Pramipexole dihydrochloridis Monohydratorum CAS 191217-81-9 Intende 98.0~ 102.0%

C10H17N3S·2HCl·H2O 302.26
(S)-2-Amino-4,5,6,7-tetrahydro-6-(propylamino)benzothiazole dihydrochloride monohydrato [191217-81-9].
DEFINITIO
Pramipexolum dihydrochloridum NLT 98.0% continet et NMT 102.0% C10H19Cl2N3S, in fundamento anhydroso computatum.
IDENTIFICATIO
• A. Absorptio infrared <197A> seu <197M>
Undo numerus ambitus: <197A>, 3800 cm-1 ad 650 cm-1;<197M>, 4000 cm-1 ad 600 cm-1
• B. Retentionis tempus solutionis maioris cacuminis in Sample solutioni respondet pramipexoli (S-enantiomer) in solutione idoneitatis systematis in probatione puritatis Enantiomeric.
• C. sativum Testi-generalis, Chloride <191>
Sample: 1 mg/mL Pramipexole dihydrochloridis in aqua
Acceptatio criteria: Nitrata argenti probatio praepropera occurrit
TEMPTATIO
• De modo procedendi
Solutio A: solve 9.1 g phosphas potassii dihydrogenis et 5.0 g monohydratorum natrii 1-octanesulfonatis in 1 L aquae.Acidum phosphoricum ad pH 3.0 compone.
Solutio B: Acetonitrile et Solutio A (1. 1).
Diluent: Acetonitrile et Solutio A (1:4).
Mobile tempus: Vide infra mensam gradientem.
Solutio tempus (min) Solutio A (%) Solutio B (%)
0 60 40
15 20 80
15.1 60 40
20 60 40
Solutio aptabilitas systematis: 1.5 mg/mL USP Pramipexoli dihydrochloridis RS et 0,8 mg/mL of USP Pramipexole Related Compone A RS in Diluent
Solutio Standard: 1.5 mg/mL USP Pramipexoli dihydrochloridis RS in Diluent
Sample solutio: 1.5 mg/mL Pramipexoli dihydrochloridis in diluentia
Systema chromatographicum
(Vide Chromatographiam <621>, Ratio idoneitatis.)
Modus: LC
Detector: UV 264 nm
Columna: 4.6-mm × 15-cm;5-µm stipare L1
columna temperatura: 40 ± 5
Fluunt rate: 1.5 mL/min
Iniectio amplitudo: 5 µL
Ratio convenientia
Exempla: Ratio idoneitatis solutionis solutionis Standardi [Nota-retentionis relativa tempora pro pramipexole affinis compositi A et pramipexoli sunt circiter 0.7 et 1.0, respective.]
Convenientia requisita
Resolutio: NLT 6.0 inter pramipexolum compositum A et pramipexolum relatum, solutio ratio convenientiae
Tailing factor: NMT 2.0 pro pramipexole, ratio solutionis idoneitatis
Vexillum relativum declinationis: NMT 1.0%, Standard solution
Analysis
Exempla: Standard solution et Sample solutionem
Calculare recipis C10H19Cl2N3S in portione Pramipexoli dihydrochloridis sumpti;
Proventus = (rU/rS) (CS/CU) (Mr1/Mr2) 100
rU = apicem responsio ex Sample solutione
rS = apicem responsio ex solutione Latin
CS = intentio USP Pramipexole dihydrochloride RS in solutione Standard (mg/mL)
CU = retrahitur Sample solutionis (mg/mL)
Mr1 = pondus hypotheticum pramipexoli dihydrochloridis, 284.26
Mr2 = pondus hypotheticum monohydratorum pramipexoli dihydrochloridis, 302,26
Acceptatio criteria: 98.0% -102.0% in anhydrous basis
IMPURITIES
Inorganic immunditias
• Residuum in Ignitione <281>: NMT 0.10%
• Metalla gravia, Methodus I <231>
Solutio Standard: Solutio in Latin Duc, 10 ppm
Sample solutio: Cinerum 2 g Pramipexoli dihydrochloridis usque dum massam carbonised paene aridam obtinet.Residuum refrigerant, adde acidi nitrici concentrati 2.0 mL et 5 guttas acidi sulphurici concentrati, et fumos diligenter evolvere permittunt.D-600 accende donec carbonis totaliter exuratur.Residuum refrigerant, addunt 4 mL acidum hydrochlorici 6 M, testae tegunt, et in aqua ferventi lavacrum 15 min concoquunt.Exalat ad siccitatem.Adde unam guttam acidi hydrochlorici concentrati et 10 mL aquae calidae, et plura 2 min in balneum aquae fervidae concoquere.Solutio ammoniaci 6 M guttatim adde donec solutio alcalina sit infirma, et cum 1 M acidum aceticum componas ad pH 3.0-4.0.Solutio sparguntur in lagena voluminis 25-mL, et aqua diluunt ad 25 mL lavando uas et colum.
