Orlistat CAS 96829-58-2 API Hoʻohaʻahaʻa i ke kaumaha o ka lāʻau maʻemaʻe 98.0~101.5%

ʻO Orlistat
C29H53NO5 495.73
l-Leucine, N-formyl-, 1-[(3-hexyl-4-oxo-2-oxetanyl)methyl]dodecyl ester, [2S-[2(R*), 3]]-;
N-Formyl-l-leucine, ester me (3S,4S) -3-hexyl-4-[(2S) -2-hydroxytridecyl]-2-oxetanone [96829-58-2].
HOAKAKA
Loaʻa iā Orlistat ka NLT 98.0% a me ka NMT 101.5% o C29H53NO5, i helu ʻia ma ke kumu anhydrous, solvent-free.
IKE
• A. Hoʻopili ʻana i ka infrared <197M>
B. ʻO ka manawa paʻa o ke kiʻekiʻe nui o ka hāʻina Laʻana e pili ana i ka hopena maʻamau, e like me ka loaʻa ʻana ma ka Assay.
HANA
• Kaʻina hana
[E hoʻomanaʻo-E hōʻalo i ka hoʻohana ʻana i nā ipu plastik no ka hoʻomākaukau ʻana a i ʻole ka hoʻopaʻa ʻana i kekahi hopena i kēia loiloi.]
Māhele kelepona: Acetonitrile, phosphoric acid, a me ka wai (860: 0.05: 140)
Haʻina maʻamau: 0.5 mg/mL o USP Orlistat RS ma ka pae Mobile.Inject koke ma hope o ka hoʻomākaukau ʻana a i ʻole mālama ʻia ma 5.
Laʻana hoʻonā: 0.5 mg / mL o Orlistat i ka pae Mobile.Inject koke ma hope o ka hoʻomākaukau ʻana a i ʻole mālama ʻia ma 5.
Pūnaehana Chromatographic
(E nana Chromatography <621>, Pūnaehana Pono.)
Ke ano: LC
ʻIke: UV 195
kolamu: 3.9-mm × 15-cm;4-µm paʻi L1
Kahe kahe: 1.0 mL / min
Ka nui o ka hoʻopio: 20 µL
Kūpono ʻōnaehana
Laʻana: Haʻina maʻamau
Nā koi kūpono
Wehewehe maʻamau pili: NMT 2.0%
Kānāwai
Nā Laʻana: Haʻina maʻamau a me ka hāʻina Laʻana
E helu i ka pākēneka o orlistat (C29H53NO5) ma ka ʻāpana o Orlistat i lawe ʻia:
Ka hopena = (rU/rS) × (CS/CU) × 100
rU = pane kiʻekiʻe mai ka hāʻina Laʻana
rS = pane kiʻekiʻe mai ka hoʻonā maʻamau
CS = ka manaʻo o ka USP Orlistat RS i ka hopena maʻamau (mg/mL)
CU = ka hoʻopaʻa ʻana o Orlistat i ka hāʻina Laʻana (mg/mL)
Paʻa ʻae ʻia: 98.0% -101.5% ma ke kumu anhydrous, solvent-free.
NA mea haumia
Nā mea haumia ʻole
• Ke koena ma ka ʻā ʻana <281>: NMT 0.1%
• Nā Metala Kaumaha, Hana II <231>: 20 ppm
Nā mea haumia kino
• Kaʻina Hana 1: Ka palena o Orlistat Related Compound A
ʻO ka hoʻonā maʻamau: 0.1 mg/mL o USP Orlistat Related Compound A RS i ka acetone
Laʻana hoʻonā: 50 mg/mL o Orlistat i ka acetone
Pūnaehana Chromatographic
(E nana Chromatography <621>, Thin-Layer Chromatography.)
Ke ano: TLC
Adsorbent: 0.25-mm papa o ka huila silica gel chromatographic
Ka nui o ka noi: 10 µL
Ke kūkulu nei i ka ʻōnaehana solvent: Toluene a me ka ethyl acetate (4:1)
ʻO ka hopena ʻike: E hoʻololi i 2.5 g o ka waikawa phosphomolybdic a me 1 g o ka cerric sulfate i loko o kahi pahu volumetric 100-mL, hoʻoheheʻe ʻia a hoʻoheheʻe ʻia me ka methanol i ka nui.
Kānāwai
Nā Laʻana: Haʻina maʻamau a me ka hāʻina Laʻana
Wehe i ka pā, a maloʻo loa i ka ea.E kāpīpī i ka pā maloʻo me ka Detection solution, a waiho i ka pā i loko o ka umu ma 120 no 30 min.
Paʻa e ʻae ai: ʻAʻole ʻoi aku ka ikaika o kēlā me kēia wahi lua mai ka hopena laʻana e pili ana i ka hui pili orlistat A ma mua o ka wahi e pili ana mai ka solution Standard (0.2%).
