Orlistat CAS 96829-58-2 API Taumaha Ngaronga Tarukino Purity 98.0~101.5%

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, hākawa me (3S,4S) -3-hexyl-4- [(2S) -2-hydroxytridecyl] -2-oxetanone [96829-58-2].
WHAKAMAHI
Kei roto i te Orlistat te NLT 98.0% me te NMT 101.5% o C29H53NO5, kua tatauhia i runga i te waikore, te whakarewa-kore.
WHAKATAUTANGA
• A. Te Kohanga Pokarekare <197M>
• B. Ko te wa pupuri o te tihi nui o te otinga Tauira e rite ana ki tera o te otinga Paerewa, i riro mai i roto i te Assay.
WHAKAMAHI
• Tikanga
[Tuhipoka-A ape i te whakamahi i nga ipu kirihou mo te whakarite, te pupuri ranei i tetahi otinga i roto i tenei tātaritanga.]
Waahanga pūkoro: Acetonitrile, waikawa phosphoric, me te wai (860: 0.05: 140)
Te otinga paerewa: 0.5 mg/mL o te USP Orlistat RS i te wahanga Waea.Inuhia i muri tonu i te takahanga, te rongoa ranei i te 5.
Tauira otinga: 0.5 mg / mL o Orlistat i te wahanga Waea Waea.Inuhia i muri tonu i te takahanga, te rongoa ranei i te 5.
Pūnaha Chromatographic
(Tirohia te Chromatography <621>, Whakaritenga Pūnaha.)
Aratau: LC
Kaitirotiro: UV 195
Tīwae: 3.9-mm × 15-cm;4-µm tākai L1
Rere rere: 1.0 mL/min
Rahi werohanga: 20 µL
Te pai o te punaha
Tauira: otinga Paerewa
Nga whakaritenga e tika ana
Inenga Paerewa Paanga: NMT 2.0%
Tātaritanga
Tauira: otinga Paerewa me te otinga Tauira
Tātaihia te ōrau o te orlistat (C29H53NO5) i te wahanga o Orlistat i tangohia:
Hua = (rU/rS) × (CS/CU) × 100
rU = te whakautu teitei mai i te Tauira otinga
rS = te whakautu teitei mai i te otinga Paerewa
CS = te kukū o te USP Orlistat RS i te otinga Paerewa (mg/mL)
CU = te kukū o Orlistat i roto i te Tauira otinga (mg/mL)
Paearu whakaae: 98.0%-101.5% i runga i te waikore, te whakarewa-kore.
NGA POKE
Nga poke parakore
• Te toenga i runga i te mura <281>: NMT 0.1%
• Nga Koura Nui, Tikanga II <231>: 20 ppm
Nga poke pararopi
• Tikanga 1: Te Tepe o te Puhui Paatahi Orlistat A
Wairewa Paerewa: 0.1 mg/mL o USP Orlistat Pānga Pūhui A RS i roto i te acetone
Tauira otinga: 50 mg/mL o Orlistat i roto i te acetone
Pūnaha Chromatographic
(Tirohia te Chromatography <621>, Thin-Layer Chromatography.)
Aratau: TLC
Adsorbent: 0.25-mm te paparanga o te ranunga chromatographic silica gel
Rōrahi tono: 10 µL
Te whakawhanake i te punaha whakarewa: Toluene me te ethyl acetate (4:1)
Te otinga rapu: Whakawhitihia te 2.5 karae o te waikawa phosphomolybdic me te 1 karaehe o te cerric sulfate ki roto i te ipu 100-mL, memeha ki roto ka waimeha ki te mewaro ki te rōrahi.
Tātaritanga
Tauira: otinga Paerewa me te otinga Tauira
Tangohia te pereti, ka whakamarokehia ki te hau.Ringihia te pereti maroke ki te otinga Detection, ka waiho te pereti ki roto i te oumu i te 120 mo te 30 meneti.
