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].
DEFINITION
Pramipexole Dihydrochloride ine NLT 98.0% uye NMT 102.0% yeC10H19Cl2N3S, yakaverengwa pane anhydrous basis.
KUZIVA
• A. Infrared Absorption <197A> kana <197M>
Wave number range: <197A>, 3800 cm-1 kusvika 650 cm-1;<197M>, 4000 cm-1 kusvika 600 cm-1
• B. Nguva yekuchengetedza yepamusoro pepamusoro muSample solution inoenderana nepramipexole (S-enantiomer) muSystem suitability solution mukuedzwa kweEnantiomeric Purity.
• C. Identification Tests-General, Chloride <191>
Muenzaniso: 1 mg / mL yePramipexole Dihydrochloride mumvura
Maitiro ekugamuchira: Inosangana nezvinodiwa zvesirivheri nitrate precipitate bvunzo
ASSAY
• Maitiro
Mhinduro A: Dissolve 9.1 g ye potassium dihydrogen phosphate uye 5.0 g ye sodium 1-octanesulfonate monohydrate mu 1 L yemvura.Gadzirisa nephosphoric acid kusvika pH ye3.0.
Mhinduro B: Acetonitrile uye Solution A (1:1)
Diluent: Acetonitrile uye Solution A (1:4)
Nharembozha: Ona tafura yegradient pazasi.
Nguva (min) Solution A (%) Solution B (%)
0 60 40
15 20 80
15.1 60 40
20 60 40
Sistimu yakakodzera mhinduro: 1.5 mg/mL yeUSP Pramipexole Dihydrochloride RS uye 0.8 mg/mL yeUSP Pramipexole Related Compound A RS in Diluent
Yakajairwa mhinduro: 1.5 mg/mL yeUSP Pramipexole Dihydrochloride RS mu Diluent
Sample solution: 1.5 mg/mL yePramipexole Dihydrochloride muDiluent
Chromatographic system
(Ona Chromatography <621>, System Suitability.)
Modhi: LC
Detector: UV 264 nm
Column: 4.6-mm × 15-cm;5-µm kurongedza L1
Column tembiricha: 40 ± 5
Kuyerera kweyero: 1.5 mL/min
Jekiseni saizi: 5 µL
Kukodzera kwehurongwa
Samples: Kukodzera kweSystem solution uye Standard solution [Cherechedza-Iyo nguva yekuchengetedza yepramipexole ine hukama nekomboni A uye pramipexole ingangoita 0.7 uye 1.0, zvichiteerana.]
Kukodzera zvinodiwa
Kugadziriswa: NLT 6.0 pakati pepramipexole inoenderana nekamu A uye pramipexole, Sistimu yakakodzera mhinduro
Tailing factor: NMT 2.0 yepramipexole, Sistimu yakakodzera mhinduro
Relative mwero kutsauka: NMT 1.0%, Standard mhinduro
Analysis
Samples: Yakajairwa mhinduro uye Sample mhinduro
Verengai muzana yeC10H19Cl2N3S muchikamu chePramipexole Dihydrochloride yakatorwa:
Mhedzisiro = (rU/rS) × (CS/CU) × (Mr1/Mr2) × 100
rU = peak mhinduro kubva kuSample solution
rS = mhinduro yepamusoro kubva kune Standard solution
CS = kusungwa kwe USP Pramipexole Dihydrochloride RS mu Standard solution (mg/mL)
CU = kusangana kweSample solution (mg/mL)
Mr1 = molecular uremu wepramipexole dihydrochloride, 284.26
Mr2 = molecular uremu wepramipexole dihydrochloride monohydrate, 302.26
Maitiro ekugamuchira: 98.0% -102.0% pane anhydrous basis
KUSIRIRA
Inorganic Impurities
• Zvakasara paKubatidza <281>: NMT 0.10%
• Heavy Metals, Nzira I <231>
Yakajairika mhinduro: Standard Lead Solution, 10 ppm
Sample solution: Madota 2 g yePramipexole Dihydrochloride kusvika yatoda kuoma, carbonized mass inowanikwa.Nyatsodza zvakasara, wedzera 2.0 mL yeconcentrated nitric acid uye 5 madonhwe econcentrated sulfuric acid, uye nyatsobvumira kuti utsi huvepo.Batidza pa500-600 kusvika kabhoni yatsva zvachose.Kutonhodza zvakasara, wedzera 4 mL ye6 M hydrochloric acid, vhara crucible, uye chera pamvura inopisa yekugezera kwemaminetsi gumi nemashanu.Evaporate kusvika pakuoma.Wedzera donhwe rimwe re concentrated hydrochloric acid uye 10 mL yemvura inopisa, uye chera kweimwe 2 min pakugeza kwemvura inopisa.Wedzera 6 M ammonia solution dropwise kusvika mushonga wacho waita kushaya alkaline, wogadzirisa ne1 M acetic acid kusvika pH ye3.0–4.0.Sefa mhinduro mu 25-mL volumetric flask, uye dilue nemvura kusvika 25 mL nekugeza crucible uye sefa.