• Ke Kaʻina Hana 2: Ka palena o Orlistat Related Compound B
Haʻina maʻamau: 0.025 mg/mL o ka USP Orlistat Pili pūhui B RS i ka methylene chloride
Laʻana hoʻonā: 50 mg/mL o Orlistat i ka methylene chloride
ʻO ka hāʻina hāpana spiked: 50 mg/mL o Orlistat i ka hoʻonā maʻamau
Pūnaehana Chromatographic
(E nana Chromatography <621>, Pūnaehana Pono.)
Ke ano: GC
Mea ʻIke: Hoʻopā ahi
kolamu: 0.32-mm x 30-m silica fused, uhi ʻia me kahi pae kū mau 0.25-µm G27
Ka wela o ke kolamu: E nānā i ka pākaukau papahana wela ma lalo.
Mahana Hoʻomaka () Ramp Mahana (/min) Mahana Hope () Manawa Paʻa i ka Mahana Hope (min)
50 4 170 -
170 30 300 30
Mahana
Mea hoʻokomo: 270
ʻIke: 280
ʻeaea halihali: Helium
Kahe kahe: 30 mL / min
Māhele māhele: 10:1
Ka nui o ka injection: 2 µL
Kūpono ʻōnaehana
Laʻana: Haʻina maʻamau
Nā koi kūpono
Wehewehe maʻamau pili: NMT 10.0%
Kānāwai
Nā Laʻana: Laʻana haʻina a me Spiked hāpana hāpana
E helu i ka pākēneka o ka hui B i pili i ka orlistat ma ka ʻāpana o Orlistat i lawe ʻia:
Ka hopena = [rU/(rSP rU)] × (CS/CT) × 100
rU = pane kiʻekiʻe o ka hui B pili orlistat mai ka hāʻina Laʻana
rSP = pane kiʻekiʻe o orlistat pili pūhui B mai ka Spiked sample solution
CS = ka hoʻopaʻa ʻana o ka USP Orlistat Pūnaʻi Pili B RS i ka hoʻonā maʻamau (mg/mL)
CT = ka manaʻo o Orlistat i loko o ka hāpana hāpana Spiked (mg/mL)
Loaʻa nā pae ʻae: NMT 0.05% o ka hui B pili orlistat.
• Kaʻina hana 3
[E hoʻomanaʻo-E hōʻalo i ka hoʻohana ʻana i nā ipu plastik no ka hoʻomākaukau ʻana a i ʻole ka hoʻopaʻa ʻana i kekahi hopena i kēia loiloi.]
ʻO ka pae paʻa paʻa, Haʻina maʻamau, a me ka hopena laʻana: E hoʻomākaukau e like me ke kuhikuhi ʻana ma ka Assay.
ʻO ka hopena kūpono o ka ʻōnaehana: 10 µg/mL o USP Orlistat RS, 0.1 µg/mL o USP Orlistat Related Compound C RS, a me 0.25 µg/mL o USP Orlistat Related Compound D RS ma ka pae Mobile
Pūnaehana Chromatographic
(E nana Chromatography <621>, Pūnaehana Pono.)
E hoʻomau e like me ke kuhikuhi ʻana ma ka Assay, koe wale ka chromatograph i ka ʻōnaehana kūpono kūpono.
Kūpono ʻōnaehana
Laʻana: Haʻina kūpono ʻōnaehana
Nā koi kūpono
Lakiō hōʻailona-a-leo: NLT 3 no ka hui orlistat pili C a me orlistat pili pūhui D piko.
Hoʻokaʻawale maʻamau pili: NMT 10.0% no ka piko orlistat
Kānāwai
Nā Laʻana: Haʻina maʻamau a me ka hāʻina Laʻana
E helu i ka pakeneka o kēlā me kēia haumia i ka ʻāpana o Orlistat i lawe ʻia:
Ka hopena = (rU/rS) × (CS/CU) × (1/F) × 100
rU = pane kiʻekiʻe no kēlā me kēia haumia mai ka hāʻina Laʻana
rS = pane kiʻekiʻe o ka USP Orlistat RS mai ka hopena maʻamau
CS = ka manaʻo o ka USP Orlistat RS i ka hopena maʻamau (mg/mL)
CU = ka hoʻopaʻa ʻana o Orlistat i ka hāʻina Laʻana (mg/mL)
F = kumu pane pili e like me ka mea i hāʻawi ʻia ma ka Papa Hoʻomaʻemaʻe 1
Nā pae ʻae ʻae: E ʻike i ka Papa ʻAi ʻole 1.