Paearu whakaae: Ko nga waahi tuarua mai i te Tauira otinga e rite ana ki te orlistat e pa ana ki te puhui A kaore i te kaha ake i te waahi mai i te otinga Paerewa (0.2%).
• Tikanga 2: Te Tepe o Orlistat Related Compound B
Wairewa Paerewa: 0.025 mg/mL o te USP Orlistat Related Compound B RS i roto i te methylene chloride
Tauira otinga: 50 mg/mL o Orlistat i roto i te methylene chloride
Ko te otinga tauira tiihi: 50 mg/mL o Orlistat i roto i te otinga Paerewa
Pūnaha Chromatographic
(Tirohia te Chromatography <621>, Whakaritenga Pūnaha.)
Aratau: GC
Kaipupuri: Te katote mura
Tīwae: 0.32-mm x 30-m te kirika tuitui, ka pania ki te 0.25-µm G27 wahanga tu
Te pāmahana o te tīwae: Tirohia te ripanga hōtaka pāmahana i raro nei.
Te Paemahana Tuatahi () Te Paemahana Ramp (/min) Te Wehenga Whakamutunga () Te Waa Pupuri i te Waahi Whakamutunga (meneti)
50 4 170 -
170 30 300 30
Te pāmahana
Injector: 270
Kaitirotiro: 280
Te hau kawe: Helium
Rere rere: 30 mL/min
Ritua ōwehenga: 10:1
Rahi werohanga: 2 µL
Te pai o te punaha
Tauira: otinga Paerewa
Nga whakaritenga e tika ana
Inenga Paerewa Paanga: NMT 10.0%
Tātaritanga
Tauira: Tauira otinga me Spiked tauira otinga
Tātaihia te ōrau o te pūhui B e pā ana ki te orlistat i te wahanga o Orlistat i tangohia:
Hua = [rU/(rSP rU)] × (CS/CT) × 100
rU = te whakautu teitei o te orlistat e pa ana ki te pūhui B mai i te Tauira otinga
rSP = te whakautu teitei o te orlistat e pa ana ki te pūhui B mai i te otinga tauira Spiked
CS = te kukū o te USP Orlistat Pānga Pūhui B RS i te otinga Paerewa (mg/mL)
CT = te kukū o Orlistat i roto i te otinga tauira Spiked (mg/mL)
Paearu whakaae: NMT 0.05% o te orlistat e pa ana ki te pūhui B kua kitea.
• Tikanga 3
[Tuhipoka-A ape i te whakamahi i nga ipu kirihou mo te whakarite, te pupuri ranei i tetahi otinga i roto i tenei tātaritanga.]
Wāhanga pūkoro, otinga Paerewa, me te otinga Tauira: Whakaritea kia rite ki te tohutohu i roto i te Whakatau.
Te otinga pai o te punaha: 10 µg/mL o USP Orlistat RS, 0.1 µg/mL o USP Orlistat Related Compound C RS, me te 0.25 µg/mL o USP Orlistat Related Compound D RS i te wahanga Waea
Pūnaha Chromatographic
(Tirohia te Chromatography <621>, Whakaritenga Pūnaha.)
Haere tonu ki te whakahau i roto i te Tirohanga, engari ki te chromatograph te otinga pai o te punaha.
Te pai o te punaha
Tauira: Te otinga pai o te punaha
Nga whakaritenga e tika ana
Te ōwehenga tohu-ki-haruru: NLT 3 mo te orlistat-related compound C me te orlistat related compound D tihika
Te inenga paerewa whaitake: NMT 10.0% mo te tihi orlistat
Tātaritanga
Tauira: otinga Paerewa me te otinga Tauira
Tātaihia te ōrau o ia poke i te wahanga o Orlistat i tangohia:
Hua = (rU/rS) × (CS/CU) × (1/F) × 100
rU = te whakautu teitei mo ia poke takitahi mai i te otinga Tauira
rS = whakautu teitei o USP Orlistat RS mai i te otinga Paerewa
CS = te kukū o te USP Orlistat RS i te otinga Paerewa (mg/mL)
CU = te kukū o Orlistat i roto i te Tauira otinga (mg/mL)
F = tauwehe whakautu whanaunga i homai ki te Ripanga poke 1
Paearu whakaae: Tirohia te Ripanga poke 1.