Maitiro ekugamuchira: NMT 10 ppm
Organic Kusachena
• Maitiro
Solution A, Solution B, Diluent, Mobile phase, uye Chromatographic system: Enderera sezvinorayirwa muAssay.
Sistimu yakakodzera mhinduro: 7.5 µg/mL yeUSP Pramipexole Dihydrochloride RS uye 3 µg/mL yeUSP Pramipexole Inoenderana Compound A RS muDiluent
Yakajairwa mhinduro: 1.5 µg/mL yeUSP Pramipexole Dihydrochloride RS mu Diluent
Sample solution: 1.5 mg/mL yePramipexole Dihydrochloride muDiluent
Kukodzera kwehurongwa
Samples: Kukodzera sisitimu mhinduro uye Standard mhinduro
Kukodzera zvinodiwa
Kugadziriswa: NLT 6.0 pakati pepramipexole inoenderana nekamu A uye pramipexole, Sistimu yakakodzera mhinduro
Tailing factor: NMT 2.0 yepramipexole, Sistimu yakakodzera mhinduro
Relative mwero kutsauka: NMT 5.0%, Standard solution
Analysis
Samples: Yakajairwa mhinduro uye Sample mhinduro
Verengai muzana yekusachena chero kwemunhu muchikamu chePramipexole Dihydrochloride yakatorwa:
Mhedzisiro = (rU/rS) × (CS/CU) × (Mr1/Mr2) × 100
rU = peak mhinduro yekusachena yega yega kubva kuSample solution
rS = peak mhinduro yepramipexole kubva kune Standard solution
CS = kusungwa kwe USP Pramipexole Dihydrochloride RS mu Standard solution (mg/mL)
CU = kusangana kwepramipexole dihydrochloride monohydrate muSample solution (mg/mL)
Mr1 = molecular uremu wepramipexole dihydrochloride, 284.26
Mr2 = molecular uremu wepramipexole dihydrochloride monohydrate, 302.26
Maitiro ekugamuchira
Kusachena kwemunhu: Ona Kusachena Tafura 1.
Yese tsvina: NMT 0.5%
Kusachena Tafura 1
Zita Zvinoenderana Nekuchengeta Nguva Yekugamuchirwa, NMT (%)
Pramipexole propionamidea 0.5 0.15
Pramipexole yakabatana musanganiswa Ab 0.7 0.15
Pramipexole 1.0 -
N-Propylpramipexolec 1.4 0.15
Pramipexole dimerd 1.7 0.15
Chero kumwe kusachena kwemunhu kusingazivikanwe - 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).Iyi dimer yepramipexole (musanganiswa wemasomeri mana anogoneka).
ZVIYEDZO ZVAKANAKA
• Kusarudza Mvura, Nzira I <921>: NLT 4.5% uye NMT 6.5%
• Enantiomeric Kuchena
Nharembozha: n-Hexane, doro rakapera mvura, uye diethylamine (850:150:1)
Kukodzera kweSystem stock solution: 1 mg/mL imwe neimwe yeUSP Pramipexole Dihydrochloride RS uye USP Pramipexole Inoenderana Compound D RS mudoro risina mvura.
Kukodzera kweSystem mhinduro: 0.01 mg/mL imwe neimwe yeUSP Pramipexole Dihydrochloride RS uye USP Pramipexole Related Compound D RS kubva kuSystem suitability stock solution in Mobile phase
Yakajairwa stock solution: 2.0 mg/mL yeUSP Pramipexole Inoenderana Mushonga D RS mudoro risina mvura
Yakajairwa mhinduro: 1.5 µg/mL yeUSP Pramipexole Inoenderana Musanganiswa D RS muMobile phase
Sample solution: 0.3 mg/mL, yakagadzirirwa nekunyungudutsa yakafanira kuyerwa huwandu hwePramipexole Dihydrochloride mu25% yeflask volume yedoro rakapera uye kudiluted neMobile phase kusvika kuvhoriyamu.
