Pramipexole Dihydrochloride Monohydrate CAS 191217-81-9 Assay 98.0~102.0%

C10H17N3S·2HCl·H2O 302.26
(S) -2-Amino-4,5,6,7-tetrahydro-6-(propylamino) benzothiazole dihydrochloride monohydrate [191217-81-9].
TANTHAUZO
Pramipexole Dihydrochloride ili ndi NLT 98.0% ndi NMT 102.0% ya C10H19Cl2N3S, yowerengedwa pa maziko a anhydrous.
CHIZINDIKIRO
• A. Infrared Absorption <197A> kapena <197M>
Chiwerengero cha mafunde: <197A>, 3800 cm-1 mpaka 650 cm-1;<197M>, 4000 cm-1 mpaka 600 cm-1
• B. Nthawi yosungirako pachimake chachikulu mu Sample solution ikufanana ndi pramipexole (S-enantiomer) mu System suitability solution mu kuyesa kwa Enantiomeric Purity.
• C. Mayeso Ozindikiritsa-General, Chloride <191>
Chitsanzo: 1 mg/mL ya Pramipexole Dihydrochloride m'madzi
Njira zovomerezeka: Imakwaniritsa zofunikira za mayeso a silver nitrate precipitate
ZOYESA
• Ndondomeko
Yankho A: Sungunulani 9.1 g wa potassium dihydrogen phosphate ndi 5.0 g wa sodium 1-octanesulfonate monohydrate mu 1 L yamadzi.Sinthani ndi phosphoric acid kukhala pH ya 3.0.
Yankho B: Acetonitrile ndi Solution A (1:1)
Diluent: Acetonitrile ndi Solution A (1:4)
Gawo la m'manja: Onani tebulo la gradient pansipa.
Nthawi (mphindi) Yankho A (%) Yankho B (%)
0 6040
15 2080
15.1 60 40
20 6040
Njira yothetsera vutoli: 1.5 mg/mL ya USP Pramipexole Dihydrochloride RS ndi 0.8 mg/mL ya USP Pramipexole Related Compound A RS mu Diluent
Njira yothetsera: 1.5 mg/mL ya USP Pramipexole Dihydrochloride RS mu Diluent
Yankho lachitsanzo: 1.5 mg/mL ya Pramipexole Dihydrochloride mu Diluent
Chromatographic system
(Onani Chromatography <621>, Kukwanira Kwadongosolo.)
Njira: LC
Chowunikira: UV 264 nm
Mzere: 4.6-mm × 15-cm;5-µm kunyamula L1
Kutentha kwapakati: 40 ± 5
Kuthamanga: 1.5 mL / min
Kukula kwa jakisoni: 5 µL
Kuyenerera kwadongosolo
Zitsanzo: Njira yothetsera kuyenerera kwadongosolo ndi njira yokhazikika [Zindikirani-Nthawi zosungirako zokhudzana ndi pramipexole A ndi pramipexole ndi za 0.7 ndi 1.0, motsatira.]
Zofunikira zoyenera
Kusamvana: NLT 6.0 pakati pa pramipexole yokhudzana ndi mankhwala A ndi pramipexole, njira yothetsera vuto
Zomwe zimapangidwira: NMT 2.0 ya pramipexole, njira yothetsera kukwanira kwadongosolo
Kupatuka kofananira: NMT 1.0%, njira yokhazikika
Kusanthula
Zitsanzo: Yankho lokhazikika ndi yankho lachitsanzo
Werengani kuchuluka kwa C10H19Cl2N3S mu gawo la Pramipexole Dihydrochloride yotengedwa:
Zotsatira = (rU/rS) × (CS/CU) × (Mr1/Mr2) × 100
rU = kuyankha kwapamwamba kuchokera ku Sample solution
rS = kuyankha kwakukulu kuchokera ku Standard solution
CS = kuchuluka kwa USP Pramipexole Dihydrochloride RS mu Standard solution (mg/mL)
CU = ndende ya Sample solution (mg/mL)
Mr1 = molekyulu yolemetsa ya pramipexole dihydrochloride, 284.26
Mr2 = molecular kulemera kwa pramipexole dihydrochloride monohydrate, 302.26
Njira zolandirira: 98.0% -102.0% pamaziko a anhydrous
ZOCHITSA
Zowonongeka Zachilengedwe
• Zotsalira pakuyatsa <281>: NMT 0.10%
• Zitsulo Zolemera, Njira I <231>
Yankho lokhazikika: Standard Lead Solution, 10 ppm
Yankho lachitsanzo: Phulusa 2 g wa Pramipexole Dihydrochloride mpaka pafupifupi youma, mpweya wochuluka wapezeka.Muziziziritsa zotsalirazo, onjezerani 2.0 mL wa nitric acid wokhazikika ndi madontho asanu a concentrated sulfuric acid, ndipo mosamala lolani kuti utsiwo usinthe.Yatsani pa 500-600 mpaka mpweya utatenthedwa.Kuziziritsa zotsalira, kuwonjezera 4 mL wa 6 M hydrochloric acid, kuphimba crucible, ndi kugaya pa osamba madzi otentha kwa mphindi 15.Kutentha mpaka kuuma.Onjezani dontho limodzi la concentrated hydrochloric acid ndi 10 mL wa madzi otentha, ndi kugaya kwa 2 min zina pamadzi osamba otentha.Onjezani 6 M ammonia solution dropwise mpaka yankho likhala lopanda mchere wamchere, ndipo sinthani ndi 1 M acetic acid ku pH ya 3.0–4.0.Seferani yankho mu botolo la volumetric 25-mL, ndikuthira ndi madzi mpaka 25mL potsuka crucible ndi fyuluta.
