ye-gyroscope ngaphambi kovavanyo, uze ugcwalise ityhubhu yokuvavanya ngesisombululo sesampuli, urekhode i-Angle yokuphambuka yokujikeleza, kwaye ubale ukujikeleza okuthe ngqo kwesampuli usebenzisa le fomula ilandelayo.
[α]20/D= (r×50) ÷(L×W)
Apho:
[α]20 / D: Ukujikeleza okuthe ngqo kwesisombululo sesampuli kwi-25℃
r: Ukujikeleza kubonwe kwi-25 ℃ kwisisombululo sesampuli
50: Lungiselela umthamo wesisombululo sesampuli (ml)
w: Ubunzima besampulu (g)
L: Ubude betyhubhu yokubona (dm)
6. Uhlalutyo lwe-TCL
Ukulungiswa kwesampuli: isampuli ye-0.5000g ilinganiswe ngokuchanekileyo kwaye ihanjiswe kwibhotile ye-volumetric ecocekileyo neyomileyo ye-50ml, i-40ml EtoH yongezwa, ibhotile yayifakwe i-capped kwaye ishukunyiswe ukuchithwa, kwaye emva koko ihlanjululwe kwisikali nge-EtoH.
Ukulungiswa kwesampulu yokulawula: isampuli ye-0.5000g ilinganiswe ngokuchanekileyo kwaye ihanjiswe kwibhotile ye-volumetric ecocekileyo neyomileyo ye-50ml, amanzi angama-40ml kunye namaconsi e-2 e-6N hydrochloric acid yongezwa, ibhotile yayifakwe i-capped kwaye ishukunyiswe ukuba inyibilike, kwaye emva koko ihlanjululwe kwisikali kunye amanzi.Emva koko thatha i-0.5 yolwelo olungentla kwaye uhlambulule nge-ethanol kwibhotile yevolumu ye-100ml kwisampulu yereferensi kunye ne-1.0% yesikali se-amino acid eseleyo.
Iisampuli ze-microliter ze-10 zithathwe nge-syringe ye-microsampling, kwaye iisampuli zafakwa kwi-plate ye-silicone ye-GF254.I-5 microliter, i-microliter eyi-10 kunye ne-15 i-microliter point plate ithathwe ngamanqaku okuthelekisa, ngokulandelanayo.
I-arhente yokuphuhlisa: i-n-butanol: i-acetic acid ye-glacial: amanzi = 4: 1: 1.
I-arhente yokuphuhlisa umbala: 5% isisombululo se-ninhydrin methanol.
Umsebenzi wokuphuhlisa umbala: okokuqala, sebenzisa isomisi seenwele ukomisa i-silica gel plate ephuhlisiweyo, emva koko uyidibanise kwi-5% yesisombululo se-ninhydrin methanol, emva koko uvuthuze, kwaye ubhake kwiqondo lokushisa eliphezulu kwisithando sombane sophuhliso lombala.
Isigwebo: Jonga ixesha lombala wemveliso, ubungakanani bebala, ukugxilwa kombala kunye nokuthelekisa kunye nemveliso yokulawula, gweba ukuba ikuloo luhlu.