I-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].
INCAZELO
I-Pramipexole Dihydrochloride iqukethe i-NLT 98.0% ne-NMT 102.0% ye-C10H19Cl2N3S, ibalwe ngesisekelo se-anhydrous.
UKUKHOMBA
• A. I-Infrared Absorption <197A> noma <197M>
Ibanga lezinombolo zamagagasi: <197A>, 3800 cm-1 kuya ku-650 cm-1;<197M>, 4000 cm-1 kuya ku-600 cm-1
• B. Isikhathi sokugcina sesiqongo esikhulu kusixazululo Sesampuli sihambisana naleso se-pramipexole (S-enantiomer) kusixazululo sokufaneleka Kwesistimu ekuhlolweni kwe-Enantiomeric Purity.
• C. Ukuhlolwa Kokuhlonza Okujwayelekile, I-Chloride <191>
Isampula: 1 mg/mL ye-Pramipexole Dihydrochloride emanzini
Indlela yokwamukela: Ihlangabezana nezimfuneko zokuhlolwa kwe-silver nitrate precipitate
ISIVIVINYO
• Inqubo
Isixazululo A: Chaza u-9.1 g we-potassium dihydrogen phosphate kanye no-5.0 g we-sodium 1-octanesulfonate monohydrate ku-1 L yamanzi.Lungisa nge-phosphoric acid ibe yi-pH engu-3.0.
Isixazululo B: I-Acetonitrile nesixazululo A (1:1)
I-Diluent: I-Acetonitrile nesixazululo A (1:4)
Isigaba seselula: Bona ithebula legradient ngezansi.
Isikhathi (imizuzu) Isixazululo A (%) Isixazululo B (%)
0 6040
15 20 80
15.1 60 40
20 60 40
Isixazululo sokufaneleka kwesistimu: 1.5 mg/mL ye-USP Pramipexole Dihydrochloride RS kanye no-0.8 mg/mL we-USP Pramipexole Inhlanganisela Ehlobene A RS ku-Diluent
Isixazululo esijwayelekile: 1.5 mg/mL ye-USP Pramipexole Dihydrochloride RS ku-Diluent
Isixazululo sesampula: 1.5 mg/mL ye-Pramipexole Dihydrochloride ku-Diluent
Isistimu yeChromatographic
(Bona i-Chromatography <621>, Ukufaneleka Kwesistimu.)
Imodi: LC
Umtshina: UV 264 nm
Ikholomu: 4.6-mm × 15-cm;5-µm ukupakisha i-L1
Izinga lokushisa lekholomu: 40 ± 5
Izinga lokugeleza: 1.5 mL/min
Usayizi womjovo: 5 µL
Ukufaneleka kwesistimu
Amasampula: Isixazululo sokufaneleka kwesistimu kanye nesixazululo Esijwayelekile [Qaphela-Izikhathi zokugcinwa okuhlobene kwe-pramipexole ehlobene nenhlanganisela A kanye ne-pramipexole cishe zingu-0.7 kanye no-1.0, ngokulandelana.]
Izidingo zokufaneleka
Isixazululo: I-NLT 6.0 phakathi kwe-pramipexole ehlobene ne-compound A ne-pramipexole, isisombululo sokufaneleka kwesistimu
Isici somsila: I-NMT 2.0 ye-pramipexole, isixazululo sokufaneleka kwesistimu
Ukuchezuka okujwayelekile okuhlobene: I-NMT 1.0%, Isixazululo esijwayelekile
Ukuhlaziya
Amasampula: Isixazululo esijwayelekile kanye nesixazululo esiyisampula
Bala iphesenti le-C10H19Cl2N3S engxenyeni ye-Pramipexole Dihydrochloride ethathiwe:
Umphumela = (rU/rS) × (CS/CU) × (Mr1/Mr2) × 100
rU = impendulo ephezulu evela kusixazululo Sesampula
rS = impendulo ephezulu evela kusixazululo Esijwayelekile
CS = ukuhlushwa kwe-USP Pramipexole Dihydrochloride RS kusixazululo Esijwayelekile (mg/mL)
I-CU = ukugxila kwesixazululo sesampula (mg/mL)
Mr1 = isisindo samangqamuzana e-pramipexole dihydrochloride, 284.26
Mr2 = isisindo samangqamuzana e-pramipexole dihydrochloride monohydrate, 302.26
Indlela yokwamukela: 98.0%–102.0% kusisekelo se-anhydrous
UKUNGCOLA
Ukungcola Okungaphili
• Insalela Ekuthutheni <281>: NMT 0.10%
• Izinsimbi Ezisindayo, Indlela I <231>
Isixazululo esijwayelekile: Isixazululo Esijwayelekile Sokuhola, 10 ppm
Isixazululo esiyisampula: Umlotha 2 g wePramipexole Dihydrochloride kuze kutholakale isisindo esicishe somile, esine-carbonized.Pholisa insalela, engeza u-2.0 mL we-nitric acid egxilile kanye namaconsi angu-5 e-sulfuric acid egxilile, bese uvumela ngokucophelela ukuthi intuthu iguquke.Bamba ku-500-600 kuze kube yilapho ikhabhoni ishiswa ngokuphelele.Pholisa insalela, engeza u-4 mL we-6 M hydrochloric acid, umboze i-crucible, futhi ugaye emanzini okugeza abilayo imizuzu engu-15.Shutheka kome.Engeza iconsi elilodwa le-hydrochloric acid egxilile kanye no-10 mL wamanzi ashisayo, bese ugaya eminye imizuzu emi-2 okugeza kwamanzi abilayo.Engeza isixazululo se-ammonia esingu-6 M ngokwehla kuze kube yilapho isixazululo sine-alkaline ebuthakathaka, futhi ulungise ne-acetic acid engu-1 kuya ku-pH engu-3.0–4.0.Hlunga ikhambi ku-25-mL ye-volumetric flask, bese uhlanza ngamanzi ku-25 mL ngokugeza i-crucible kanye nesihlungi.
