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

Methodus analyseos L-4-Nitrophenylalanini Methyl Ester HCl (H-Phe(4-NO2)-OMe·HCl) (CAS: 17193-40-7)
Description: Locum circa 2 g specimen in catino puro et sicco petri et speciem exempli observare.Reporting: Report observationis
Identificaiton: Confer retentionis tempus cacuminis maioris in chromatogrammo probati praeparationis cum retentione temporis maioris cacuminis in praparatione chromatogrammi systematis idoneitatis prout habetur in puritate chromatographica ab HPLC.
Damnum in Siccatio: sicca vitreo obturante, utrem vadum appendens ad 105±2℃ pro 30 minutis.Sinite eam refrigerandi ut locus temperatus in desciccator.Accurate lagenam cum spissamento pensare et pondus notare (W1).Translatio circiter 1 ad 2g accurate ponderata quantitas substantiae testi in lagenam appensionem.Leni, obliqua concussione, specimina experimenti distribue quam aequaliter ut palam fieri potest ad altitudinem circiter 5 mm.Pone onustam lagenam pensantem et notare pondus (W2).Pone lagenam onustam in clibano siccescente, sublato spissamento et relinquendo eam etiam in conclavi.Excoquatur experimentum specimen apud CV±2℃ pro III horis.Cubiculum aperiens, lagenam cito claude, et ad cubiculum desicatoris permitte venire.Utrem cum spissamento ponderare accurate et ponderare recidi (W3).Recipis damnum calculare de siccatione exempli utendo sequenti formula:
Calculus Loss de exsiccatione (% w/w)= (W2-W3) (W2-W1) x 100
Enantiomer Content ab HPLC:
Chemical & Reagents:
n-Hexane AR gradus
Methanol HPLC gradus
Sin Isopropyl HPLC gradus
Diethylamine AR gradus
Signa: L-4-Nitrophenylalanine Methyl Ester HCl standard;L-4-Nitrophenylalanine Methyl Ester HCl enantiomer standard
Mobile Phase: Para mixturam homogeneam n-Hexane, Isopropyl Alcohol, Methanol et Diethylamine (65:20:15:0.1 v/v/v/v)
Praeparatio blank: Translatio 2.5ml Methanoli in lagena voluminis 10-ml, ad volumen cum periodo mobili diluta et permisceto.
Ratio apta praeparationis:
Accurate expende et transfer circa 5 mg singulorum L-4-Nitrophenylalanini Methyl Ester HCl vexillum et L-4-Nitrophenylalanini Methyl Ester HCl enantiomer vexillum in lagena voluminis 10-ml, solve circa 2.5ml methanolum, dilutum ad volumen cum mobili pascha et misce.
Praeparatio Test:
Expende accurate et transfer de 5 mg exempli in ampulla voluminis 10-mol, dissolve circa 2.5ml methanolum, dilutum ad volumen cum periodo mobili et permisceto.
Parametri instrumentales:
Instrument: HPLC instructum injectore, Pump, UV detectore et commentariis
Columna: ChiralPak-IC (4.6mm x 250mm) 5 μ or equivalent
Fluunt rate: 1.0 ml/minute
Necem: 260nm
Iniectio voluminis: 10 μL
Columna coven temp.: 25℃
Currere tempus: XX minuta
De modo procedendi
Injiciunt solutiones de quibus in sequenti ordine.Nota chromatogramma et criteria:
Description of Injections Numerus Injectionum Criteria
Blank Praeparatio 1 Nullum impedimentum apicem servetur in retentione temporis L-4-Nitrophenylalanini Methyl Ester HCl seu enantiomer.
Ratio congruentia praeparationis 1 Resolutio inter Methyl Ester HCl et enantiomer cacumen L-4-Nitrophenylalanine non minus quam 2.0 esse debet.
Test praeparatio 1 Usus test chromatogrammum ad enantiomer contentum in sample determinare.
Relativa retentionis tempora:
L-4-Nitrophenylalanine Methyl Ester HCl 1.0
Enantiomer de 1.11
Retentionis tempus L-4-Nitrophenylalanini Methyl Ester HCl est circiter 9.8 minuta.
Calculus: In chromatogramma ex experimento praeparationis adepta omnia iugis neglecta exspectant L-4-Nitrophenylalanine Methyl Ester HCl et Enantiomer.Referre enantiomer contentus in sample in area ordinationem methodi.
Chromatogrpahic puritas et immunditia per HPLC:
Chemical & Reagents:
Diammonium phosphas AR grade
Acidum phosphoricum AR gradus
Methanol HPLC gradus
Aqua mundata
Signa
L-4-Nitrophenylalanine Methyl Ester HCl standard
4-Nitro-L-Phenylalanine vexillum monohydratum
Mobile Phase-A
Diammonium phosphas 1000ml aquae purgatae solve 6.6.Adpone pH solutionis huius ad 6.0 cum acido phosphorico.Colum et degas.Priusquam pH solutionis metiaris, metrum pH calibrate cum solutione obolo quiddam pH 4.01 ET 7.00.
Mobile Phase-B
Methanol HPLC gradus
Praeparatio Ratio idoneitas
Accurate expende et transfer circa 25 mg singulas mensuras L-4-Nitrophenylalanini Methyl Ester HCl et 4-Nitro-L-Phenylalanini vexillum monohydratum in lagena voluminis 50 ml, solve in ac dilutum ad volumen cum methanolo et misce.
Praeparatio Test:
Expende accurate et transfer de 25 mg specimen in lagena voluminis 50-ml, dissolve et dilue ad volumen cum methanolo et misce.
Parametri instrumentales:
Instrument: HPLC instructum injectore, Pump, UV detectore et commentariis
Columna: XTerra RP-18 (4.6mm x 150mm) 5 μ or equivalent
Fluunt rate: 1.0 ml/minute
Necem: 265nm
Iniectio volumen: 20 μL
Columna coven temp.: 25℃
Currere tempus: XLV minuta
Gradiente Program
Tempus (min) Mobile Phase-A % Mobile Phase-B %
0.01 90 10
15 60 40
35 40 60
40 35 65
41 90 10
45 90 10
De modo procedendi:
Injiciunt solutiones de quibus in sequenti ordine.Nota chromatogramma et criteria:
Blank Praeparatio 1 Nullum impedimentum apicum observandum est tempore retentionis L-4-Nitrophenylalanini Methyl Ester HCl.
Systema convenientia praeparationis 1 Tailing factor pro L-4-Nitrophenylalanine Methyl Ester HCl apicem non minus quam 2.0 esse debet.
Praeparatio probata 1 Usus chromatogrammi probatio ad puritatem chromatographicam et immunditias determinandas.
Relativa retentionis tempora:
L-4-Nitrophenylalanine Methyl Ester HCl 1.0 (retention tempus circiter 11.4 minuta)
4-Nitro-L-Phenylalanine de 0.4
Toluene de 2.3
Rationes:
In chromatogrammo ex experimento praeparationis, post blank correctionem, apicem toluene ob neglectum.Renuntiatio puritatis chromatographicae, 4-Nitro-L-Phenylalanini contenta et plenaria immunditiae in sample per methodum ordinationem area.