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

Indlela yoVavanyo lwe-L-4-Nitrophenylalanine Methyl Ester HCl (H-Phe(4-NO2)-OMe·HCl) (CAS: 17193-40-7)
Inkcazo: Beka malunga ne-2 g yesampuli kwindawo ecocekileyo neyomileyo ye-petri-dish kwaye ugcine imbonakalo yesampuli.Ukunika ingxelo: Xela uqwalaselo
I-Identificaiton: Thelekisa ixesha lokugcinwa kwencopho enkulu kwichromatogram yolungiselelo lovavanyo kunye nexesha lokugcinwa kwencopho enkulu kwikhromatogram yokulunga kwenkqubo njengoko ifunyenwe kucoceko lwechromatographic yi-HPLC.
Ilahleko Ekomisweni: Yomisa ibhotile emiswe ngeglasi, umlinganiselo ongekho nzulu nge-105±2℃ kangangemizuzu engama-30.Yivumele ukuba iphole kwiqondo lobushushu begumbi kwi-desciccator.Viyisha ngokuchanekileyo ibhotile yokulinganisa ngesithinteli kwaye urekhode ubunzima (W1).Dlulisa malunga ne-1 ukuya kwi-2g ngokuchanekileyo ubungakanani bento yovavanyo kwibhotile yokuwayisha.Ngokungcangcazela okuthambileyo, ecaleni, unikezelo lovavanyo ngokulinganayo kangangoko kunokwenzeka kubunzulu obumalunga ne-5 mm.Yenza umlinganiselo webhotile elayishiweyo kwaye urekhode ubunzima (W2).Beka ibhotile elayishiweyo kwi-oven yokumisa, ukususa isivalo kwaye usishiye kwigumbi.Yomisa isampuli yovavanyo kwi-105±2℃ iiyure ezi-3.Xa uvula igumbi, vala ibhotile ngokukhawuleza, kwaye uyivumele ukuba ifike kubushushu begumbi kwi-desiccator.Viyisha ngokuchanekileyo ibhotile yokuwayisha ngesithinteli kwaye ubuyise ubunzima (W3).Bala ipesenti yelahleko ekomisweni kwesampulu ngokusebenzisa ifomula ilandelayo:
Ukubala Ilahleko ekomisweni (% w/w)= (W2-W3) ÷ (W2-W1) x 100
Isiqulatho se-Enantiomer yi-HPLC:
Imichiza kunye nezixhobo zokusebenza:
n-Hexane AR ibakala
Ibanga leMethanol HPLC
Isopropyl Alcohol HPLC ibakala
Diethylamine AR ibakala
Imigangatho: L-4-Nitrophenylalanine Methyl Ester HCl umgangatho;L-4-Nitrophenylalanine Methyl Ester HCl enantiomer umgangatho
ISigaba seMobile: Lungisa umxube we-n-Hexane, i-Isopropyl Alcohol, i-Methanol kunye ne-Diethylamine (65:20:15: 0.1 v/v/v/v)
Ukulungiselela okungenanto: Dlulisa i-2.5ml ye-Methanol kwi-flask ye-volumetric ye-10-ml, nciphisa umthamo kunye nesigaba seselula kunye nokuxuba.
Ukulungiswa kokufaneleka kwenkqubo:
Ukulinganisa ngokuchanekileyo kwaye udlulisele malunga ne-5 mg nganye ye-L-4-Nitrophenylalanine ye-Methyl Ester HCl umgangatho kunye ne-L-4-Nitrophenylalanine Methyl Ester HCl umgangatho we-enantiomer kwi-flask ye-volumetric ye-10-ml, inyibilika malunga ne-2.5ml ye-methanol, ihlambulule ivolumu kunye neselula isigaba kunye nokuxuba.
Ukulungiselela uvavanyo:
Ukulinganisa ngokuchanekileyo kwaye udlulise malunga ne-5 mg yesampuli kwi-flask ye-volumetric ye-10-mol, ichithe malunga ne-2.5ml ye-methanol, ihlambulule ivolumu kunye nesigaba seselula kunye nokuxuba.
Iiparamitha zesixhobo:
Isixhobo: I-HPLC ixhotyiswe nge-injector, impompo, umtshini we-UV kunye neRekhoda
Ikholamu: ChiralPak-IC (4.6mm x 250mm) 5 μ okanye ilingana
Izinga lokuhamba: 1.0 ml / ngomzuzu
Ubude bobude: 260nm
Umthamo wokutofa: 10 μL
Iqondo lobushushu lekholamu yomnqophiso: 25℃
Ixesha lokubaleka: imizuzu engama-20
Inkqubo
Tofa izisombululo njengoko kukhankanyiwe kolu landelelwano lulandelayo.Rekhoda iichromatogram kwaye uqinisekise imilinganiselo:
Inkcazo yezitofu Inani leekhrayitheriya zokutofa
Ukulungiswa okungenanto 1 Akukho ncopho yokuphazamisayo kufuneka ibonwe ngexesha lokugcinwa kwe-L-4-Nitrophenylalanine Methyl Ester HCl okanye i-enantiomer.