Acceptatio criteria: NMT 10 ppm
Impurities organica
• De modo procedendi
Solutio A, Solutio B, Diluente, Phase mobile, et systema chromatographicum: Perge ut fertur in primordio.
Solutio aptabilitas systematis: 7.5 µg/mL USP Pramipexoli dihydrochloridis RS et 3 µg/mL USP Pramipexoli Compositae A RS in Diluent.
Solutio Standard: 1.5 μg/mL USP Pramipexoli dihydrochloridis RS in Diluent
Sample solutio: 1.5 mg/mL Pramipexoli dihydrochloridis in diluentia
Ratio convenientia
Exempla: Ratio idoneitatis solutionis et solutionis Standardi
Convenientia requisita
Resolutio: NLT 6.0 inter pramipexolum compositum A et pramipexolum relatum, solutio ratio convenientiae
Tailing factor: NMT 2.0 pro pramipexole, ratio solutionis idoneitatis
Vexillum relativum declinationis: NMT 5.0%, Standard solution
Analysis
Exempla: Standard solution et Sample solutionem
Calculare recipis immunditiam singularem in portione Pramipexoli dihydrochloridis sumptae;
Proventus = (rU/rS) (CS/CU) (Mr1/Mr2) 100
rU = apicem responsionis cuiusque immunditiae ex Sample solutione
rS = apicem responsionis pramipexole ex solutione Standard
CS = intentio USP Pramipexole dihydrochloride RS in solutione Standard (mg/mL)
CU = intentio pramipexoli dihydrochloridis monohydratorum in Sample solutione (mg/mL)
Mr1 = pondus hypotheticum pramipexoli dihydrochloridis, 284.26
Mr2 = pondus hypotheticum monohydratorum pramipexoli dihydrochloridis, 302,26
Criteria acceptatio
Individua Impudicitia: Vide Mensam Impuritas 1 .
Totalis immunditiae: NMT 0.5%
De immunitate Tabula 1
Nomen relativum Retentionis Tempus acceptationis Criteria, NMT (%)
Pramipexole propionamideum 0.5 0.15
Pramipexole affinis compositi Ab 0.7 0.15
Pramipexole 1.0 —
N-Propylpramipexolec 1.4 0.15
Pramipexole dimerd 1.7 0.15
Quaelibet alia individua immunditia unidentificata - 0.10
a (S)-N-(2-Amino-4,5,6,7-tetrahydrobenzothiazol-6-yl)propionamide.
b (S)-4,5,6,7-Tetrahydrobenzothiazole-2,6-diamine.
c (S)-2,6-Dipropylamino-4,5,6,7-tetrahydrobenzothiazole.
d N6,N6'-[2-Methylpentanum-1,3-diyl]bis(4,5,6,7-tetrahydrobenzothiazole-2,6-diamine).Hoc dimer pramipexole est (mistura quatuor isomers fieri).
IN SPECIE TESTS
• Determinatio aquae, Methodus I <921>: NLT 4.5% et NMT 6.5%
• Puritas Enantiomeric
Mobile tempus: n-Hexane, alcohol dehydratum, et diethylamine (850:150:1)
Systema idoneitatem stirpem solutionis: 1 mg/mL singulae USP Pramipexole dihydrochloride RS et USP Pramipexole Compositi D RS in alcohole dehydrato coniuncti.
