Pramipexole Dihydrochloride Monohydrate CAS 191217-81-9 Hōʻike 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].
HOAKAKA
Loaʻa iā Pramipexole Dihydrochloride ka NLT 98.0% a me ka NMT 102.0% o C10H19Cl2N3S, i helu ʻia ma ke kumu anhydrous.
IKE
• A. Hoʻopili ʻana i ka infrared <197A> a i ʻole <197M>
Launa helu nalu: <197A>, 3800 knm-1 a 650 knm-1;<197M>, 4000 knm-1 a 600 knm-1
B. ʻO ka manawa paʻa o ke kiʻekiʻe nui i ka hopena Laʻana e pili ana i ka pramipexole (S-enantiomer) i loko o ka ʻōnaehana kūpono i ka hoʻāʻo no Enantiomeric Purity.
• C. Identification Tests-General, Chloride <191>
Laʻana: 1 mg/mL o Pramipexole Dihydrochloride i loko o ka wai
Nā pae ʻae ʻae: E hoʻokō i nā koi o ka hoʻāʻo ʻana i ka hoʻāʻo ʻana o ka nitrate precipitate
HANA
• Kaʻina hana
Pane A: E hoʻoheheʻe i 9.1 g o ka potassium dihydrogen phosphate a me 5.0 g o ka sodium 1-octanesulfonate monohydrate i 1 L o ka wai.Hoʻoponopono me ka waikawa phosphoric i kahi pH o 3.0.
Pane B: Acetonitrile a me A (1:1)
Mea hoʻoheheʻe: Acetonitrile a me ka Solution A (1: 4)
Māhele paʻalima: E ʻike i ka papa gradient ma lalo.
Manawa (min) Hoʻonā A (%) Haʻina B (%)
0 60 40
15 20 80
15.1 60 40
20 60 40
ʻO ka hoʻonā kūpono o ka ʻōnaehana: 1.5 mg/mL o USP Pramipexole Dihydrochloride RS a me 0.8 mg/mL o USP Pramipexole Related Compound A RS ma ka Diluent
Haʻina maʻamau: 1.5 mg/mL o USP Pramipexole Dihydrochloride RS i ka Diluent
Laʻana hoʻonā: 1.5 mg/mL o Pramipexole Dihydrochloride i Diluent
Pūnaehana Chromatographic
(E nana Chromatography <621>, Pūnaehana Pono.)
Ke ano: LC
ʻIke: UV 264 nm
kolamu: 4.6-mm × 15-cm;5-µm paʻi L1
Ka wela o ke kolamu: 40 ± 5
Kahe kahe: 1.5 mL / min
Ka nui o ka hoʻopio: 5 µL
Kūpono ʻōnaehana
Nā Laʻana: ʻO ka hoʻonā kūpono o ka ʻōnaehana a me ka hoʻonā maʻamau [Note-ʻO nā manawa paʻa pili no ka pūhui pili pramipexole A me ka pramipexole ma kahi o 0.7 a me 1.0.]
Nā koi kūpono
Hoʻoholo: NLT 6.0 ma waena o ka pūhui pili i ka pramipexole A a me ka pramipexole, ʻO ka hoʻonā kūpono kūpono.
ʻO ke kumu huelo: NMT 2.0 no pramipexole, ʻO ka hoʻonā kūpono o ka ʻōnaehana
Hoʻokaʻawale maʻamau pili: NMT 1.0%, Haʻina maʻamau
Kānāwai
Nā Laʻana: Haʻina maʻamau a me ka hāʻina Laʻana
E helu i ka pākēneka o C10H19Cl2N3S ma ka ʻāpana o Pramipexole Dihydrochloride i lawe ʻia:
Ka hopena = (rU/rS) × (CS/CU) × (Mr1/Mr2) × 100
rU = pane kiʻekiʻe mai ka hāʻina Laʻana
rS = pane kiʻekiʻe mai ka hoʻonā maʻamau
CS = ka manaʻo o ka USP Pramipexole Dihydrochloride RS i loko o ka hopena maʻamau (mg/mL)
CU = ka hoʻopaʻa ʻana o ka hāpana laʻana (mg/mL)
Mr1 = ke kaumaha mole o pramipexole dihydrochloride, 284.26
Mr2 = ke kaumaha molekala o pramipexole dihydrochloride monohydrate, 302.26
Nā pae ʻae ʻae: 98.0%–102.0% ma ke kumu anhydrous
NA mea haumia
Nā mea haumia ʻole
• Ke koena ma ka ʻā ʻana <281>: NMT 0.10%
• Nā Metala Kaumaha, Keʻano I <231>
ʻO ka hopena maʻamau: ʻO ke alakaʻi alakaʻi maʻamau, 10 ppm
Laʻana hoʻonā: Ash 2 g o Pramipexole Dihydrochloride a hiki i kahi maloʻo, carbonized nuipaʻi loaʻa.E hooluolu i ke koena, e hookomo i 2.0 mL o ka waika nitric concentrated a me 5 kulu o ka waika sulfuric concentrated, a ae akahele i ka mahuka e ulu.E puhi ma 500-600 a hiki i ka pau ana o ke kalapona.E hooluolu i ke koena, e hookomo i 4 mL o 6 M hydrochloric acid, e uhi i ka pahu, a e hooluu ma ka wai auau no 15 min.E evaporate a maloʻo.E hoʻohui i hoʻokahi kulu o ka waika hydrochloric concentrated a me 10 mL o ka wai wela, a e hoʻoheheʻe no 2 mau minuke ma ka ʻauʻau wai paila.E hoʻonui i ka waiʻona amonia he 6 M me ka liʻiliʻi a hiki i ka nāwaliwali o ka hopena, a hoʻoponopono me 1 M acetic acid i kahi pH o 3.0-4.0.E kānana i ka hopena i loko o ka pahu volumetric 25-mL, a e hoʻoheheʻe me ka wai i 25 mL ma ka holoi ʻana i ke kīʻaha a me ka kānana.
