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

Ọna Itupalẹ ti L-4-Nitrophenylalanine Methyl Ester HCl (H-Phe (4-NO2) -OMe · HCl (CAS: 17193-40-7)
Apejuwe: Gbe nipa 2 g ti ayẹwo ni mimọ ati ki o gbẹ petri-satelaiti ati ki o ṣe akiyesi ifarahan ti ayẹwo.Iroyin: Jabo akiyesi
Identificaiton: Ṣe afiwe akoko idaduro ti tente oke pataki ni chromatogram ti igbaradi idanwo pẹlu akoko idaduro ti tente oke pataki ni chromatogram ti adaṣe ibamu eto bi a ti gba ni mimọ chromatographic nipasẹ HPLC.
Pipadanu lori Gbigbe: Gbẹ gilasi-duro, igo iwuwo aijinile ni 105± 2℃ fun ọgbọn išẹju 30.Gba laaye lati tutu si iwọn otutu yara ni desciccator.Ṣe iwọn deede igo iwuwo pẹlu iduro ati ṣe igbasilẹ iwuwo naa (W1).Gbigbe ni iwọn 1 si 2g ni deede iwọn opoiye ti nkan idanwo sinu igo iwuwo.Nipa irẹlẹ, gbigbọn ni ẹgbẹ, pin kaakiri apẹrẹ idanwo bi boṣeyẹ bi o ti ṣee ṣe si ijinle nipa 5 mm.Ṣe iwọn igo iwuwo ti kojọpọ ki o ṣe igbasilẹ iwuwo naa (W2).Fi igo ti a kojọpọ sinu adiro gbigbẹ, yọ idaduro naa kuro ki o si tun fi silẹ ni iyẹwu naa.Gbẹ ayẹwo idanwo ni 105 ± 2 ℃ fun awọn wakati 3.Nigbati o ba ṣii iyẹwu naa, pa igo naa ni kiakia, ki o jẹ ki o wa si iwọn otutu yara ni ẹrọ ẹlẹmi.Ṣe iwọn deede igo iwuwo pẹlu iduro ati tunṣe iwuwo naa (W3).Ṣe iṣiro pipadanu ogorun lori gbigbẹ ti ayẹwo nipasẹ lilo agbekalẹ atẹle:
Ipadanu Iṣiro lori gbigbe (% w/w)= (W2-W3) ÷ (W2-W1) x 100
Akoonu Enantiomer nipasẹ HPLC:
Kemikali & Awọn atunmọ:
n-Hexane AR ite
Methanol HPLC ite
Isopropyl Ọtí HPLC ite
Diethylamine AR ite
Awọn ajohunše: L-4-Nitrophenylalanine Methyl Ester HCl boṣewa;L-4-Nitrophenylalanine Methyl Ester HCl enantiomer boṣewa
Alakoso Alagbeka: Mura idapọ isokan ti n-Hexane, Ọti Isopropyl, Methanol ati Diethylamine (65:20:15:0.1 v/v/v/v)
Igbaradi òfo: ​​Gbigbe 2.5ml ti Methanol ni 10-ml volumetric flask, dilute si iwọn didun pẹlu alakoso alagbeka ati dapọ.
Igbaradi ibamu eto:
Ṣe iwọn ni deede ati gbigbe nipa 5 miligiramu kọọkan ti L-4-Nitrophenylalanine Methyl Ester HCl boṣewa ati L-4-Nitrophenylalanine Methyl Ester HCl enantiomer boṣewa ni 10-milimita flask volumetric kan, tu ni bii 2.5ml ti kẹmika, dilute si iwọn didun pẹlu alagbeka alagbeka. alakoso ati illa.
Igbaradi idanwo:
Ṣe iwọn ni deede ati gbe nkan bii miligiramu 5 ti ayẹwo ni ọpọn iwọn didun 10-mol, tu ni bii 2.5ml ti kẹmika kẹmika, dilute si iwọn didun pẹlu ipele alagbeka ati dapọ.
Awọn paramita ẹrọ:
Irinse: HPLC ni ipese pẹlu injector, Fifa, UV aṣawari ati Agbohunsile
Ọwọn: ChiralPak-IC (4.6mm x 250mm) 5 μ tabi deede
Iwọn sisan: 1.0 milimita / iṣẹju
Ipari: 260nm
Iwọn abẹrẹ: 10 μL
Iwọn otutu majẹmu ọwọn: 25 ℃
Akoko ṣiṣe: iṣẹju 20
Ilana
Fi awọn ojutu silẹ bi a ti mẹnuba ninu ọkọọkan atẹle.Ṣe igbasilẹ awọn chromatogram ki o jẹrisi awọn ibeere:
Apejuwe Nọmba Awọn Abẹrẹ Awọn Abẹrẹ
Igbaradi òfo 1 Ko si tente interfering ko yẹ ki o ṣe akiyesi ni akoko idaduro L-4-Nitrophenylalanine Methyl Ester HCl tabi enantiomer.