Ukulungiswa kokufaneleka kwenkqubo 1 Isisombululo phakathi kwe-L-4-Nitrophenylalanine Methyl Ester HCl kunye nencopho ye-enantiomer kufuneka ingabi ngaphantsi kwe-2.0
Ukulungiswa kovavanyo 1 Sebenzisa ichromatogram yovavanyo ukujonga umxholo we-enantiomer kwisampulu.
Amaxesha okuGcina okunxulumeneyo:
L-4-Nitrophenylalanine Methyl Ester HCl 1.0
I-Enantiomer Malunga ne-1.11
Ixesha lokugcinwa kwe-L-4-Nitrophenylalanine Methyl Ester HCl malunga nemizuzu eyi-9.8.
Ukubala: Kwichromatogram efunyenwe kulungiselelo lovavanyo, ukugatya zonke iincopho zilindele i-L-4-Nitrophenylalanine Methyl Ester HCl kunye ne-Enantiomer.Xela isiqulatho se-enantiomer kwisampulu ngokwendlela yokwenziwa kwesiqhelo kwendawo.
Ubunyulu beChromatogrpahic kunye nokungacoceki yi-HPLC:
Imichiza kunye nezixhobo zokusebenza:
Diammonium phosphate AR ibakala
Iphosphoric acid AR ibakala
Ibanga leMethanol HPLC
Amanzi acocekileyo
Imigangatho
L-4-Nitrophenylalanine Methyl Ester HCl umgangatho
4-Nitro-L-Phenylalanine monohydrate umgangatho
Isigaba esiselfowuni-A
Chitha i-6.6 g ye-Diammonium phosphate kwi-1000ml yamanzi ahlambulukileyo.Lungisa i-pH yesi sisombululo kwi-6.0 kunye ne-Phosphoric acid.Isihluzo kunye ne-degas.Phambi kokulinganisa i-pH yesisombululo, linganisa imitha ye-pH ngesisombululo esiqhelekileyo sesithinteli pH 4.01 KUNYE 7.00.
ISigaba esiphathwayo-B
Ibanga leMethanol HPLC
ULungiselelo lokufaneleka kweNkqubo
Ukulinganisa ngokuchanekileyo kwaye udlulise malunga ne-25 mg nganye ye-L-4-Nitrophenylalanine ye-Methyl Ester HCl umgangatho kunye ne-4-Nitro-L-Phenylalanine monohydrate umgangatho kwi-flask ye-volumetric ye-50-ml, inyibilika kwaye ihlanjululwe kwivolumu kunye ne-methanol kunye nokuxuba.
ULungiselelo loVavanyo:
Ukulinganisa ngokuchanekileyo kwaye udlulise malunga ne-25 mg isampuli kwi-flask ye-volumetric ye-50-ml, udibanise kwaye udibanise umthamo kunye ne-methanol kunye nokuxuba.
Iiparamitha zesixhobo:
Isixhobo: I-HPLC ixhotyiswe nge-injector, impompo, umtshini we-UV kunye neRekhoda
Uluhlu: XTerra RP-18 (4.6mm x 150mm) 5 μ okanye ilingana
Izinga lokuhamba: 1.0 ml / ngomzuzu
Ubude bobude: 265nm
Umthamo wokutofa: 20 μL
Iqondo lobushushu lekholamu yomnqophiso: 25℃
Ixesha lokuqhuba: imizuzu engama-45
Inkqubo yeGradient
Ixesha (umzuzu) iSigaba seMobile-A % iSigaba esiSetyenzwayo-B %
0.01 90 10
15 60 40
35 40 60
40 35 65
41 90 10
45 90 10
Inkqubo:
Tofa izisombululo njengoko kukhankanyiwe kolu landelelwano lulandelayo.Rekhoda iichromatogram kwaye uqinisekise imilinganiselo:
Ukulungiselela okungenanto 1 Akukho ncopho yokuphazamisayo kufuneka ibonwe ngexesha lokugcinwa kwe-L-4-Nitrophenylalanine Methyl Ester HCl.
Ukulungiswa kokufaneleka kwenkqubo 1 I-Tailing factor ye-L-4-Nitrophenylalanine Methyl Ester Incopho yeHCl kufuneka ingabi ngaphantsi kwe-2.0
Amalungiselelo ovavanyo 1 Sebenzisa ichromatogram yovavanyo ukujonga ukucoceka kwechromatographic kunye nokungcola.
Amaxesha okuGcina okunxulumeneyo:
L-4-Nitrophenylalanine Methyl Ester HCl 1.0 (ixesha lokugcinwa malunga nemizuzu eyi-11.4)
4-Nitro-L-Phenylalanine Malunga ne-0.4
Toluene Malunga 2.3
Ubalo:
Kwichromatogram efunyenwe ekulungiseleleni uvavanyo, emva kokulungiswa okungenanto, ungayinaki incopho ngenxa ye-toluene.Xela ukucoceka kwe-chromatographic, umxholo we-4-Nitro-L-Phenylalanine kunye nokungcola okupheleleyo kwisampulu ngendlela yokulinganisa indawo.