Acesulfame K CAS 55589-62-3 Acesulfame potassium puritatis >99.0% (HPLC)

DEFINITIO
Acesulfame Potassium NLT 99.0% continet et NMT 101.0% C4H4NO4SK, in fundamento siccato computatum.
IDENTIFICATIO
• A. ABSORPTION INFRARED <197K>
• B. IDENTIFICATIO TESTIMONIA GENERALIS, Potassium <191>
Sample solutio: 100 mg/mL
Acceptatio criteria: Meets
TEMPTATIO
• MODO PROCEDENDI
Sample: 150 mg
Systema titrimetricum (Vide Titrimetricum <541>)
Modus: Direct titration
Titrant: 0.1 N acidum perchloricum VS
Blank: acidi glacialis acetici 50 mL
Endpoint deprehensio: Potentiometric
Analysis: Disolve Sample in 50 mL acidi glacialis.
Titrate cum acido perchlorico 0.1 N VS.Praestare blank determinatio.
Recipis potassae acesulfami (C4H4NO4SK) in Sample:
Proventus = [(V B) N F 100]/W
V = volumen titrant consumptum Sample (mL)
B = volumen titrant consumptum a Blank (mL)
N = titrant normalitatis (mEq/mL)
F = factor equivalency, 201.2 mg/mEq
W = pondus Sample (medicamentum)
Acceptatio criteria: 99.0% -101.0% in exaruit basis
IMPURITIES
• FINIS FLUORIDE
[NOTA-Usus plasticware per totum hoc test.]
Solutio A: solve 210 g acidi citrici monohydratorum in aquae 400 mL.Adpone ammoniae coactae ad pH 7.0, et aqua dilue ad 1000 mL.
Solutio B: 132 mg/mL ammonium dibasici phosphatis
Solutio C: Suspensio acidi edetici in aquae 500 mL 292 g, hydroxidum ammonium 200 mL adde, hydroxidum ammonium inter 6 et 7 pH compone, et aqua dilutum ad 1000 mL fac.
Solutio quiddam: Misce paria volumina Solutionis A, Solutio B et Solutio C, et hydroxidem ammonium pH 7.5.
Solutio generum stirpis: Expende 0.442 g sodium fluoride, antea 300° pro 12 h exsiccata, in lagena voluminis 1-L, et aqua ad volumen diluta.Repone solutionem in vase plastico clauso.Statim ante usum, fistulae 5 mL solutionis huius in lagena voluminis 100-mL, et aqua ad volumen diluta.Quaelibet mL huius solutionis continet 10µg fluoride ionis.
Solutio Standard A: Misce 0.5 mL solutionis stirpis Standardi et 15.0 mL solutionis Buffer, et aqua diluti ad 50mL.
Solutio Standard B: Misce 1.0 mL solutionis latini stirpis et 15.0 mL solutionis Buffer, et aqua diluto ad 50mL.
Solutio Standard C: Misce 1.5 mL solutionis stirpis Standardi et solutionis Bufferae 15.0 mL, et aqua diluto ad 50mL.
Solutio Standard D: Misce 3.0 mL solutionis latini stirpis et 15.0 mL solutionis Buffer, et aqua diluto ad 50mL.
Sample solutio: Lagena voluminis L-mL adde 3 g Acesulfame potassii.Solve in aqua, solve solutionem Buffer 15.0 mL, et aqua diluto ad volumen.
Analysis
Exempla: Solutio Latin A, Solutio Latin B, Solutio Standard C, Solutio Standard D, ac Solutio Sample
Concomitanter metiuntur potentiae (cf. Titrimetry <541>) in mV, solutionum Latinarum et solutionum Sample, cum metro congruo instructum cum electrode fluoride-specificatione et chloride argenteo electrode referente.Cum mensuris capiendis, solutionem in 25-mL compensatoris transferas, et electrodes immergas.Insert polytef-cotatam vectem in potorio, poculum in excitante magnetico cacumine insulato habentem et commovere permittite donec aequilibrium attingatur (1-2 min).Accende intus stupam, et electrodes inter mensuras exsiccas, cavens ne crystallum in electrode fluoride speciali Ione scalpas.Metire potentiam solutionis utriusque Standardi, et concentratio fluorida, in µg/mL, versus potentialem, in mV, in charta semilogarithmica dispone.Potentialem solutionis Sample metiaris et de intentione fluoridis curvae vexillum determina, in µg/mL.
Compute, in ppm, de fluoride in parte Acesulfame potassae sumptae;
Proventus = (V C/W)
V = volumen solutionis Sample (mL)
C = concentratio fluoride in solutione Sample, e curva norma (mg/mL)
W = pondus Acesulfame potassium sumptum ad solutionem parandam Sample (g)
Acceptatio criteria: NMT 3 ppm
• METALS GRAVIUS, Methodus I <231>: NMT 10 ppm .
• CHROMATOGRAPHICA PUDICITIA
Solutio A: 3.3 mg/mL tetrabutylammonium hydrogenii sulfatis
Mobile phase: Acetonitrile et Solutio A (2:3).
Solutio ratio congruentia: 2 µg/mL singulae USP acesulfame potassae RS et ethylparaben
Solutio Standard: 0.2 µg/mL of USP Acesulfame potassium RS
Sample solutio: 10 mg/mL
Systema chromatographicum
(Vide Chromatographiam <621>, Ratio idoneitatis.)
Modus: LC
Detector: UV 227 nm
Columna: 4.6-mm × 25-cm;5-µm stipare L1
Fluunt rate: 1 mL/min
Iniectio amplitudo: 20 µL
Ratio convenientia
Sample: Ratio idoneitatis solutionis
Convenientia requisita
Resolutio: NLT 2 inter acesulfamum potassium et ethylparaben .
Analysis
Exempla: Standard solution et Sample solutionem
Nota chromatogrammata pro temporis spatio NLT 3 temporibus retentionis tempus apicem potassii acesulfami, et responsiones iugis aream metientes.
Re- gulae acceptationis: Responsio cuiuslibet apici ad tempus retentionis praeterquam quod solutionis acesulfamae potassii e sample solution non excedit responsionem acesulfami potassii apicem e solutione vexillifer (0.002%).
IN SPECIE TESTS
• ACIDITAS VEL ALKALINITY
Sample solutio: 4.0 g in 20 mL aquae dioxide-liberi
Analysis: Adde 0.1 mL de bromothymol caeruleo TS.Si solutio flavus est, titrate cum 0.01 N sodium hydroxidum caeruleum efficit colorem.Si solutio caerulea est, titrate cum acido 0.01 N hydrochloride ad colorem luteum producendum.
Re- gulae acceptationis: NMT 0.2 mL ex 0.01 N hydroxidum sodium vel NMT 0.2 mL ex Acidum hydrochloricum 0.01 N requiritur.
• AMISSIONE DE ARIFICATIONE <731>: exemplum sicca apud 105° pro 3 h: amittit NMT 1.0% sui ponderis.
ADDITICIUS REQUISITIS
• FASCICULUS ET RECONCILIO: In vase bene clauso conserva et a luce protege.Repono in locus temperatus.
USP Reference STANDARDS <XI>
USP Acesulfame Potassium RS