Solutio aptabilitas systematis: 0.01 mg/mL singulae USP Pramipexole dihydrochloridi RS et USP Pramipexole Composita D RS ex solutione systematis idoneitatis stirpis in tempore Mobili
Standard stock solution: 2.0 mg/mL of USP Pramipexole Related Compone D RS in alcohole siccitatis
Solutio Standard: 1.5 µg/mL of USP Pramipexole Composito D RS in Mobili periodo
Sample solutio: 0,3 mg/mL, praeparata solvendo aptam quantitatem pramipexoli dihydrochloridi ponderatam in 25% voluminis ampullae alcoholi dehydratae et diluentis cum tempore ad volumen mobile.
Systema chromatographicum
(Vide Chromatographia 621, Ratio Suitability).
Modus: LC
Detector: UV 254 nm
Columna: 4.6-mm × 25-cm;10-µm stipare L51
Fluunt rate: 1.5 mL/min
Magnitudo: 75 µL
Ratio convenientia
Exempla: Solutio idoneitatis systematis [Nota-retentio relativa temporum ad pramipexolum compositum D (R-enantiomer) et pramipexolum (S-enantiomer) sunt 0.5 et 1.0, respective.]
Convenientia requisita
Resolutio: NLT 5.0 inter pramipexolum compositum D et pramipexolum relatum, solutio ratio convenientiae
Tailing factor: NMT 2.4 pro pramipexole, ratio solutionis idoneitatis
Analysis
Exempla: Standard solution et Sample solutionem
Calculare recipis pramipexoli compositi D relati in portione Pramipexoli dihydrochloridis sumpti;
Proventus = (rU/rS) (CS/CU) 100
rU = apicem responsionis pramipexoli compositi D relati ex solutione Sample
rS = cacumen responsionis pramipexole affinis compositi D ex solutione Standard
CS = retrahitur pramipexole affinis compositi D in solutione Standard (mg/mL)
CU = retrahitur Sample solutionis (mg/mL)
Criteria acceptationis: NMT 1.0% pramipexoli compositi D . relati
• Palladii modus
[Nota hoc experimentum praestare si Palladium sit notum inorganicae immunditiae.]
Diluent: 0.1 M acidum hydrochloricum
Solutio Standard: 40 µg/L palladii in Diluent, ex commercio solutionis normae Palladii praesto pro effusio atomica / inductive plasma copulatum.Hanc solutionem nuper usui necessariam praeparet.]
Sample solutio: Ad 0.5 g pramipexoli dihydrochloridis in L-mL lagena voluminis 5.00 mL ex 1 M acidum hydrochloricum adde et cum calefactione solvendum.Frigidus est locus temperatus, et aqua diluto ad volumen.
Spectrometric conditiones
(See Spectrophotometry and Light-Scattering 851).
Modus: Effusio atomica spectrophotometry
Analytica necem: Palladium emissio lineae ad 247.6 nm
Lucerna: cavum cathode
Fons atomisationum: Graphite fornax.[Nota—sequere sequentia programmandi artificis commendatur.]
Magnitudo exempli: 20 µL
Blank: Diluent
Ratio convenientia
Sample: Latin solution
Convenientia requisita
Absorbance: NLT 0.034
Analysis
Exempla: Standard solution et Sample solutionem
Determinare intentionem Palladii in Sample solutione per modum normae adiectae.
Acceptatio criteria: NMT 5 ppm
ADDITICIUS REQUISITIS
• Packaging and storage : Conserva in vasis bene clausis , ab humido et lumine munitus .
• USP Reference signa 11
USP Pramipexole Dihydrochloride RS Click to View Structure
USP Pramipexole Related Compone A RS
(S)-4,5,6,7-Tetrahydrobenzothiazole-2,6-diamine.
C7H11N3S 169.25
USP Pramipexole Related Compone D RS
(R) -2-Amino-4,5,6,7-tetrahydro-6-(propylamino)benzothiazole.
C10H17N3S 211.33