Indlela yokwamukela: NMT 10 ppm
Ukungcola Okuphilayo
• Inqubo
Isixazululo A, Isixazululo B, I-Diluent, Isigaba Seselula, kanye nesistimu ye-Chromatographic: Qhubeka njengoba kuqondiswe ku-Assay.
Isixazululo sokufaneleka kwesistimu: 7.5 µg/mL ye-USP Pramipexole Dihydrochloride RS kanye no-3 µg/mL we-USP Pramipexole Related Compound A RS in Diluent
Isixazululo esijwayelekile: 1.5 µg/mL ye-USP Pramipexole Dihydrochloride RS ku-Diluent
Isixazululo sesampula: 1.5 mg/mL ye-Pramipexole Dihydrochloride ku-Diluent
Ukufaneleka kwesistimu
Amasampula: Isixazululo sokufaneleka kwesistimu nesixazululo Esijwayelekile
Izidingo zokufaneleka
Isixazululo: I-NLT 6.0 phakathi kwe-pramipexole ehlobene ne-compound A ne-pramipexole, isisombululo sokufaneleka kwesistimu
Isici somsila: I-NMT 2.0 ye-pramipexole, isixazululo sokufaneleka kwesistimu
Ukuchezuka okujwayelekile okuhlobene: I-NMT 5.0%, Isixazululo esijwayelekile
Ukuhlaziya
Amasampula: Isixazululo esijwayelekile kanye nesixazululo esiyisampula
Bala iphesenti lanoma yikuphi ukungcola komuntu ngamunye engxenyeni ye-Pramipexole Dihydrochloride ethathiwe:
Umphumela = (rU/rS) × (CS/CU) × (Mr1/Mr2) × 100
i-rU = impendulo ephakeme kakhulu yokungcola ngakunye okuvela kusixazululo Sesampula
rS = impendulo ephezulu ye-pramipexole evela kusixazululo Esijwayelekile
CS = ukuhlushwa kwe-USP Pramipexole Dihydrochloride RS kusixazululo Esijwayelekile (mg/mL)
I-CU = ukuhlushwa kwe-pramipexole dihydrochloride monohydrate kusixazululo Sesampula (mg/mL)
Mr1 = isisindo samangqamuzana e-pramipexole dihydrochloride, 284.26
Mr2 = isisindo samangqamuzana e-pramipexole dihydrochloride monohydrate, 302.26
Imibandela yokwamukela
Ukungcola komuntu ngamunye: Bheka Ithebula Lokungcola 1.
Ukungcola okuphelele: NMT 0.5%
Ithebula Lokungcola 1
Qamba Imibandela Yokwamukela Isikhathi Sokugcinwa Okuhlobene, i-NMT (%)
I-Pramipexole propionamidea 0.5 0.15
Inhlanganisela ehlobene ne-Pramipexole Ab 0.7 0.15
I-Pramipexole 1.0 -
I-N-Propylpramipexolec 1.4 0.15
I-Pramipexole dimerd 1.7 0.15
Noma yikuphi okunye ukungcola komuntu okungaziwa — 0.10
i-(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).Lena i-dimer ye-pramipexole (ingxube yama-isomer amane angaba khona).
IZIVIVINYO EZITHILE
• Ukunqunywa kwamanzi, Indlela I <921>: I-NLT 4.5% kanye ne-NMT 6.5%
• Ukuhlanzeka kwe-Enantiomeric
Isigaba seselula: i-n-Hexane, utshwala obuphelelwe amanzi emzimbeni, ne-diethylamine (850:150:1)
Isixazululo sesitoko sokufaneleka kwesistimu: 1 mg/mL ngayinye ye-USP Pramipexole Dihydrochloride RS kanye ne-USP Pramipexole Inhlanganisela Ehlobene D RS kutshwala obuphelelwe amanzi
Isixazululo sokufaneleka kwesistimu: 0.01 mg/mL ngayinye ye-USP Pramipexole Dihydrochloride RS kanye ne-USP Pramipexole Inhlanganisela Ehlobene D RS kusukela kusixazululo sesitoko sokufaneleka kweSistimu kusigaba Seselula
Isixazululo sesitoko esijwayelekile: 2.0 mg/mL ye-USP Pramipexole Inhlanganisela Ehlobene D RS kutshwala obuphelelwe amanzi
Isixazululo esijwayelekile: 1.5 µg/mL ye-USP Pramipexole Inhlanganisela Ehlobene D RS esigabeni Seselula
Isixazululo sesampula: 0.3 mg/mL, esilungiselelwe ngokuncibilikisa inani elifanele lesisindo sePramipexole Dihydrochloride ku-25% wevolumu yeflask yotshwala obuphelelwe amanzi futhi ihlanjululwe ngesigaba seselula ukuya kuvolumu
Isistimu yeChromatographic
(Bona i-Chromatography 621, Ukufaneleka Kwesistimu.)