Nā pae ʻae ʻae: NMT 10 ppm
Nā mea haumia kino
• Kaʻina hana
Pane A, Solution B, Diluent, Mobile phase, a me Chromatographic system: E hoʻomau e like me ke kuhikuhi ʻana i ka Assay.
ʻO ka hoʻonā kūpono o ka ʻōnaehana: 7.5 µg/mL o USP Pramipexole Dihydrochloride RS a me 3 µg/mL o USP Pramipexole Related Compound A RS i ka Diluent
Haʻina maʻamau: 1.5 µg/mL o USP Pramipexole Dihydrochloride RS i ka Diluent
Laʻana hoʻonā: 1.5 mg/mL o Pramipexole Dihydrochloride i Diluent
Kūpono ʻōnaehana
Nā Laʻana: Haʻina kūpono ʻōnaehana a me ka hopena maʻamau
Nā koi kūpono
Hoʻoholo: NLT 6.0 ma waena o ka pūhui pili i ka pramipexole A a me ka pramipexole, ʻO ka hoʻonā kūpono kūpono.
ʻO ke kumu huelo: NMT 2.0 no pramipexole, ʻO ka hoʻonā kūpono o ka ʻōnaehana
Hoʻokaʻawale maʻamau pili: NMT 5.0%, Haʻina maʻamau
Kānāwai
Nā Laʻana: Haʻina maʻamau a me ka hāʻina Laʻana
E helu i ka pākēneka o kēlā me kēia haumia ma ka ʻāpana o Pramipexole Dihydrochloride i lawe ʻia:
Ka hopena = (rU/rS) × (CS/CU) × (Mr1/Mr2) × 100
rU = pane kiʻekiʻe o kēlā me kēia haumia mai ka Haʻina Haʻawina
rS = pane kiʻekiʻe o pramipexole mai ka hoʻonā maʻamau
CS = ka manaʻo o ka USP Pramipexole Dihydrochloride RS i loko o ka hopena maʻamau (mg/mL)
CU = ka hoʻopaʻa ʻana o ka pramipexole dihydrochloride monohydrate i loko o ka hāpana Laʻana (mg/mL)
Mr1 = ke kaumaha mole o pramipexole dihydrochloride, 284.26
Mr2 = ke kaumaha molekala o pramipexole dihydrochloride monohydrate, 302.26
Nā pae ʻae ʻae
Nā haumia o kēlā me kēia kanaka: E nānā i ka Papa Hoʻomaʻemaʻe 1.
Huina haumia: NMT 0.5%
Helu 1
Inoa Hoʻopaʻa ʻana i ka manawa e ʻae ʻia, NMT (%)
Pramipexole propionamidea 0.5 0.15
Puhui pili Pramipexole Ab 0.7 0.15
Pramipexole 1.0 —
N-Propylpramipexolec 1.4 0.15
Pramipexole dimerd 1.7 0.15
ʻO nā mea haumia ʻē aʻe i ʻike ʻole ʻia - 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).ʻO kēia kahi dimer o pramipexole (kahi hui ʻana o nā isomers hiki ke hiki).
NA HOAO KUAI
• Ka Hoʻoholo Wai, Ka Hana I <921>: NLT 4.5% a me NMT 6.5%
• Maemae Enantiomeric
Māhele kelepona: n-Hexane, waiʻona waiʻona, a me diethylamine (850:150:1)
ʻO ka hoʻonā waiwai waiwai kūpono: 1 mg/mL kēlā me kēia USP Pramipexole Dihydrochloride RS a me USP Pramipexole Related Compound D RS i loko o ka waiʻona maloʻo.
Hoʻonā kūpono o ka ʻōnaehana: 0.01 mg/mL kēlā me kēia o USP Pramipexole Dihydrochloride RS a me USP Pramipexole Related Compound D RS mai ka hoʻonā waiwai waiwai kūpono ma ka pae Mobile.
Haʻina waiwai maʻamau: 2.0 mg/mL o USP Pramipexole Pūhui D RS pili i loko o ka waiʻona waiʻona.