Ripanga poke 1
Ingoa Wā Pupuri Whanaungatanga Whakautu Paanga Paearu Whakaaetanga, NMT (%)
Formylleucinea 0.10 4.0 0.2
Orlistat pūhui C 0.13 33 0.05
Orlistat mowhiti tuwhera epimerb 0.44 1.0 0.2
Pūhui pātahi Orlistat D* 0.90 - Kua tātaihia ki roto
Tikanga 4
Orlistat mowhiti tuwhera amidec* 0.90 - Tatauhia i roto
Tikanga 4
Orlistat 1.00 - -
d-Leucine orlistatd 1.18 1.0 0.2
Te poke takitahi - 1.0 0.1
* Ka uru ki roto i tenei punaha LC, ka whakatauhia ma te whakamahi i te Tikanga 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 or enantiomer.
• Tikanga 4: Te Tepe o te Puhui Paa Orlistat D
Wāhanga pūkoro: Methanol me te wai (83:17)
Te otinga pai o te punaha: 4 mg/mL o USP Orlistat RS me 2.4 µg/mL o USP Orlistat Related Compound D RS i roto i te acetonitrile, ia
Te otinga paerewa: 5.0 mg/mL o USP Orlistat RS i roto i te acetonitrile
Tauira otinga: 5.0 mg/mL o Orlistat i roto i te acetonitrile
Pūnaha Chromatographic
(Tirohia Chromatography 621, Pūnaha Whakaritenga.)
Aratau: LC
Kaitirotiro: 205 nm
Tīwae: 4.0-mm × 25-cm;5-µm kiki L7
Rere rere: 0.6 mL/min
Rahi werohanga: 20 µL
Te pai o te punaha
Tauira: Te otinga pai o te punaha
Nga whakaritenga e tika ana
Te ōwehenga tohu-ki-haruru: NLT 3 mo te tihi D e pa ana ki te orlistat
Te inenga paerewa whaitake: NMT 10.0% mo te tihi orlistat
Tātaritanga
Tauira: otinga Paerewa me te otinga Tauira
Tātaihia te ōrau o ia poke i te wahanga o Orlistat i tangohia:
Hua = (rU/rS) × (CS/CU) × (1/F) × 100
rU = te whakautu teitei mo ia poke takitahi mai i te otinga Tauira
rS = whakautu teitei mo USP Orlistat RS mai i te otinga Paerewa
CS = te kukū o te USP Orlistat RS i te otinga Paerewa (µg/mL)
CU = te kukū o Orlistat i te Tauira otinga (µg/mL)
F = tauwehe whakautu whanaunga i whiwhi i te Ripanga poke 2
Paearu whakaae: Tirohia te Ripanga poke 2.
Ripanga poke 2
Ingoa Wā Pupuri Whanaungatanga Whakautu Paanga Paearu Whakaaetanga, NMT (%)
Pūhui pātahi Orlistat D 0.94 1.0 0.2
Orlistat 1.00 - -
Orlistat mowhiti tuwhera 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.
• Tikanga 5: Te Tepe o Orlistat Related Compound E
Pūreirei: 0.4 N te wairewa borate, he mea whakarite ki te pH 10.2
Kaipupuri whakaheke: otinga o-Phthaldehyde (OPA).[Tuhipoka-Ki te kore e taea te hoko mai i te hokohoko, ka taea te whakarite i te kaihoko Whakarewa hei 1% mo ia waikawa 3-mercaptopropionic me te o-phthaldialdehyde i roto i te wairewa buffer borate 0.4 M.]
