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

Izinqubo zokuhlola
1. Ukubukeka
-- Ukuhlola okubonakalayo
2. Ubumsulwa (HPLC)
2.1 Ithuluzi
Ukusebenza okuphezulu kwe-chromatography ye-liquid, umtshina we-PDA.
Ibhalansi yokuhlaziya ye-elekthronikhi
2.2 I-Reagent
I-Acetonitrile (ibanga le-chromatographic), i-trifluoroacetic acid (ibanga le-chromatographic)
2.3 Izimo zeChromatographic
2.3.1 Ikholomu: YMC-ODS-AM, 5 μl, 250x4.6 mm
2.3.2 Ubude begagasi bokutholwa: INC220nm
Izinga lokugeleza: 1.0mL/min
Usayizi wesampula: 10 μl (inkomba)
I-Diluent: i-acetonitrile
Isikhathi sokuqoqwa kwedatha: 25.00min
2.4 Ukulungiselela isigaba sikamakhalekhukhwini
Isigaba seselula A (0.1% samanzi e-trifluoroacetic acid): ukumuncwa okunembayo 2. Nciphisa i-Oml trifluoroacetic acid ngamanzi ukuya ku-2000m1, hlanganisa kahle, futhi ukhiphe umoya;
Isigaba seselula B (0.1% i-acetonitrile trifluoroacetic acid): ukumuncwa okunembile okungu-2.0ml i-trifluoroacetic acid kuhlanjululwe ku-2000m1 nge-acetonitrile, exutshwe kanye ne-degassing;
2.5 Uhlelo lwe-Gradient lwesigaba seselula
Isikhathi (amaminithi) 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 kwesixazululo sesampula
Kala bese uncibilikisa isampula engu-0.1g nge-acetonitrile bese uncibilikisa ibe ngu-100ml, xukuza kahle ukuze uyisebenzise, ​​noma ukugxila okufanayo.Lungiselela amasampula amabili ngokuhambisana.
2.7 Ukunqunywa kwesampula
Hlaziya isampula ngokuya ngenqubo yamasampula elandelayo:
Umjovo ongaphezu ko-1 wesixazululo esingenalutho
Isixazululo sesampula somthungo ongu-1 1#
Isampula yomthungo engu-1 2#
2.8 Ukubalwa kwemiphumela
2.8.1 Indlela yokujwayela yendawo ephakemeyo yasetshenziswa ukubala ubumsulwa be-HPLC ngokudonsa indawo engenalutho.
2.8.2 Isilinganiso sokuchezuka kokuhlanzeka kwezinaliti ezimbili akufanele sibe ngaphezu kuka-1%
2.8.3 Uma imiphumela yayo yomibili imijovo ihlangabezana nemibandela yokwamukelwa, ukuhlanzeka okumaphakathi kuthathwa njengomphumela wokugcina.
3, Indawo encibilikayo -- RY-1 ithuluzi lokuncibilika
4. Ukulahleka kwendlela yokuthola ukomisa
4.1 Izinsimbi:
Ihhavini yokomisa i-thermostatic kagesi, ibhalansi eyodwa ezinkulungwaneni eziyishumi.
4.2 Inqubo:
Ebhodleleni lesisindo esiyisicaba elinesembozo somlomo ophansi esinesisindo esingaguquki kanye nokomisa ngokweqile, kala i-1 gram yesampula (enembile ukuya ku-0.0001 gram).Isampula kufanele isakazwe ngokulinganayo ngaphansi kwebhodlela lesisindo ngogqinsi olungekho ngaphezu kuka-10mm, ifakwe kuhhavini omisiwe kagesi oshisa njalo, yome ku-105-110 ℃ amahora angu-3, ​​bese ingena ekamelweni lokumisa, ipholile. ekamelweni lokushisa kanye nesisindo.
Ukubala: Ukuncipha kwesisindo okomile %= (M1-M2) ÷M×100
Kuphi: M1: Inqwaba yesampula nebhodlela lesisindo ngaphambi kokoma, g
I-M2: Inqwaba yesampula nebhodlela lesisindo ngemva kokoma, g
M: Isisindo sesampula, igremu
5. Ukujikeleza okuqondile
-- Ukuzungeza okuqondile kukalwa ngokuhambisana ne-GB/T613-1988
Ukulungiswa kwesampula: I-0.5000g yesampula yakala ngokunembile futhi yadluliselwa ebhodleleni le-volumetric engu-50ml ehlanzekile neyomile ene-20ml Ethyl acetate.Ibhodlela lalifakwe ukhokho futhi lanyakaziswa ukuze kuncibilike i-Ethyl acetate.
Isivivinyo: Lungisa uziro we-gyroscope ngaphambi kokuhlolwa, bese ugcwalisa ithubhu lokuhlola ngesixazululo sesampula, urekhode i-engeli yokuchezuka yokuzungezisa, futhi ubale ukuzungezisa okuthile kwesampula usebenzisa ifomula elandelayo.
[α]20/D= (r×50) ÷(L×W)
Kuphi:
[α]20/D: Ukuzungezisa okuqondile kwesixazululo sesampula ku-25℃
r: Ukuzungezisa kubonwe ku-25℃ ukuthola isisombululo sesampula
50: Lungiselela umthamo wesixazululo sesampula (ml)
w: Isisindo sesampula (g)
L: Ubude beshubhu yokubuka (dm)
6. Ukuhlaziywa kwe-TCL
Ukulungiswa kwesampula: isampula ye-0.5000g yakalwa ngokunembile futhi yayiswa ebhodleleni le-volumetric elingu-50ml elihlanzekile nelomile, i-40ml EtoH yengezwa, ibhodlela lavalwa futhi lanyakaziswa ukuze lincibilike, lase lihlanjululwa esikalini nge-EtoH.
Ukulungiswa kwesampula yokulawula: isampula ye-0.5000g yalinganiswa ngokunembile futhi yayiswa ebhodleleni levolumu ye-50ml ehlanzekile neyomile, amanzi angu-40ml kanye namaconsi angu-2 we-6N hydrochloric acid angeziwe, ibhodlela lalimbozwa futhi lanyakaziswa ukuze lincibilike, bese lihlanjululwa esikalini. amanzi.Bese uthatha u-0.5 walolu ketshezi olungenhla futhi uluhlambulule nge-ethanol ebhodleleni levolumu engu-100ml uye kusampula yereferensi ene-1.0% yesikali sensalela ye-amino acid.
Amasampula ama-microliter ayi-10 athathwe ngesirinji encane yesampling, futhi amasampuli abekwa epuleti le-silicone le-GF254.5 microliter, 10 microliter kanye 15 microliter amaphuzu amapuleti athathwe ukuze kuqhathaniswe amaphuzu, ngokulandelana.
I-ejenti yokuthuthukisa: n-butanol: i-glacial acetic acid: amanzi =4:1:1.
I-ejenti ethuthukisa umbala: isixazululo se-ninhydrin methanol esingu-5%.
Ukusebenza kokuthuthukiswa kombala: okokuqala, sebenzisa isomisi sezinwele ukuze usule ipuleti yejeli ye-silica ethuthukisiwe, bese uyicwilisa ku-5% isixazululo se-ninhydrin methanol, bese uphefumula, bese ubhaka ekushiseni okuphezulu esithandweni sikagesi sokuthuthukiswa kombala.
Ukwahlulela: Bheka isikhathi sombala womkhiqizo, usayizi wendawo, ukugxila kombala kanye nokuqhathanisa nomkhiqizo olawulayo, yahlulela ukuthi ukulolo hlu.