Helu 1
Inoa Hoʻopaʻa Manawa Pilina Mea Manaʻo Manaʻo E ʻae ʻia, NMT (%)
Formylleucinea 0.10 4.0 0.2
Huihui pili Orlistat C 0.13 33 0.05
Orlistat apo apo epimerb 0.44 1.0 0.2
Orlistat pili pūhui D* 0.90 - helu ʻia i loko
Kaʻina hana 4
Orlistat open ring amidec* 0.90 - helu ʻia i loko
Kaʻina hana 4
Orlistat 1.00 - -
d-Leucine orlistatd 1.18 1.0 0.2
He haumia ʻike ʻole ʻia kēlā me kēia kanaka - 1.0 0.1
* Coelutes i kēia ʻōnaehana LC, hoʻoholo ʻia me ka hoʻohana ʻana i ke Kaʻina 4.
he N-Formyl-l-leucine.
b (2S,3R,5S)-5-[(S)-2-Formylamino-4-methyl-pentanoyloxy]-2-hexyl-3-hydroxy-hexadecanoic acid.
c N-Formyl-l-leucine (S)-1-[(2S,3S)-2-hydroxy-3-[1-phenyl-R-ethylcarbomoyl]nonyl]-dodecyl ester.
d N-Formyl-d-leucine (S)-1-[[(2S,3S)-3-hexyl-4-oxo-2-oxetanyl]methyl]dodecyl ester a i ʻole enantiomer.
• Ke Kaʻina Hana 4: Ka palena o Orlistat Related Compound D
Māhele kelepona: Methanol a me ka wai (83:17)
ʻO ka hopena kūpono o ka ʻōnaehana: 4 mg/mL o USP Orlistat RS a me 2.4 µg/mL o USP Orlistat Related Compound D RS i ka acetonitrile, kēlā me kēia.
ʻO ka hopena maʻamau: 5.0 mg / mL o USP Orlistat RS i ka acetonitrile
Laʻana hoʻonā: 5.0 mg/mL o Orlistat i ka acetonitrile
Pūnaehana Chromatographic
(E nānā i ka Chromatography 621, Pūnaehana Pono.)
Ke ano: LC
ʻIke: 205 nm
kolamu: 4.0-mm × 25-cm;5-µm paʻi L7
Kahe kahe: 0.6 mL / min
Ka nui o ka hoʻopio: 20 µL
Kūpono ʻōnaehana
Laʻana: Haʻina kūpono ʻōnaehana
Nā koi kūpono
Lakiō hōʻailona-a-noise: NLT 3 no ka hui pūhui D pili orlistat
Hoʻokaʻawale maʻamau pili: NMT 10.0% no ka piko orlistat
Kānāwai
Nā Laʻana: Haʻina maʻamau a me ka hāʻina Laʻana
E helu i ka pakeneka o kēlā me kēia haumia i ka ʻāpana o Orlistat i lawe ʻia:
Ka hopena = (rU/rS) × (CS/CU) × (1/F) × 100
rU = pane kiʻekiʻe no kēlā me kēia haumia mai ka hāʻina Laʻana
rS = pane kiʻekiʻe no ka USP Orlistat RS mai ka hopena maʻamau
CS = ka manaʻo o ka USP Orlistat RS i loko o ka hoʻonā maʻamau (µg/mL)
CU = ka hoʻopaʻa ʻana o Orlistat i ka hāʻina Laʻana (µg/mL)
F = kumu pane pili e like me ka mea i loaʻa ma ka Paʻa ʻole 2
Nā pae ʻae ʻae: E ʻike i ka papa ʻaina ʻino 2.
Helu 2
Inoa Hoʻopaʻa Manawa Pilina Mea Manaʻo Manaʻo E ʻae ʻia, NMT (%)
Huihui pili Orlistat D 0.94 1.0 0.2
Orlistat 1.00 - -
Orlistat hāmama apo amidea 1.25 4.3 0.1
he N-Formyl-l-leucine (S)-1-[(2S,3S)-2-hydroxy-3-[1-phenyl-R-ethylcarbomoyl]nonyl]-dodecyl ester.
• Ke Kaʻina Hana 5: Ka palena o Orlistat Related Compound E
Pahu: 0.4 N ka hopena borate, hoʻoponopono ʻia i ka pH o 10.2
Mea hoʻoheheʻe: ʻO-Phthaldehyde (OPA) solution.[E hoʻomanaʻo-Inā ʻaʻole hiki ke loaʻa ma ke kālepa, hiki ke hoʻomākaukau ʻia ka mea hoʻoheheʻe Derivitizing e like me 1% o kēlā me kēia 3-mercaptopropionic acid a me ka o-phthaldialdehyde i loko o 0.4 M borate buffer solution.]
