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].
Qeexitaan
Pramipexole Dihydrochloride wuxuu ka kooban yahay NLT 98.0% iyo NMT 102.0% ee C10H19Cl2N3S, oo lagu xisaabiyo ku salaysan anhydrous.
AQOONSIGA
• A. Nuugista Infrared <197A> ama <197M>
Nambarka hirarka kala duwan: <197A>, 3800 cm-1 ilaa 650 cm-1;<197M>, 4000 cm-1 ilaa 600 cm-1
B. Waqtiga haynta ee ugu sarraysa ee xalka Tusaalaha waxay u dhigantaa tan pramipexole (S-enantiomer) ee xalka ku habboonaanta Nidaamka ee imtixaanka Enantiomeric Purity.
C. Tijaabada Aqoonsiga-Guud, Chloride <191>
Tusaalaha: 1 mg/ml ee Pramipexole Dihydrochloride ee biyaha
Shuruudaha aqbalaadda: Buuxiyay shuruudaha tijaabada nitrate-ka qalinka ah
ASSAY
Habka
Xalka A: Kala diri 9.1 g oo ah potassium dihydrogen phosphate iyo 5.0 g of sodium 1-octanesulfonate monohydrate 1 L oo biyo ah.Ku hagaaji phosphoric acid una beddel pH 3.0.
Xalka B: Acetonitrile iyo Xalka A (1:1)
Dareeraha: Acetonitrile iyo Xalka A (1:4)
Marxaladda guurguura: Eeg shaxda gradient ee hoose.
Waqtiga (min) Xalka A (%) Xalka B (%)
060 40
15 20 80
15.1 60 40
20 60 40
Xalka ku habboonaanta nidaamka: 1.5 mg/mL ee USP Pramipexole Dihydrochloride RS iyo 0.8 mg/mL ee USP Pramipexole Laxidhiidha Iskuxidhka A RS ee Diluent
Xalka caadiga ah: 1.5 mg/mL oo ah USP Pramipexole Dihydrochloride RS ee dareeraha
Xalka muunada: 1.5 mg/ml ee Pramipexole Dihydrochloride ee dareeraha ah
Nidaamka Chromatographic
(Fiiri Chromatography <621>, Habboonaanta Nidaamka.)
Habka: LC
Baaraha: UV 264 nm
Tiirka: 4.6-mm × 15-cm;5-µm xirmo L1
Heerkulka tiirka: 40 ± 5
Heerka socodka: 1.5 ml/min
Cabbirka duritaanka: 5µL
Ku habboonaanta nidaamka
Tusaalooyinka: Xalka ku habboonaanta nidaamka iyo xalalka caadiga ah [Xusuusin-Wakhtiyada sii haynta qaraabada ah ee isku xidhka pramipexole ee A iyo pramipexole waa qiyaastii 0.7 iyo 1.0, siday u kala horreeyaan.]
Shuruudaha ku habboonaanta
Xallinta: NLT 6.0 inta u dhaxaysa barxadda la xidhiidha pramipexole A iyo pramipexole, Xalka ku habboonaanta nidaamka
Qodobka dabada: NMT 2.0 ee pramipexole, nidaamka ku habboonaanta xalka
Isbeddelka heerka qaraabada: NMT 1.0%, Xalka caadiga ah
Falanqaynta
Tusaalooyinka: Xalka caadiga ah iyo xalalka muunada
Xisaabi boqolkiiba C10H19Cl2N3S ee qaybta Pramipexole Dihydrochloride ee la qaatay:
Natiijadu = (rU/rS) × (CS/CU) × (Mr1/Mr2) × 100
rU = jawaabta ugu sarreysa ee xalka Tusaalaha
rS = jawaabta ugu sarreysa ee xalalka caadiga ah
CS = fiirsashada USP Pramipexole Dihydrochloride RS ee xalka caadiga ah (mg/mL)
CU = fiirsashada saamiga saamiga (mg/mL)
Mr1 = Miisaanka molecular ee pramipexole dihydrochloride, 284.26
Mr2 = Miisaanka molecular ee pramipexole dihydrochloride monohydrate, 302.26
Shuruudaha aqbalaadda: 98.0%-102.0% ku salaysan anhydrous
XANUUNKA
wasakhda aan noolaha ahayn
• Hadhaaga dabka <281>: NMT 0.10%
• Biraha culus, Habka I <231>
Xalka caadiga ah: Xalka Lead ee caadiga ah, 10 ppm
Xalka Tusaalaha: Ash 2 g oo ah Pramipexole Dihydrochloride ilaa inta la helayo cuf kaarboonaysan oo ku dhow qalalan.Qabo hadhaaga, ku dar 2.0 ml oo nitric acid ah iyo 5 dhibcood oo sulfuric acid ah, si taxadar lehna u ogolow qiiqa inuu kobco.Shid 500-600 ilaa kaarboonku gabi ahaanba ka gubto.Qabooji haraaga, ku dar 4 mL oo ah 6 M hydrochloric acid, dabool qoloflaha, oo dheefshiidka qubeyska biyaha karkaraya 15 daqiiqo.Uumi u bixi qallayl.Ku dar hal dhibic oo ah hydrochloric acid iyo 10 ml oo biyo kulul ah, oo dheefshiido 2 daqiiqo oo kale qubeyska biyaha karkarinta.Ku dar 6 M xal ammonia hoos u dhac ilaa uu xalku daciif yahay alkaline, oo ku hagaaji 1 M acetic acid pH of 3.0-4.0.Ku sifee xalka 25-mL weel mug leh, oo ku mil biyo ilaa 25 mL adiga oo dhaqaya weelka iyo shaandhada.
