L-4-Nitrophenylalanine Methyl Ester HCl CAS 17193-40-7 H-Phe(4-NO2) -OMe·HCl Assay>98.5% (HPLC) Ụlọ ọrụ

Usoro nyocha nke L-4-Nitrophenylalanine Methyl Ester HCl (H-Phe(4-NO2) -OMe·HCl (CAS: 17193-40-7)
Nkọwa: Debe ihe dị ka 2 g nke sample n'ime efere petri-nke dị ọcha na nke akọrọ ma hụ ọdịdị nke nlele.Akuko: Kwuo ihe nleba anya
Identificaiton: Tulee oge njide nke isi kacha elu na chromatogram nke nkwadebe ule na oge njide nke isi kacha elu na chromatogram nke usoro dabara adaba dịka enwetara na ịdị ọcha chromatographic site na HPLC.
Ọnwụ na ihicha: Kpochapụ karama ntụ ntụ na-adịghị na-emighị emi na 105± 2℃ maka nkeji 30.Kwe ka ọ dị jụụ ruo n'ime ụlọ n'ime ihe nrịbama.Jiri nkwụsịtụ tụọ karama atụ ahụ nke ọma ma dekọọ ibu ya (W1).Nyefee ihe dị ka 1 ruo 2g nke ihe nlele a tụrụ nke ọma n'ime karama atụ.Site n'iji nwayọọ, ịma jijiji n'akụkụ akụkụ, kesaa ihe nlele ule ahụ dịka o kwere mee na omimi nke ihe dịka 5 mm.Tulee karama a na-atụnye ibu ma dekọọ ibu ya (W2).Debe karama ahụ a na-ebunye na oven ihicha, wepụ ihe nkwụsị ma hapụ ya n'ime ụlọ.Kpọọ ihe nlele ule na 105± 2℃ maka awa 3.Mgbe imepechara ụlọ ahụ, mechie karama ahụ ngwa ngwa, ma kwe ka ọ bịaruo okpomọkụ n'ime ụlọ n'ime igwe nhicha.Jiri nkwụsịtụ tụọ karama a na-atụ atụ nke ọma ma weghachite ịdị arọ ya (W3).Gbakọọ mfu pasentị na ihicha ihe nlele site na iji usoro a:
Mfu mgbako na ihicha (% w/w)= (W2-W3) ÷ (W2-W1) x 100
Ọdịnaya Enantiomer nke HPLC:
Chemical & Reagents:
n-Hexane AR ọkwa
Methanol HPLC ọkwa
Isopropyl mmanya HPLC ọkwa
Diethylamine AR ọkwa
Ụkpụrụ: L-4-Nitrophenylalanine Methyl Ester HCl ọkọlọtọ;L-4-Nitrophenylalanine Methyl Ester HCl enantiomer ọkọlọtọ
Usoro mkpanaaka: Kwadebe ngwakọta nke n-Hexane, mmanya Isopropyl, methanol na Diethylamine (65:20:15:0.1 v/v/v/v)
Nkwadebe oghere: Nyefee 2.5ml nke methanol n'ime flask volumetric 10-ml, gbanye olu na usoro mkpanaka na mix.
Nkwadebe nke dabara na sistemụ:
Were nha nke ọma ma nyefee ihe dịka 5 mg nke ọ bụla nke L-4-Nitrophenylalanine Methyl Ester HCl ọkọlọtọ na L-4-Nitrophenylalanine Methyl Ester HCl enantiomer ọkọlọtọ na 10-ml volumetric flask, gbazee n'ihe dị ka 2.5ml nke methanol, gbanye na olu na mobile mobile. oge na mix.
Nkwadebe nwale:
Were nha nke ọma ma bufee ihe dịka 5 mg nke sample n'ime flask volumetric 10-mol, gbarie n'ihe dịka 2.5ml nke methanol, gbanye ya na olu na usoro mkpanaka wee gwakọta ya.
Ngwa ngwa:
Akụrụngwa: HPLC kwadoro ya na injector, Pump, UV detector and Recorder
Ogidi: ChiralPak-IC (4.6mm x 250mm) 5 μ ma ọ bụ dakọtara
Ọsọ ọsọ: 1.0 ml / nkeji
Ogologo ogologo: 260nm
Olu ogwu ogbugba: 10 μL
Okpomọkụ agba agba: 25 ℃
Oge ịgba ọsọ: nkeji 20
Usoro
Tinye ihe ngwọta dị ka ekwuru n'usoro na-esonụ.Dekọọ chromatogram ma kwado njirisi:
Nkọwapụta Ọnụọgụ Ịgba Ọgbanye
Nkwadebe oghere 1 Ọnweghị ọnụ ọgụgụ kacha elu na-etinye aka na oge njide L-4-Nitrophenylalanine Methyl Ester HCl ma ọ bụ enantiomer.
