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

Kuongorora maitiro
1. Chitarisiko
-- Visual kuongorora
2. Kuchena (HPLC)
2.1 Chiridzwa
Yakakwira performance liquid chromatography, PDA detector.
Electronic analytical balance
2.2 Reagent
Acetonitrile (chromatographic giredhi), trifluoroacetic acid (chromatographic giredhi)
2.3 Chromatographic mamiriro
2.3.1 Koramu: YMC-ODS-AM, 5 μl, 250x4.6 mm
2.3.2 Kuona wavelength: INC220nm
Kuyerera kweyero: 1.0mL/min
Saizi yemuenzaniso: 10 μl (referensi)
Diluent: acetonitrile
Nguva yekuunganidza data: 25.00min
2.4 Kugadzirira kwechikamu chenhare
Nharembozha chikamu A (0.1% trifluoroacetic acid mvura): kunyatsotora 2. Dilute Oml trifluoroacetic acid nemvura kusvika 2000m1, sanganisa zvakanaka, uye degassing;
Nharembozha chikamu B (0.1% acetonitrile trifluoroacetic acid): kunyatsotora 2.0ml trifluoroacetic acid yakaderedzwa kusvika 2000m1 neacetonitrile, yakasanganiswa uye degassing;
2.5 Gradient chirongwa che mobile phase
Nguva (miniti) A% B%
0.00 90 10
13.00 10 90
18.00 10 90
18.01 90 10
23.00 90 10
2.6 Kugadzirira kwemuenzaniso mhinduro
Weresa uye nyungudutsa 0.1g sampuli ine acetonitrile uye dilute kusvika ku100ml, zunza zvakanaka kuti ushandiswe, kana iwo iwo mafungidziro akafanana.Gadzirira sampuli mbiri dzakafanana.
2.7 Sample Kutsunga
Ongorora sampuli maererano neanotevera sampling maitiro:
Kupfuura jekiseni 1 remhinduro isina chinhu
1 musono muenzaniso mhinduro 1#
1 musono muenzaniso mhinduro 2#
2.8 Mhedzisiro kuverenga
2.8.1 Peak area normalization nzira yakashandiswa kuverenga kuchena kweHPLC nekubvisa nzvimbo isina chinhu.
2.8.2 Iyo hama inoreva kutsauka kwekuchena kwetsono mbiri haifaniri kudarika 1%
2.8.3 Kana mhedzisiro yemajekiseni ese ari maviri akazadzisa maitiro ekugamuchirwa, avhareji yekuchena inotorwa semhedzisiro yekupedzisira.
3, Melting point -- RY-1 melting point chiridzwa
4. Kurasikirwa pakuomeswa kwekuona nzira
4.1 Zviridzwa:
Electric thermostatic drying oven, imwe muzviuru gumi pasara.
4.2 Maitiro:
Mubhodhoro rehuremu rakatsetseka rine chifukidziro chevhu chevhu ne uremu hunogara huripo uye kunyanya kuomesa, kuyera 1 gramu yemuenzaniso (yakarurama kusvika 0.0001 gramu).Sample inofanira kuparadzirwa zvakaenzana pazasi pebhodhoro rekuyeresa nehupamhi husingapfuuri 10mm, isa muhovhoni yekuomesa yemagetsi, yakaoma pa105-110 ℃ kwemaawa matatu, uye wozopinda muimba yekuomesa, inotonhorera. kusvika kukamuri tembiricha uye kuyera.
Kuverenga: Dry uremu kurasikirwa %= (M1-M2) ÷M×100
Kupi: M1: uwandu hwesample uye bhodhoro rekuyeresa risati raoma, g
M2: Misa yemuenzaniso uye bhodhoro rekuyera mushure mekuoma, g
M: Sample mass, giramu
5. Kutenderera chaiko
-- Kutenderera chaiko kunoyerwa zvinoenderana neGB/T613-1988
Kugadzirira kwemuenzaniso: 0.5000g yemuenzaniso yakayerwa zvakarurama uye yakaendeswa kune yakachena uye yakaoma 50ml volumetric bhodhoro ne 20ml Ethyl acetate.Bhodhoro rakanga rakakoshwa uye rakazunguzirwa kunyungudutsa iyo Ethyl acetate.
Muedzo: Gadzirisa zero yegyroscope isati yaedzwa, wobva wazadza chubhu yebvunzo nemhinduro yemuenzaniso, rekodha deflection Angle yekutenderera, uye verenga kutenderera chaiko kwemuenzaniso uchishandisa fomura rinotevera.
[α]20/D= (r×50) ÷(L×W)
Kupi:
[α] 20 / D: Kutenderera kwakananga kwemuenzaniso mhinduro pa25 ℃
r: Kutenderera kunoonekwa pa25 ℃ yemuenzaniso mhinduro
50: Gadzirira chiyero chemhinduro yemuenzaniso (ml)
w: uremu hwemuenzaniso (g)
L: Optical chubhu kureba (dm)
6. TCL Analysis
Kugadzirira kwemuenzaniso: 0.5000g sampuli yakayerwa zvakarurama uye yakaendeswa kune yakachena uye yakaoma 50ml volumetric bhodhoro, 40ml EtoH yakawedzerwa, bhodhoro rakavharwa uye rakazununguswa kuti rinyunguduke, ndokuzoderedzwa kusvika pachiyero neEtoH.
Kugadzirira kwekutonga sampuli: 0.5000g sampu yakayerwa nemazvo uye yakaendeswa kune yakachena uye yakaoma 50ml volumetric bhodhoro, 40ml mvura uye 2 madonhwe e6N hydrochloric acid akawedzerwa, bhodhoro rakavharwa uye rakazununguswa kuti rinyunguduke, ndokuzoderedzwa kusvika pachiyero ne mvura.Wobva watora 0.5 yemvura iri pamusoro woikanya ne ethanol mubhodhoro revhoriyamu 100ml kune referensi sampuli ine 1.0% amino acid yasara sikero.
10 microliter samples dzakatorwa neine microsampling sirinji, uye samples dzakaiswa paGF254 silicone plate.5 microliter, 10 microliter uye 15 microliter point plates dzakatorwa kuti dzienzanise pfungwa, maererano.
Developing agent: n-butanol: glacial acetic acid: mvura =4:1:1.
Ruvara runovandudza mumiriri: 5% ninhydrin methanol mhinduro.
Mashandiro ekuvandudza ruvara: kutanga, shandisa chinoomesa bvudzi kuomesa silika gel plate, wozoinyika mu5% ninhydrin methanol solution, wobva wafuridza, uye bika nekupisa kwakanyanya muchoto chemagetsi chekuvandudza ruvara.
Kutonga: Tarisai panguva yechigadzirwa cheruvara, saizi yevara, kusungirirwa kwemavara uye kuenzanisa nechigadzirwa chekutonga, tongai kuti chiri muchikamu ichocho.