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

Hanyoyin dubawa
1. Bayyanar
-- Duban gani
2. Tsafta (HPLC)
2.1 Kayan aiki
Babban aikin chromatography ruwa, mai gano PDA.
Ma'aunin nazari na lantarki
2.2 Reagent
Acetonitrile (jin chromatographic), trifluoroacetic acid (jin chromatographic)
2.3 Yanayi na chromatographic
2.3.1 Rukunin: YMC-ODS-AM, 5 μl, 250x4.6 mm
2.3.2 Tsawon Gano: INC220nm
Yawan gudu: 1.0ml/min
Samfurin girman: 10 μl (labarin)
Diluent: acetonitrile
Lokacin tattara bayanai: 25.00min
2.4 Shirye-shiryen lokaci na wayar hannu
Wayar hannu lokaci A (0.1% trifluoroacetic acid ruwa): daidaitaccen sha 2. Dilute Oml trifluoroacetic acid da ruwa zuwa 2000m1, Mix da kyau, da degassing;
Lokacin wayar hannu B (0.1% acetonitrile trifluoroacetic acid): daidaitaccen sha 2.0ml trifluoroacetic acid an diluted zuwa 2000m1 tare da acetonitrile, gauraye da degassing;
2.5 Tsarin gradient na lokacin wayar hannu
Lokaci (min) A% B%
0.0090 10
13.00 10 90
18.00 10 90
18.01 90 10
23.00 90 10
2.6 Shiri na samfurin bayani
Yi nauyi da narkar da samfurin 0.1g tare da acetonitrile kuma a tsarma zuwa 100ml, girgiza da kyau don amfani, ko taro iri ɗaya.Shirya samfurori guda biyu a layi daya.
2.7 Samfurin Ƙaddamarwa
Yi nazarin samfurin bisa ga tsarin samfur mai zuwa:
Fiye da allura 1 na bayani mara kyau
1 stitch sample solution 1#
1 dinki samfurin bayani 2#
2.8 Sakamakon sakamako
2.8.1 An yi amfani da hanyar daidaita yanayin yanki mafi girma don ƙididdige tsaftar HPLC ta hanyar cire sarari mara kyau.
2.8.2 Ma'anar ma'anar ma'anar tsarki na allura biyu ba za ta fi 1% ba.
2.8.3 Idan sakamakon alluran biyu sun cika ka'idojin yarda, ana ɗaukar matsakaicin tsafta azaman sakamako na ƙarshe.
3, Matsayin narkewa -- RY-1 kayan aikin narkewa
4. Asarar hanyar gano bushewa
4.1 Kayan aiki:
Electric thermostatic bushewa tanda, daya daga cikin dubu goma ma'auni.
4.2 Tsari:
A cikin lebur kwalban aunawa tare da murfin bakin ƙasa tare da nauyi akai-akai da bushewa, auna gram 1 na samfurin (daidai zuwa gram 0.0001).Samfurin ya kamata a yada a ko'ina a kasan kwalban auna tare da kauri ba fiye da 10mm ba, a saka shi a cikin tanda mai bushewa na lantarki akai-akai, bushe a 105-110 ℃ na 3 hours, sa'an nan kuma matsawa cikin ɗakin bushewa, sanyi. zuwa zafin jiki da awo.
Lissafi: Busassun nauyi %= (M1-M2) ÷M×100
Inda: M1: yawan samfurin da kwalban awo kafin bushewa, g
M2: Yawan samfuri da kwalbar auna bayan bushewa, g
M: Misalin taro, gram
5. Takamaiman juyawa
-- Ana auna takamaiman juyawa daidai da GB/T613-1988
Shirye-shiryen samfurin: 0.5000g na samfurin an auna daidai kuma an canja shi zuwa kwalban 50ml mai tsabta da bushe tare da 20ml Ethyl acetate.An toshe kwalbar kuma an girgiza don narkar da Ethyl acetate.
Gwaji: Daidaita sifilin gyroscope kafin gwajin, sannan cika bututun gwajin tare da maganin samfurin, yi rikodin kusurwar jujjuyawar juyi, kuma ƙididdige takamaiman jujjuya samfurin ta amfani da dabara mai zuwa.
[α]20/D= (r×50) ÷(L×W)
Inda:
[α] 20/D: Musamman jujjuyawar samfurin bayani a 25 ℃
r: Juyawa lura a 25 ℃ ga samfurin bayani
50: Shirya samfurin bayani girma (ml)
w: Misalin nauyi (g)
L: Tsawon bututun gani (dm)
6. Binciken TCL
Shirye-shiryen samfurin: 0.5000g samfurin an auna daidai kuma an motsa shi zuwa kwalban 50ml mai tsabta da bushe, an ƙara 40ml EtoH, an rufe kwalban kuma girgiza don narkewa, sa'an nan kuma an diluted zuwa sikelin tare da EtoH.
Shirye-shiryen samfurin sarrafawa: 0.5000g samfurin an auna daidai kuma an motsa shi zuwa kwalban 50ml mai tsabta da bushe, ruwa 40ml da 2 saukad da na 6N hydrochloric acid an kara, kwalban an rufe shi da girgiza don narkewa, sa'an nan kuma diluted zuwa sikelin tare da ruwa.Daga nan sai a dauki 0.5 na ruwan da ke sama a tsoma shi da ethanol a cikin kwalban girma na 100ml zuwa samfurin tunani tare da sikelin ragowar amino acid 1.0%.
An dauki samfuran microliter 10 tare da sirinji na microsampling, kuma an sanya samfuran akan farantin silicone na GF254.An dauki 5 microliter, 10 microliter da 15 microliter faranti don kwatanta maki, bi da bi.
Wakilin haɓakawa: n-butanol: glacial acetic acid: ruwa = 4: 1: 1.
Wakilin haɓaka launi: 5% ninhydrin methanol bayani.
Ayyukan haɓaka launi: da farko, yi amfani da na'urar bushewa don bushe farantin silica gel ɗin da aka haɓaka, sannan a tsoma shi cikin 5% ninhydrin methanol solution, sannan a bushe, da gasa da zafi mai zafi a cikin tanderun lantarki don haɓaka launi.
Hukunci: Dubi lokacin launi samfurin, girman tabo, tattara launi da kwatanta tare da samfurin sarrafawa, yanke hukunci cewa yana cikin wannan kewayon.