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

Usoro nyocha
1. Ọdịdị
-- Nlele anya
2. Ịdị ọcha (HPLC)
2.1 Ngwa
chromatography mmiri mmiri na-arụ ọrụ dị elu, ihe nchọpụta PDA.
Ntụle nyocha eletrọnịkị
2.2 Reagent
Acetonitrile (ọkwa chromatographic), trifluoroacetic acid (ọkwa chromatographic)
2.3 Ọnọdụ chromatographic
2.3.1 Ogidi: YMC-ODS-AM, 5 μl, 250x4.6 mm
2.3.2 Ogologo nchọta: INC220nm
Onu ogugu: 1.0ml/min
Nlele nha: 10 μl (ntụaka)
Ihe ngwọta: acetonitrile
Oge nchịkọta data: 25.00min
2.4 Mobile usoro nkwadebe
Usoro mkpanaka A (0.1% mmiri trifluoroacetic acid): nnabata ziri ezi 2. Dilute Oml trifluoroacetic acid na mmiri na 2000m1, jikọta nke ọma, na degassing;
Usoro mkpanaaka B (0.1% acetonitrile trifluoroacetic acid): absorption 2.0ml trifluoroacetic acid ziri ezi ka 2000m1 na acetonitrile, agwakọta na degassing;
2.5 mmemme gradient nke usoro mkpanaka
Oge (nkeji) A% B%
0.00 90 10
13.00 10 90
18.00 10 90
18.01 90 10
23.00 90 10
2.6 Nkwadebe nke ngwọta sample
Tụnye na igbari 0.1g sample na acetonitrile na itughari ka 100ml, maa jijiji nke ọma maka ojiji, ma ọ bụ otu itinye uche.Kwadebe ihe atụ abụọ n'otu aka ahụ.
2.7 Nnwale mkpebi
Nyochaa ihe nlele ahụ dịka usoro nlele ndị a si dị:
Ihe kariri ogwu ogwu efu 1
1 stitch sample ngwọta 1 #
1 stitch sample ngwọta 2#
2.8 Ngụkọta nsonaazụ
2.8.1 A na-eji usoro nhazi nke mpaghara kacha elu iji gbakọọ ịdị ọcha HPLC site n'iwepụ oghere oghere.
2.8.2 Ntugharị ikwu nke ịdị ọcha nke agịga abụọ agaghị adị karịa 1%
2.8.3 Ọ bụrụ na nsonaazụ nke injections abụọ ahụ na-agbaso ụkpụrụ nnabata, a na-ewere nkezi ịdị ọcha dị ka nsonaazụ ikpeazụ.
3, Ebe mgbaze -- RY-1 ihe mgbaze
4. Ọnwụ na usoro nchọpụta ihicha
4.1 Ngwa:
Igwe ọkụ ọkụ ọkụ ọkụ eletrik, otu n'ime nha puku iri.
4.2 Usoro:
N'ime karama na-atụ ihe dị larịị nke nwere mkpuchi ọnụ ala nke nwere ịdị arọ mgbe niile yana ihicha oke, tụọ gram 1 nke nlele (nke ziri ezi na gram 0.0001).The sample kwesịrị evenly gbasaa na ala nke arọ karama na a ọkpụrụkpụ nke ọ dịghị ihe karịrị 10mm, tinye na a mgbe nile okpomọkụ electric ihicha oven, nkụ na 105-110 ℃ maka 3 awa, wee banye n'ime ihicha ụlọ, jụụ. ruo ụlọ okpomọkụ ma tụọ.
Ngụkọta: Mbelata arọ akọrọ %= (M1-M2) ÷M×100
Ebe: M1: uka nke sample na karama atụ tupu ihicha, g
M2: Uka nke sample na karama atụ mgbe akpọchara, g
Nna-ukwu: Ihe nlere anya, gram
5. Ntughari pụrụ iche
-- Specific ntụgharị ka a tụrụ dị ka GB/T613-1988 si dị
Nkwadebe ihe atụ: 0.5000g nke ihe nlele tụrụ n'ụzọ ziri ezi wee bufee ya na karama volumetric 50ml dị ọcha ma kpọọ nkụ na 20ml Ethyl acetate.A kpachiri karama ahụ ma maa jijiji ka ọ gbazee Ethyl acetate.
Nnwale: Gbanwee efu nke gyroscope tupu ule ahụ, wee jupụta tube ule ahụ na ngwọta nlele, dekọọ akụkụ ntụgharị nke ntụgharị, wee gbakọọ ntụgharị a kapịrị ọnụ nke nlele ahụ site na iji usoro a.
[α]20/D= (r×50) ÷(L×W)
Ebe:
[α] 20/D: Ntugharị akọwapụtara nke ngwọta nlele na 25 ℃
r: Ntughari hụrụ na 25 ℃ maka sample ngwọta
50: Kwadebe olu ngwọta sample (ml)
w: Nlereanya arọ (g)
L: Ogologo tube anya (dm)
6. Nyocha TCL
Nkwadebe ihe atụ: 0.5000g sample tụrụ n'ụzọ ziri ezi ma kwaga na karama volumetric 50ml dị ọcha ma kpọọ nkụ, 40ml EtoH gbakwunyere, karama ahụ kpuchie ma maa jijiji ka ọ gbazee, wee gbanye ya na EtoH.
Nkwadebe nke njikwa ihe nlele: 0.5000g sample tụrụ n'ụzọ ziri ezi ma kwaga na karama volumetric 50ml dị ọcha ma kpọọ nkụ, 40ml mmiri na 2 tụlee nke 6N hydrochloric acid, etinyere karama ahụ ma maa jijiji ka ọ gbazee, wee diluted na ọnụ ọgụgụ ya. mmiri.Were 0,5 nke mmiri mmiri dị n'elu ma gbanye ya na ethanol n'ime karama olu 100ml gaa na nlele ntụaka nwere nha 1.0% amino acid fọdụrụnụ.
Ejiri sirinji microsampling were were 10 microliter sample, ma tinye ihe nlele ahụ na efere silicone GF254.5 microliter, 10 microliter na 15 microliter point plates were were maka ntụnyere n'otu n'otu.
Onye na-emepe emepe: n-butanol: glacial acetic acid: mmiri =4:1:1.
Ihe na-emepe emepe agba: 5% ninhydrin methanol ngwọta.
Ịrụ ọrụ mmepe agba: nke mbụ, jiri igwe na-ehicha ntutu iji kpoo efere silica gel nke mepere emepe, tinyezie ya n'ime 5% ninhydrin methanol solution, wee kpochaa, na akpọọ nkụ na okpomọkụ dị elu na ọkụ eletrik maka mmepe agba.
Ikpe: Lelee oge agba ngwaahịa, nha ntụpọ, ntinye agba na ntụnyere ngwaahịa njikwa, kpee ikpe na ọ dị n'ụdị ahụ.