Shuruudaha aqbalaadda: NMT 10 ppm
Waxyeellada dabiiciga ah
Habka
Xalka A, Xalka B, Diluent, Marxaladda Mobilka, iyo Nidaamka Chromatographic: U wad sida lagu faray Assay.
Xalka ku habboonaanta nidaamka: 7.5 µg/ml ee USP Pramipexole Dihydrochloride RS iyo 3 µg/mL ee USP Pramipexole Isku-xidhka Laxidhiidha A RS ee Diluent
Xalka caadiga ah: 1.5 µg/ml ee USP Pramipexole Dihydrochloride RS
Xalka muunada: 1.5 mg/ml ee Pramipexole Dihydrochloride ee dareeraha ah
Ku habboonaanta nidaamka
Tusaalooyinka: Xalka ku habboonaanta nidaamka iyo xalalka caadiga ah
Shuruudaha ku habboonaanta
Xallinta: NLT 6.0 inta u dhaxaysa barxadda la xidhiidha pramipexole A iyo pramipexole, Xalka ku habboonaanta nidaamka
Qodobka dabada: NMT 2.0 ee pramipexole, nidaamka ku habboonaanta xalka
Isbeddel heerka qaraabada ah: NMT 5.0%, Xalka caadiga ah
Falanqaynta
Tusaalooyinka: Xalka caadiga ah iyo xalalka muunada
Xisaabi boqolleyda wasakh kasta oo shakhsi ah ee qaybta Pramipexole Dihydrochloride ee la qaatay:
Natiijadu = (rU/rS) × (CS/CU) × (Mr1/Mr2) × 100
rU = jawaabta ugu sarreysa ee wasakh kasta oo ka timaadda xalka Tusaalaha
rS = jawaabta ugu sarreysa ee pramipexole oo ka timid xalalka caadiga ah
CS = fiirsashada USP Pramipexole Dihydrochloride RS ee xalka caadiga ah (mg/mL)
CU = fiirsashada pramipexole dihydrochloride monohydrate ee xalka Tusaalaha (mg/mL)
Mr1 = Miisaanka molecular ee pramipexole dihydrochloride, 284.26
Mr2 = Miisaanka molecular ee pramipexole dihydrochloride monohydrate, 302.26
Shuruudaha aqbalaadda
Wasakhda Shakhsiyeed: Eeg Shaxda 1aad ee wasakhda.
Wadarta wasakhda: NMT 0.5%
Shaxda wasakhaysan 1
Magaca Shuruudaha Ogolaanshaha Wakhtiga Haynta Qaraabo, NMT (%)
Pramipexole propionamidea 0.5 0.15
Xarunta Pramipexole ee la xidhiidha Ab 0.7 0.15
Pramipexole 1.0 —
N-Propylpramipexolec 1.4 0.15
Pramipexole dimerd 1.7 0.15
Mid kasta oo kale oo aan la aqoonsan shakhsi ahaan wasakhnimo - 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).Kani waa dimer of pramipexole (isku dar ah afar isomers oo suurtagal ah).
IMTIXAANO GAAR AH
• Go'aaminta Biyaha, Habka I <921>: NLT 4.5% iyo NMT 6.5%
• Nadiifinta Enantiomeric
Marxaladda wareegta: n-Hexane, khamriga fuuqbaxay, iyo diethylamine (850:150:1)
Xalka saamiga ku habboonaanta nidaamka: 1 mg/mL midkiiba USP Pramipexole Dihydrochloride RS iyo USP Pramipexole Compound D RS ee khamriga fuuqbaxay
Xalka ku habboonaanta nidaamka: 0.01 mg/mL midkiiba USP Pramipexole Dihydrochloride RS iyo USP Pramipexole Combound D RS oo ka yimid nidaamka ku habboonaanta saamiga ee wejiga mobilada
Xalka saamiga caadiga ah: 2.0 mg/mL ee USP Pramipexole La Xiriira Isku-dhafka D RS ee khamriga fuuqbaxay
Xalka caadiga ah: 1.5 µg/ml ee USP Pramipexole La Xiriira Isku-dhafka D RS ee wajiga mobaylka
Tusaalaha xalalka: 0.3 mg/mL, oo ​​loo diyaariyey iyadoo lagu milmay tiro miisaaman oo ku habboon Pramipexole Dihydrochloride 25% ee mugga galaaska khamriga fuuqbaxay iyo lagu milo wejiga mobilada ilaa mugga.