Nkwadebe dabara adaba sistemu 1 Mkpebi dị n'etiti L-4-Nitrophenylalanine Methyl Ester HCl na elu enantiomer ekwesịghị ịbụ ihe na-erughị 2.0
Nkwadebe ule 1 Jiri chromatogram nnwale chọpụta ọdịnaya enantiomer dị n'omume.
Oge njide emetụtara:
L-4-Nitrophenylalanine Methyl Ester HCl 1.0
Enantiomer Ihe dị ka 1.11
Oge njide nke L-4-Nitrophenylalanine Methyl Ester HCl bụ ihe dịka nkeji 9.8.
Ngụkọta: Na chromatogram enwetara site na nkwadebe ule, eleghara ọnụ ọgụgụ niile anya na-atụ anya L-4-Nitrophenylalanine Methyl Ester HCl na Enantiomer.Kwuo ọdịnaya enantiomer dị na nlele ahụ site na usoro nhazi mpaghara.
Chromatogrpahic dị ọcha na adịghị ọcha nke HPLC:
Chemical & Reagents:
Diammonium phosphate AR ọkwa
Phosphoric acid AR ọkwa
Methanol HPLC ọkwa
Mmiri dị ọcha
Ụkpụrụ
L-4-Nitrophenylalanine Methyl Ester HCl ọkọlọtọ
4-Nitro-L-Phenylalanine monohydrate ọkọlọtọ
Usoro mkpanaaka-A
Igbari 6.6 g nke Diammonium phosphate na 1000ml nke mmiri dị ọcha.Gbanwee pH nke ngwọta a na 6.0 na Phosphoric acid.Nyo na degas.Tupu ị tụọ pH nke ngwọta, mezie pH mita na ọkọlọtọ ihe ngwọta pH 4.01 NA 7.00.
Usoro mkpanaaka-B
Methanol HPLC ọkwa
Nkwadebe dabara adaba sistemụ
Were nha nke ọma ma bufee ihe dịka 25 mg nke ọ bụla nke L-4-Nitrophenylalanine Methyl Ester HCl ọkọlọtọ na ọkọlọtọ 4-Nitro-L-Phenylalanine monohydrate na flask volumetric 50 ml, gbazee ma gbanye ya na methanol na mix.
Nkwadebe nwale:
Were nha nke ọma ma bufee ihe dịka 25 mg sample n'ime flask volumetric 50-ml, gbazee ma gbanye ya na methanol na mix.
Ngwa ngwa:
Akụrụngwa: HPLC kwadoro ya na injector, Pump, UV detector and Recorder
Ogidi: XTerra RP-18 (4.6mm x 150mm) 5 μ ma ọ bụ dakọtara
Ọsọ ọsọ: 1.0 ml / nkeji
Ogologo ogologo: 265nm
Olu ogwu ogbugba: 20 μL
Okpomọkụ agba agba: 25 ℃
Oge ịgba ọsọ: nkeji 45
Mmemme gradient
Oge (nkeji) Usoro mkpanaaka-A % Usoro mkpanaaka-B %
0.01 90 10
15 60 40
35 40 60
40 35 65
41 90 10
45 90 10
Usoro:
Tinye ihe ngwọta dị ka ekwuru n'usoro na-esonụ.Dekọọ chromatogram ma kwado njirisi:
Nkwadebe oghere 1 Ọnweghị ọnụ ọgụgụ kacha elu na-etinye aka na oge njide L-4-Nitrophenylalanine Methyl Ester HCl.
Nkwadebe dabara adaba sistemu 1 ihe ọdụdụ maka L-4-Nitrophenylalanine Methyl Ester HCl kacha elu ekwesịghị ịbụ ihe na-erughị 2.0
Nkwadebe nnwale 1 Jiri chromatogram nnwale chọpụta ịdị ọcha na adịghị ọcha chromatographic.
Oge njide emetụtara:
L-4-Nitrophenylalanine Methyl Ester HCl 1.0 (oge njide ihe dị ka nkeji 11.4)
4-Nitro-L-Phenylalanine Ihe dị ka 0.4
Toluene Ihe dị ka 2.3
Mgbakọ:
Na chromatogram enwetara site na nkwadebe ule, mgbe mgbazi oghere, leghara ọnụ ọgụgụ kachasị elu n'ihi toluene.Kpesa ịdị ọcha chromatographic, ọdịnaya 4-Nitro-L-Phenylalanine na mkpokọta adịghị ọcha na nlele site na usoro nhazi mpaghara.