Njira zolandirira: NMT 10 ppm
Zowonongeka Zachilengedwe
• Ndondomeko
Yankho A, Solution B, Diluent, Mobile phase, ndi Chromatographic system: Pitirizani monga momwe mukuyendera mu Assay.
Njira yothetsera kuyenerera: 7.5 µg/mL ya USP Pramipexole Dihydrochloride RS ndi 3 µg/mL ya USP Pramipexole Related Compound A RS mu Diluent
Njira yothetsera: 1.5 µg/mL ya USP Pramipexole Dihydrochloride RS mu Diluent
Yankho lachitsanzo: 1.5 mg/mL ya Pramipexole Dihydrochloride mu Diluent
Kuyenerera kwadongosolo
Zitsanzo: Njira yothetsera kuyenerera kwadongosolo ndi njira yokhazikika
Zofunikira zoyenera
Kusamvana: NLT 6.0 pakati pa pramipexole yokhudzana ndi mankhwala A ndi pramipexole, njira yothetsera vuto
Zomwe zimapangidwira: NMT 2.0 ya pramipexole, njira yothetsera kukwanira kwadongosolo
Kupatuka kofananira: NMT 5.0%, njira yokhazikika
Kusanthula
Zitsanzo: Yankho lokhazikika ndi yankho lachitsanzo
Werengani kuchuluka kwa zodetsa zilizonse zomwe zatengedwa pa Pramipexole Dihydrochloride:
Zotsatira = (rU/rS) × (CS/CU) × (Mr1/Mr2) × 100
rU = kuyankha kwakukulu kwa zodetsa zilizonse kuchokera ku Sample solution
rS = kuyankha kwakukulu kwa pramipexole kuchokera ku Standard solution
CS = kuchuluka kwa USP Pramipexole Dihydrochloride RS mu Standard solution (mg/mL)
CU = kuchuluka kwa pramipexole dihydrochloride monohydrate mu Sample solution (mg/mL)
Mr1 = molekyulu yolemetsa ya pramipexole dihydrochloride, 284.26
Mr2 = molecular kulemera kwa pramipexole dihydrochloride monohydrate, 302.26
Zovomerezeka zovomerezeka
Zodetsedwa zapayekha: Onani Table 1.
Zonyansa zonse: NMT 0.5%
Table 1
Tchulani Zoyenera Kulandila Nthawi Yosunga Nthawi, NMT (%)
Pramipexole propionamidea 0.5 0.15
Pramipexole yokhudzana ndi mankhwala Ab 0.7 0.15
Pramipexole 1.0 -
N-Propylpramipexolec 1.4 0.15
Pramipexole dimerd 1.7 0.15
Chidetso china chilichonse chosadziwika - 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-Methylpentane-1,3-diyl] bis (4,5,6,7-tetrahydrobenzothiazole-2,6-diamine).Ichi ndi dimer ya pramipexole (kusakaniza kwa ma isomers anayi zotheka).
MAYESO AKE
• Kutsimikiza kwa Madzi, Njira I <921>: NLT 4.5% ndi NMT 6.5%
• Enantiomeric Purity
Gawo lam'manja: n-Hexane, mowa wopanda madzi, ndi diethylamine (850:150:1)
Kuyenerera kwadongosolo kwa stock solution: 1 mg/mL iliyonse ya USP Pramipexole Dihydrochloride RS ndi USP Pramipexole Yogwirizana Compound D RS mu mowa wopanda madzi.