Nidaamka Chromatographic
(Fiiri Chromatography 621, Habboonaanta Nidaamka.)
Habka: LC
Baaraha: UV 254 nm
Tiirka: 4.6-mm × 25-cm;10-µm xirmo L51
Heerka socodka: 1.5 ml/min
Cabbirka Tusaalaha: 75µL
Ku habboonaanta nidaamka
Tusaalooyinka: Xalka ku habboonaanta nidaamka [Fiiro gaar ah-Wakhtiyada haynta qaraabada ah ee isku xidhka pramipexole ee la xidhiidha D (R-enantiomer) iyo pramipexole (S-enantiomer) waa 0.5 iyo 1.0, siday u kala horreeyaan.]
Shuruudaha ku habboonaanta
Xallinta: NLT 5.0 inta u dhaxaysa xarunta pramipexole ee la xidhiidha D iyo pramipexole, Xalka ku habboonaanta nidaamka
Qodobka dabada: NMT 2.4 ee pramipexole, Nidaamka ku habboonaanta xalka
Falanqaynta
Tusaalooyinka: Xalka caadiga ah iyo xalalka muunada
Xisaabi boqolkiiba xarunta pramipexole ee D ee qaybta Pramipexole Dihydrochloride ee la qaatay:
Natiijadu = (rU/rS) × (CS/CU) × 100
rU = jawaabta ugu sarreysa ee xarunta pramipexole ee laxiriirta D ee xalka Tusaalaha
rS = jawaabta ugu sarreysa ee xarunta pramipexole ee laxiriirta D ee xalka caadiga ah
CS = fiirsashada xarunta pramipexole ee la xidhiidha D ee xalka caadiga ah (mg/mL)
CU = fiirsashada saamiga saamiga (mg/mL)
Shuruudaha aqbalaadda: NMT 1.0% ee isku dhafka pramipexole ee D
• Xadka Palladium
[Fiiro gaar ah- Samee tijaabadan haddii palladium ay tahay wasakh aan noolayn oo la yaqaan.]
Qalafsan: 0.1 M hydrochloric acid
Xalka caadiga ah: 40 µg/L ee palladium gudaha Diluent, laga bilaabo ganacsi ahaan la heli karo xalka palladium ee nuugista atomiga/balaasmaha isku xidhan[Xusuusin—Si cusub u diyaari xalkan sida loogu baahan yahay maalinta la isticmaalayo.]
Xalka Tusaalaha: Ilaa 0.5 g oo Pramipexole Dihydrochloride ah oo ku jira 50-mL caag mug leh ayaa ku dar 5.00 mL oo ah 1 M hydrochloric acid, oo ku milmi kulayl.Ku qabooji heerkulka qolka, oo ku mil biyo ilaa mugga.
Xaaladaha Spectrometric
(Fiiri Spectrophotometry iyo Iftiin-kala-firdhinta 851).
Qaabka: spectrophotometry nuugista atomiga
Dhererka mowjadda falanqaynta: Khadka qiiqa ee Palladium oo ah 247.6 nm
Lambaska: cathode madhan
Isha atomization: Foornada Graphite.[Xusuusin—Raac nidaamka soo saaraha ee taxanaha barnaamijka.]
Cabbirka Tusaalaha: 20µL
Banaan: Diluent
Ku habboonaanta nidaamka
Tusaale: Xalka caadiga ah
Shuruudaha ku habboonaanta
Nuugista: NLT 0.034
Falanqaynta
Tusaalooyinka: Xalka caadiga ah iyo xalalka muunada
Go'aami fiirsashada palladium ee xalka Tusaalaha habka isku-darka caadiga ah.
Shuruudaha aqbalaadda: NMT 5 ppm
SHURUUD DHEERAAD AH
Baakadaha iyo Kaydinta: Ku kaydi weelasha si fiican u xidhan, oo laga ilaaliyo qoyaanka iyo iftiinka.
• Heerarka Tixraaca USP 11
USP Pramipexole Dihydrochloride RS Guji si aad u aragto Qaabdhismeedka
Isku dhafka USP Pramipexole La Xiriira A RS
(S)-4,5,6,7-Tetrahydrobenzothiazole-2,6-diamine.
C7H11N3S 169.25
Isku dhafka USP Pramipexole ee la xidhiidha D RS
(R)-2-Amino-4,5,6,7-tetrahydro-6-(propylamino)benzothiazole.
C10H17N3S 211.33