Imodi: LC
Umtshina: UV 254 nm
Ikholomu: 4.6-mm × 25-cm;10-µm ukupakisha L51
Izinga lokugeleza: 1.5 mL/min
Usayizi wesampula: 75µL
Ukufaneleka kwesistimu
Amasampula: Isixazululo sokufaneleka kwesistimu [Qaphela-Izikhathi zokugcinwa okuhlobene kwe-pramipexole ehlobene nenhlanganisela D (R-enantiomer) kanye ne-pramipexole (S-enantiomer) zingu-0.5 kanye no-1.0, ngokulandelana.]
Izidingo zokufaneleka
Isixazululo: I-NLT 5.0 phakathi kwe-pramipexole ehlobene ne-compound D ne-pramipexole, isisombululo sokufaneleka kwesistimu
Isici somsila: I-NMT 2.4 ye-pramipexole, isixazululo sokufaneleka kwesistimu
Ukuhlaziya
Amasampula: Isixazululo esijwayelekile kanye nesixazululo esiyisampula
Bala iphesenti lenhlanganisela ye-pramipexole D engxenyeni ye-Pramipexole Dihydrochloride ethathiwe:
Umphumela = (rU/rS) × (CS/CU) × 100
rU = impendulo ephakeme ye-pramipexole ehlobene ne-compound D kusuka kusixazululo seSampule
rS = impendulo ephakeme ye-pramipexole ehlobene nenhlanganisela D kusukela kusixazululo Esijwayelekile
CS = ukuhlushwa kwe-pramipexole ehlobene nenhlanganisela D kusixazululo esijwayelekile (mg/mL)
I-CU = ukugxila kwesixazululo sesampula (mg/mL)
Indlela yokwamukela: I-NMT 1.0% yenhlanganisela ehlobene ne-pramipexole D
• Umkhawulo wePalladium
[Qaphela-Yenza lokhu kuhlola uma i-palladium iwukungcola okwaziwayo kwe-inorganic.]
I-Diluent: 0.1 M hydrochloric acid
Isixazululo esijwayelekile: 40 µg/L we-palladium ku-Diluent, kusukela kusixazululo esivamile se-palladium esitholakala ngokuthengiswayo sokumuncwa kwe-athomu/i-plasma ehlanganiswe ngokungenisa.[Qaphela—Lungisa lesi sixazululo njengoba kudingekile ngosuku lokusisebenzisa.]
Isixazululo esiyisampula: Ku-0.5 g we-Pramipexole Dihydrochloride ku-50-mL volumetric flask engeza u-5.00 mL we-1 M hydrochloric acid, bese uncibilikisa ngokushisa.Kuphole ekamelweni lokushisa, bese uhlanza ngamanzi ngevolumu.
Izimo ze-Spectrometric
(Bheka i-Spectrophotometry kanye ne-Light-Scattering 851).
Imodi: I-spectrophotometry yokumuncwa kwe-athomu
Ubude begagasi bokuhlaziya: Umugqa wokuphuma kwe-Palladium ku-247.6 nm
Isibani: I-cathode engenalutho
Umthombo we-Atomization: Isithando somlilo se-Graphite.[Qaphela—Landela uhlelo olunconyiwe lomkhiqizi.]
Usayizi wesampula: 20 µL
Okungenalutho: Diluent
Ukufaneleka kwesistimu
Isampula: Isixazululo esijwayelekile
Izidingo zokufaneleka
Ukungabi nalutho: NLT 0.034
Ukuhlaziya
Amasampula: Isixazululo esijwayelekile kanye nesixazululo esiyisampula
Nquma ukugxila kwe-palladium kusixazululo Sesampuli ngendlela yokwengeza evamile.
Indlela yokwamukela: NMT 5 ppm
IZIDINGO EZENGEZIWE
• Ukupakisha Nokugcina: Londoloza ezitsheni ezivalwe kahle, ezivikelekile emswakameni nasekukhanyeni.
• I-USP Reference Standards 11
USP Pramipexole Dihydrochloride RS Chofoza ukuze Ubuke Isakhiwo
I-USP Pramipexole Inhlanganisela Ehlobene A RS
(S) -4,5,6,7-Tetrahydrobenzothiazole-2,6-diamine.
I-C7H11N3S 169.25
I-USP Pramipexole Inhlanganisela Ehlobene D RS
(R) -2-Amino-4,5,6,7-tetrahydro-6-(propylamino)benzothiazole.
I-C10H17N3S 211.33