Chromatographic system
(Ona Chromatography 621, System Suitability.)
Modhi: LC
Detector: UV 254 nm
Column: 4.6-mm × 25-cm;10-µm kurongedza L51
Kuyerera kweyero: 1.5 mL/min
Saizi yemuenzaniso: 75 μL
Kukodzera kwehurongwa
Samples: Kukodzera kweSystem mhinduro [Cherechedza-Iyo nguva yekuchengetedza pramipexole ine hukama D (R-enantiomer) uye pramipexole (S-enantiomer) ndeye 0.5 uye 1.0, zvichiteerana.]
Kukodzera zvinodiwa
Kugadziriswa: NLT 5.0 pakati pepramipexole ine hukama D uye pramipexole, Sistimu yakakodzera mhinduro
Tailing factor: NMT 2.4 ye pramipexole, Sistimu yakakodzera mhinduro
Analysis
Samples: Yakajairwa mhinduro uye Sample mhinduro
Verenga iyo muzana yepramipexole inoenderana nekamu D muchikamu chePramipexole Dihydrochloride yakatorwa:
Mhedzisiro = (rU/rS) × (CS/CU) × 100
rU = peak mhinduro yepramipexole ine hukama D kubva kuSample solution
rS = peak mhinduro yepramipexole inoenderana nekamu D kubva kune Standard solution
CS = kusanganiswa kwepramipexole ine hukama D mune iyo Standard solution (mg/mL)
CU = kusangana kweSample solution (mg/mL)
Maitiro ekugamuchira: NMT 1.0% yepramipexole ine hukama musanganiswa D
• Muganho wePalladium
[Cherechedza-Ita bvunzo iyi kana palladium iri inozivikanwa inorganic tsvina.]
Diluent: 0.1 M hydrochloric acid
Mushonga wakajairwa: 40 µg/L yepalladium muDiluent, kubva kune inotengeswa palladium yakajairwa mhinduro yekunyudza atomu/inductively yakabatanidzwa plasma.[Cherechedza—Gadzirira mhinduro iyi patsva sezvinodiwa pazuva rekushandisa.]
Sample solution: Ku 0.5 g yePramipexole Dihydrochloride mu50-mL volumetric flask wedzera 5.00 mL ye 1 M hydrochloric acid, uye nyungudika nekupisa.Kutonhorera kusvika kukamuri tembiricha, uye dilue nemvura kusvika kuhuwandu.
Spectrometric mamiriro
(Ona Spectrophotometry uye Chiedza-Kuparadzira 851).
Mode: Atomic absorption spectrophotometry
Analytical wavelength: Palladium emission line pa247.6 nm
Mwenje: Hollow cathode
Atomization source: Graphite furnace.[Cherechedza—Tevedzera zvinokurudzirwa nemugadziri wemapurogiramu anotevedzana.]
Saizi yemuenzaniso: 20 µL
Chisina chinhu: Diluent
Kukodzera kwehurongwa
Muenzaniso: Standard solution
Kukodzera zvinodiwa
Kusavapo: NLT 0.034
Analysis
Samples: Yakajairwa mhinduro uye Sample mhinduro
Sarudza kuwanda kwepalladium muSample solution neyakajairwa yekuwedzera nzira.
Maitiro ekugamuchira: NMT 5 ppm
ZVIMWE ZVINODIWA
• Kurongedza uye Kuchengeta: Chengetedza mumidziyo yakavharwa zvakanaka, yakachengetedzwa kubva pakunyorova uye chiedza.
• USP Reference Standards 11
USP Pramipexole Dihydrochloride RS Dzvanya kuti uone Chimiro
USP Pramipexole Inoenderana Necompound A RS
(S) -4,5,6,7-Tetrahydrobenzothiazole-2,6-diamine.
C7H11N3S 169.25
USP Pramipexole Inoenderana Musanganiswa D RS
(R) -2-Amino-4,5,6,7-tetrahydro-6-(propylamino)benzothiazole.
C10H17N3S 211.33