Haʻina maʻamau: 1.5 µg/mL o USP Pramipexole Pūnaehana Pili D RS ma ka pae Mobile
Laʻana hoʻonā: 0.3 mg/mL, hoʻomākaukau ʻia ma ka hoʻoheheʻe ʻana i ka nui kūpono o Pramipexole Dihydrochloride i kaupaona ʻia ma 25% o ka puʻu wai o ka waiʻona dehydrated a hoʻoheheʻe ʻia me ka pae Mobile i ka nui.
Pūnaehana Chromatographic
(E nānā i ka Chromatography 621, Pūnaehana Pono.)
Ke ano: LC
ʻIke: UV 254 nm
kolamu: 4.6-mm × 25-cm;10-µm paʻi L51
Kahe kahe: 1.5 mL / min
Laʻana nui: 75 µL
Kūpono ʻōnaehana
Nā Laʻana: ʻO ka hopena kūpono o ka ʻōnaehana [Note-ʻO nā manawa paʻa pili no ka pūhui pili pramipexole D (R-enantiomer) a me ka pramipexole (S-enantiomer) he 0.5 a me 1.0.]
Nā koi kūpono
Hoʻoholo: NLT 5.0 ma waena o ka pūhui pili D a me ka pramipexole, ʻO ka hopena kūpono o ka ʻōnaehana.
ʻO ke kumu huelo: NMT 2.4 no ka pramipexole, ʻO ka ʻōnaehana kūpono
Kānāwai
Nā Laʻana: Haʻina maʻamau a me ka hāʻina Laʻana
E helu i ka pākēneka o ka pūhui e pili ana i ka pramipexole D ma ka ʻāpana o Pramipexole Dihydrochloride i lawe ʻia:
Ka hopena = (rU/rS) × (CS/CU) × 100
rU = pane kiʻekiʻe o pramipexole pili pūhui D mai ka hāʻina Laʻana
rS = pane kiʻekiʻe o pramipexole pili pūhui D mai ka hoʻonā maʻamau
CS = ka hoʻopaʻa ʻana o ka pūhui pili pramipexole D i ka hoʻonā maʻamau (mg/mL)
CU = ka hoʻopaʻa ʻana o ka hāpana laʻana (mg/mL)
Nā pae ʻae ʻae: NMT 1.0% o ka pūhui pili pramipexole D
• Ka palena o Palladium
[E hoʻomaopopo-E hana i kēia hoʻāʻo inā he haumia inorganic i ʻike ʻia ka palladium.]
Mea hoʻoheheʻe: 0.1 M hydrochloric acid
ʻO ka hopena maʻamau: 40 µg/L o ka palladium i Diluent, mai ka palladium i loaʻa i ke kūʻai kūʻai ʻana i ka hopena maʻamau no ka hoʻoheheʻe atomika/inductively coupled plasma.[E hoʻomaopopo—E hoʻomākaukau hou i kēia hoʻonā e like me ke koi ʻana i ka lā hoʻohana.]
Laʻana hoʻonā: E hoʻohui i ka 0.5 g o Pramipexole Dihydrochloride i loko o kahi pahu volumetric 50-mL 5.00 mL o 1 M hydrochloric acid, a hoʻoheheʻe me ka hoʻomehana.Hoʻolili i ka lumi wela, a hoʻoheheʻe me ka wai i ka nui.
Nā kūlana spectrometric
(E nānā i ka Spectrophotometry and Light-Scattering 851).
Ke ano: Atomeki absorption spectrophotometry
Ka lōʻihi hawewe analytical: Palladium emission line ma 247.6 nm
Kukui: Hollow cathode
Ke kumu hoʻoheheʻe ʻana: ka umu ahi graphite.[E hoʻomaopopo—E hahai i ke kaʻina hoʻolālā i ʻōlelo ʻia e ka mea hana.]
Laʻana nui: 20 µL
Blank: Diluent
Kūpono ʻōnaehana
Laʻana: Haʻina maʻamau
Nā koi kūpono
ʻAi ʻana: NLT 0.034
Kānāwai
Nā Laʻana: Haʻina maʻamau a me ka hāʻina Laʻana
E hoʻoholo i ka neʻe ʻana o ka palladium i ka hāʻina Laʻana ma ke ʻano hoʻohui maʻamau.
Nā pae ʻae ʻae: NMT 5 ppm
NA KOI HOU
• Hoʻopaʻa a me ka mālama ʻana: mālama ʻia i loko o nā pahu paʻa maikaʻi, pale ʻia mai ka makū a me ka māmā.
• Nā Kūlana Kūlana USP 11
USP Pramipexole Dihydrochloride RS Kaomi e nānā i ke kūkulu
USP Pramipexole Puhui Pili A RS
(S) -4,5,6,7-Tetrahydrobenzothiazole-2,6-diamine.
C7H11N3S 169.25
USP Pramipexole Pūhui Pili D RS
(R)-2-Amino-4,5,6,7-tetrahydro-6-(propylamino)benzothiazole.
C10H17N3S 211.33