Igbaradi ibamu eto eto 1 ipinnu laarin L-4-Nitrophenylalanine Methyl Ester HCl ati tente oke enantiomer ko yẹ ki o kere ju 2.0
Igbaradi idanwo 1 Lo chromatogram idanwo lati pinnu akoonu enantiomer ninu apẹẹrẹ.
Awọn akoko Idaduro ibatan:
L-4-Nitrophenylalanine Methyl Ester HCl 1.0
Enantiomer Nipa 1.11
Akoko idaduro L-4-Nitrophenylalanine Methyl Ester HCl jẹ nipa awọn iṣẹju 9.8.
Iṣiro: Ninu chromatogram ti o gba lati igbaradi idanwo, aibikita gbogbo awọn oke ti o nireti L-4-Nitrophenylalanine Methyl Ester HCl ati Enantiomer.Jabọ akoonu enantiomer ninu apẹẹrẹ nipasẹ ọna isọdi deede agbegbe.
Iwa-mimọ Chromatogrpahic ati Aimọ nipasẹ HPLC:
Kemikali & Awọn atunmọ:
Diammonium fosifeti AR ite
Phosphoric acid AR ite
Methanol HPLC ite
Omi ti a sọ di mimọ
Awọn ajohunše
L-4-Nitrophenylalanine Methyl Ester HCl boṣewa
4-Nitro-L-Phenylalanine monohydrate boṣewa
Alagbeka Alakoso-A
Tu 6.6 g ti Diammonium fosifeti ni 1000 milimita ti omi mimọ.Ṣatunṣe pH ti ojutu yii si 6.0 pẹlu Phosphoric acid.Àlẹmọ ati degas.Ṣaaju idiwọn pH ti ojutu, ṣe calibrate pH mita pẹlu ojutu saarin boṣewa pH 4.01 AND 7.00.
Alagbeka Ipele-B
Methanol HPLC ite
Eto Ibamu Igbaradi
Ṣe iwọn ni deede ati gbe nkan bii 25 miligiramu kọọkan ti L-4-Nitrophenylalanine Methyl Ester HCl boṣewa ati boṣewa 4-Nitro-L-Phenylalanine monohydrate ninu ọpọn iwọn didun 50-ml, tu sinu ati dilute si iwọn didun pẹlu methanol ati dapọ.
Igbaradi Idanwo:
Ṣe iwọn ni deede ati gbe iwọn iwọn miligiramu 25 sinu ọpọn iwọn didun 50-milimita, tu sinu ati dilute si iwọn didun pẹlu kẹmika ati dapọ.
Awọn paramita ẹrọ:
Irinse: HPLC ni ipese pẹlu injector, Fifa, UV aṣawari ati Agbohunsile
Ọwọn: XTerra RP-18 (4.6mm x 150mm) 5 μ tabi deede
Iwọn sisan: 1.0 milimita / iṣẹju
Ipari: 265nm
Iwọn abẹrẹ: 20 μL
Iwọn otutu majẹmu ọwọn: 25 ℃
Akoko ṣiṣe: iṣẹju 45
Eto Gradient
Akoko (iṣẹju) Alagbeka-A % Alagbeka Alakoso-B %
0.01 90 10
15 60 40
35 40 60
40 35 65
41 90 10
45 90 10
Ilana:
Fi awọn ojutu silẹ bi a ti mẹnuba ninu ọkọọkan atẹle.Ṣe igbasilẹ awọn chromatogram ki o jẹrisi awọn ibeere:
Igbaradi òfo 1 Ko si tente interfering ko yẹ ki o ṣe akiyesi ni akoko idaduro L-4-Nitrophenylalanine Methyl Ester HCl.
Igbaradi ibamu eto eto 1 ifosiwewe Tailing fun L-4-Nitrophenylalanine Methyl Ester HCl tente oke ko yẹ ki o kere ju 2.0
Igbaradi idanwo 1 Lo chromatogram idanwo lati pinnu mimọ ati awọn aimọ.
Awọn akoko Idaduro ibatan:
L-4-Nitrophenylalanine Methyl Ester HCl 1.0 (akoko idaduro nipa awọn iṣẹju 11.4)
4-Nitro-L-Phenylalanine Nipa 0.4
Toluene Nipa 2.3
Awọn iṣiro:
Ninu chromatogram ti a gba lati igbaradi idanwo, lẹhin atunse ofo, ṣaibikita tente oke nitori toluene.Jabọ mimọ kiromatogirafi, akoonu 4-Nitro-L-Phenylalanine ati awọn aimọ-aimọ lapapọ ninu apẹẹrẹ nipasẹ ọna isọdọtun agbegbe.