Njira yothetsera kuyenerera: 0.01 mg/mL iliyonse ya USP Pramipexole Dihydrochloride RS ndi USP Pramipexole Related Compound D RS kuchokera ku System suitability stock solution in Mobile phase
Njira yothetsera masheya: 2.0 mg/mL ya USP Pramipexole Related Compound D RS mu mowa wopanda madzi
Yankho lokhazikika: 1.5 µg/mL ya USP Pramipexole Yogwirizana Compound D RS mu gawo la Mobile
Yankho lachitsanzo: 0.3 mg/mL, yokonzedwa ndi kusungunula mlingo woyenera wa Pramipexole Dihydrochloride mu 25% ya botolo la mowa wopanda madzi ndi kuchepetsedwa ndi Mobile phase mpaka voliyumu.
Chromatographic system
(Onani Chromatography 621, System Suitability.)
Njira: LC
Chowunikira: UV 254 nm
Mzere: 4.6-mm × 25-cm;10-µm kunyamula L51
Kuthamanga: 1.5 mL / min
Kukula kwachitsanzo: 75µL
Kuyenerera kwadongosolo
Zitsanzo: Njira yothetsera vutoli [Zindikirani-Nthawi zosungirako zokhudzana ndi pramipexole D (R-enantiomer) ndi pramipexole (S-enantiomer) ndi 0.5 ndi 1.0, motsatira.]
Zofunikira zoyenera
Kusamvana: NLT 5.0 pakati pa pramipexole yokhudzana ndi mankhwala D ndi pramipexole, njira yothetsera kuyenerera
Chovala chamchira: NMT 2.4 ya pramipexole, yankho loyenera la System
Kusanthula
Zitsanzo: Yankho lokhazikika ndi yankho lachitsanzo
Werengani kuchuluka kwa mankhwala okhudzana ndi pramipexole D mu gawo la Pramipexole Dihydrochloride yotengedwa:
Zotsatira = (rU/rS) × (CS/CU) × 100
rU = kuyankha kwakukulu kwa pramipexole yokhudzana ndi mankhwala D kuchokera ku Sample solution
rS = kuyankha kwakukulu kwa pramipexole yokhudzana ndi mankhwala D kuchokera ku Standard solution
CS = ndende ya pramipexole yokhudzana ndi mankhwala D mu Standard solution (mg/mL)
CU = ndende ya Sample solution (mg/mL)
Njira zolandirira: NMT 1.0% ya pramipexole yokhudzana ndi pawiri D
• Malire a Palladium
[Zindikirani-Yesani izi ngati palladium ndi chodetsa chodziwika bwino.]
Kutsika: 0.1 M hydrochloric acid
Yankho lokhazikika: 40 µg/L ya palladium mu Diluent, kuchokera ku palladium yokhazikika yopezeka pamalonda yamayamwidwe a atomiki/madzi a m'magazi ophatikizana mochititsa chidwi.[Zindikirani—Konzani mwatsopano yankho ili monga likufunikira pa tsiku logwiritsa ntchito.]
Yankho lachitsanzo: Ku 0.5 g wa Pramipexole Dihydrochloride mu botolo la volumetric 50-mL onjezerani 5.00 mL ya 1 M hydrochloric acid, ndi kusungunula ndi kutentha.Kuzizira kutentha kwa chipinda, ndi kuchepetsa ndi madzi kuti voliyumu.
Mikhalidwe ya Spectrometric
(Onani Spectrophotometry ndi Light-Scattering 851).
Njira: Atomic mayamwidwe spectrophotometry
Kusanthula kwakutali: Palladium emission line pa 247.6 nm
Nyali: Hollow cathode
Gwero la Atomization: Graphite ng'anjo.[Zindikirani—Tsatirani ndondomeko zotsatiridwa ndi wopanga.]
Kukula kwachitsanzo: 20µL
Zopanda kanthu: Zopanda kanthu
Kuyenerera kwadongosolo
Chitsanzo: Njira yothetsera
Zofunikira zoyenera
Kuchokera: NLT 0.034
Kusanthula
Zitsanzo: Yankho lokhazikika ndi yankho lachitsanzo
Dziwani kuchuluka kwa palladium mu Sample solution ndi njira yowonjezera yowonjezera.
Njira zolandirira: NMT 5 ppm
ZOWONJEZERA ZOFUNIKA
• Kupaka ndi Kusunga: Sungani m’zotengera zotsekedwa bwino, zotetezedwa ku chinyezi ndi kuwala.
• USP Reference Standards 11
USP Pramipexole Dihydrochloride RS Dinani kuti muwone Kapangidwe
USP Pramipexole Related Compound A RS
(S) -4,5,6,7-Tetrahydrobenzothiazole-2,6-diamine.
Chithunzi cha C7H11N3S 169.25
USP Pramipexole Related Compound D RS
(R) -2-Amino-4,5,6,7-tetrahydro-6-(propylamino)benzothiazole.
Chithunzi cha C10H17N3S 211.33