L-Isoleucine CAS 73-32-5 (H-Ile-OH) Assy 98.5~ 101.0%

L-Isoleucinus (H-Ile-OH) (CAS: 73-32-5) AJI 97 Methodus test
Lepidium sativum: Confer spectrum ultrarubrum effusio exempli cum illa regulae per modum discus bromide potassium.
Specific rotationis [α]20/D: Aridae Sample, C=4, 6mol/L HCl
Status Solutionis (Transmittance): 0.5g in 10ml 1mol/L, HCl spectrophotometri, 430nm, 10nm cellulae crassitudinis.
Chloride (Cl): 0.7g, A-1, ref: 0.40ml of 0.01mol/L HCl
Sulfate (SO4): 1.2g, (1), ref: 0.50ml ex 0.005mol/L H2SO4
Ferrum (Fe): 1.5g, (1), ref: 1.5ml of Iron Std.(0.01mg/ml)
Metalla gravia (Pb): 2.0g, (1), solve calefaciendo, ref: 2.0ml of Pb Std.(0.01mg/ml)
Arsenicum (As2O3): 2.0g, (1), ref: 2.0ml de As2O3 Std.
Alia Amino Acides: Test Sample: 50μg, B-6-a, imperium: L-Ile 0.25μg
Damnum in remittit: ad 105℃ pro 3 horis.
Intenta: Specimen siccatum, 130mg, (3), 3ml acidum formic, 50ml acidi glacialis acetici, 0.1mol/L HCLO4 1ml=13.117mg C6H13NO2
PH Test: 0.5g in 20ml de H2O

L-Isoleucine (H-Ile-OH) (CAS: 73-32-5) USP35 Test methodus
DEFINITIO
Isoleucina continet NLT 98.5% et NMT 101,5% L-Isoleucinae (C6H13NO2), quae in fundamento siccato computatur.
IDENTIFICATIO
A. INFRARED HAUSTUS <197K>
TEMPTATIO
MODO PROCEDENDI
Sample: 130 mg de Isoleucine
Blank: Misce 3 mL acidi formici et 50 mL acidi glacialis.
Systema titrimetricum
(Vide Titrimetrium<541>)
Modus: Direct titration
Titrant: 0.1 N acidum perchloricum VS
Endpoint deprehensio: Potentiometric
Analysis: Solve Sample in 3 mL acidi formici et 50mL acidi glacialis.Titrate apud Titrant.Blank determinationem praestare.
Calculare recipis Isoleucines (C 6H13NO2) in Sample desumptum:
Exitus = {[(VS-VB) x N x F]/W} x100
VS = Titrant volumen consumpsit Sample (mL)
VB= Titrant volumen absumptum a Blank (mL)
N = re normalitatis de Titrant (mEq/mL)
F= aequivalentia factor, 131.2 mg/mEq
W = Sample pondus (medicamentum)
Acceptatio criteria: 98.5%~ 101.5% in fundamento exsiccato
IMPURITIES
RESIDUEON IGNIS <281>: NMT 0.3%
CHLORIDE ET SULFATE, CHLORIDE <221>
Solutio mensurae: 0.50mL de acido hydrochlorico N 0.020
Sample: 0.73g de Isoleucine
Acceptatio criteria: NMT 0.05%
CHLORIDE ET SULFATE, Sulfate <221>
Solutio Standard: 0.10mL ex 0.020 Acidi sulphurici N
Sample: 0.33g de Isoleucine
Acceptatio criteria: NMT 0.03%
FERRUM <241>: NMT 30ppm
Delere sequentia:
GRAVALIS METALS, Methodus I <231>: NMT 15ppm .
COGNATUS COMPONS
Solutio idoneitatis systematis: 0.4mg/mL utriusque USP L-Isoleucinae RS et USP L-Valine RS in 0.1 N acido hydrochlorico
Solutio mensurae: 0.05mg/mL ex USP L-Isoleucinis RS in 0.1 N acido hydrochlorico.[NOTA-Haec solutio retrahitur aequipollens 0.5% illius solutionis Samplei.]
Sample solutio: 10mg/mL acidum hydrochloricum in 0.1 N
Systema chromatographicum (Vide Chromatographia <621>, chromatographia Thin-Layer.)
Modus: TLC
Adsorbent: 0.25-mm iacuit chromatographico silicae gel mixtionis
Applicationem voluminis: 5μL
Solvendo ratio explicandi: Butyl alcohol, acidum glaciale aceticum, et aqua (3:1:1)
Imbre reagens: 2 mg/mL ninhydrin in mixtione alcoholi butyl et 2N acidi acetici (95:5).
Ratio convenientia
Opportunitas requisita: solutio chromatogramma Systematis convenientia ostendit duas maculas distincte separatas.
Analysis
Exempla: Ratio idoneitatis solutio, solutionis Latin, et solutionis Sample.
Post laminam aer exsiccans, imbre cum Spray gerente, et calor inter 100° et 105° pro 15 min.Discute laminam sub lumine albo.
Criteria acceptationis: Quaelibet macula secundaria solutionis Sample non maior vel intensior est quam macula principalis solutionis Standardi.
Singulae immunditiae: NMT 0.5%
Totalis immunditiae: NMT 2.0%
IN SPECIE TESTS
ROTATIO OPTICALIS, Rotatio Imprimis <781S>
Sample solutio: 40 mg/mL in 6 N acidum hydrochloricum
Criteria acceptationis: +38.9° ad +41.8°
PH <791>
Sample solutio: 10 mg/mL solutionem
Criteria acceptationis: 5.5~7.0
LOSSON DE ARIFICATIONE <731>: Exemplum sicca in 105℃ pro 3 h: amittit NMT 0.3% sui ponderis.
ADDITICIUS REQUISITIS
PACKAGING and storage: Conserva in vasis bene clausis.
USP Reference STANDARDS <XI>
USP L-Isoleucine RS
USP L-Valine RS