Pane A: E hoʻololi i 4.1 g o ka sodium acetate trihydrate a me 40 mg o ka ethylenediaminetetraacetic acid (EDTA) i loko o kahi pahu volumetric 1-L.E hoʻoheheʻe i loko o 950 mL o ka wai, a hoʻoponopono me 0.1 N sodium hydroxide i kahi pH o 7.2.E hoʻoheheʻe me ka wai i ka nui, e hoʻohui i 2.5 mL o tetrahydrofuran, a hui pū.Kānana, a degas.
Pane B: E hoʻololi i 2.7 g o ka sodium acetate trihydrate a me 40 mg o EDTA i loko o kahi pahu volumetric 1-L.E hoʻoheheʻe i loko o 200 mL o ka wai, a hoʻoponopono me 0.1 N sodium hydroxide i kahi pH o 7.2.E hoʻohui i 800 mL o ka acetonitrile, kānana, a me nā degas.
Māhele paʻalima: E ʻike i ka papa gradient ma lalo.
Manawa (min) Hoʻonā A (%) Haʻina B (%)
0 96.7 3.3
20 60 40
24 0 100
38 0 100
38 96.7 3.3
45 96.7 3.3
Haʻina maʻamau: E hoʻololi i ka nui paona ma kahi o 0.2 mg o USP Orlistat Related compound E RS i loko o kahi hue 20-mL poʻo-space.E hoʻohui i 10 mL o 4 N sodium hydroxide, a pani i ka hue.E puhi i ka hue i 100 no ka hola 1, a laila e hoʻomaha i ka mahana wela.E hoʻololi i 2 mL o ka hopena i loko o kahi pahu volumetric 50-mL, a hoʻoheheʻe me ka wai i ka nui.I ka 0.5 mL o kēia hoʻonā e hoʻohui i 2.0 mL o ka Buffer a me 0.5 mL o Derivatizing agent.
Laʻana hoʻonā: E hoʻomau e like me ke kuhikuhi ʻana no ka solution Standard, akā e hoʻohana i ka 25 mg o Orlistat e pani i ka 0.2 mg o USP Orlistat Related Compound E RS.
Pūnaehana Chromatographic
(E nana Chromatography <621>, Pūnaehana Pono.)
Ke ano: LC
ʻIke: Fluorescence 340 nm (excitation);450 nm (hoʻokuʻu)
Nā kolamu
Kiaʻi: 2.1-mm × 2-cm;50-µm paʻi L1
Analytical: 2.1-mm × 20-cm;kāʻei L1
Kahe kahe: 0.5 mL / min
Ka nui o ka hoʻopio: 20 µL
Kūpono ʻōnaehana
Laʻana: Haʻina maʻamau
Nā koi kūpono
Hoʻokaʻawale maʻamau pili: NMT 6.0% no ka hui e pili ana i ka orlistat E peak
Kānāwai
Nā Laʻana: Haʻina maʻamau a me ka hāʻina Laʻana
E helu i ka pakeneka o kēia haumia i ka hapa o Orlistat i lawe ʻia:
Ka hopena = (rU/rS) × (CS/CU) × 100
rU = pane kiʻekiʻe no ka hui orlistat pili E i ka hāʻina Laʻana
rS = pane kiʻekiʻe no ka USP Orlistat Related Compound E RS i ka hoʻonā maʻamau
CS = ka hoʻopaʻa ʻana o ka USP Orlistat Related Compound E RS i loko o ka hopena maʻamau (mg/mL)
CU = ka hoʻopaʻa ʻana o Orlistat i ka hāʻina Laʻana (mg/mL)
Nā pae ʻae ʻae
ʻO ka haumia o kēlā me kēia kanaka: NMT 0.2% o ka hui pili orlistat E loaʻa.
Ka nui o nā haumia: NMT 1.0% o ka nui o nā haumia i loaʻa, nā hopena no nā Kaʻina 1, 2, 3, 4, a me 5 e hoʻohui ʻia.
NA HOAO KUAI
• ʻO ka ʻōnaʻi ʻokiʻoki, ʻōliʻi kikoʻī <781>
Laʻana hoʻonā: 30 mg/mL i ka waiʻona maloʻo
Nā pae ʻae ʻae: Ma waena o -48.0 a me -51.0, ma 20
• Ka Hoʻoholo Wai, Ka Hana Ic <921>: NMT 0.2%
NA KOI HOU
• Hoʻopili a me ka waiho ʻana: mālama i loko o nā pahu paʻa maikaʻi ma waena o 2 a me 8 ℃.
• Nā Kūlana Kūlana USP <11>
USP Orlistat RS
USP Orlistat Puhui Pili A RS
USP Orlistat Pūhui Pili B RS
USP Orlistat Puhui Pili C RS
USP Orlistat Puhui Pili D RS
USP Orlistat Huihui E RS
USP35