Otinga A: Whakawhitihia te 4.1 g o te konutai acetate trihydrate me te 40 mg o te waikawa ethylenediaminetetraacetic (EDTA) ki roto i te ipu volumetric 1-L.Whakarewa i roto i te 950 mL o te wai, ka whakatika ki te 0.1 N konutai waihā ki te pH o 7.2.Waimeha ki te wai ki te rōrahi, tāpiri 2.5 mL o tetrahydrofuran, ka uru.Tātari, me te degas.
Otinga B: Whakawhitihia te 2.7 g o te konutai acetate trihydrate me te 40 mg o te EDTA ki roto i te ipu 1-L.Whakarewa i roto i te 200 mL o te wai, ka whakatika ki te 0.1 N te konutai waikawa ki te pH 7.2.Tāpirihia te 800 mL o te acetonitrile, te tātari, me te degas.
Wāhanga pūkoro: Tirohia te ripanga rōnaki i raro nei.
Wā (meneti) Rongoā A (%) Rongoā 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
Wairewa Paerewa: Whakawhitihia he rahinga pauna tata ki te 0.2 mg o te USP Orlistat Related compound E RS ki roto i te ipu mokowhiti 20-mL.Tāpirihia te 10 mL o te konutai waihā 4 N, ka kati te ipu.Whakawerahia te ipu ki te 100 mo te 1 haora, ka tuku kia whakamatao ki te pāmahana rūma.Whakawhitihia te 2 mL o te otinga ki roto i te ipu 50-mL, ka waimeha ki te wai ki te rōrahi.Ki te 0.5 mL o tenei wairewa ka tapirihia te 2.0 mL o te Buffer me te 0.5 mL o te kaihoko Derivatizing.
Tauira otinga: Haere tonu mo te otinga Paerewa, engari whakamahia te 25 mg o Orlistat hei whakakapi i te 0.2 mg o USP Orlistat Related Compound E RS.
Pūnaha Chromatographic
(Tirohia te Chromatography <621>, Whakaritenga Pūnaha.)
Aratau: LC
Kaipupuri: Korewharewha 340 nm (whakatairanga);450 nm (tuku)
Nga poupou
Kaitiaki: 2.1-mm × 2-cm;50-µm tākai L1
Tātari: 2.1-mm × 20-cm;kiki L1
Rere rere: 0.5 mL/min
Rahi werohanga: 20 µL
Te pai o te punaha
Tauira: otinga Paerewa
Nga whakaritenga e tika ana
Te inenga paerewa: NMT 6.0% mo te orlistat e pa ana ki te tihi E
Tātaritanga
Tauira: otinga Paerewa me te otinga Tauira
Tātaihia te ōrau o tēnei poke i te wāhanga o Orlistat i tangohia:
Hua = (rU/rS) × (CS/CU) × 100
rU = te whakautu teitei mo te orlistat e pa ana ki te pūhui E i roto i te Tauira otinga
rS = te whakautu teitei mo te USP Orlistat Related Compound E RS i roto i te otinga Paerewa
CS = te kukū o te USP Orlistat Related Compound E RS i te otinga Paerewa (mg/mL)
CU = te kukū o Orlistat i roto i te Tauira otinga (mg/mL)
Paearu whakaae
Te poke takitahi: NMT 0.2% o te orlistat e pa ana ki te pūhui E kua kitea.
Te tapeke o nga poke: NMT 1.0% o nga poke katoa ka kitea, ko nga hua mo nga Tikanga 1, 2, 3, 4, me te 5 ka taapirihia.
NGA WHAKAMATAUTANGA
• Te Hurihanga Mata, Hurihanga Tauwhāiti <781>
Tauira otinga: 30 mg/mL i te waipiro maroke
Paearu whakaae: I waenganui i -48.0 me -51.0, i te 20
• Te Whakatau Wai, Tikanga Ic <921>: NMT 0.2%
HE WHAKAMAHI ATU
• Te Whakapai me te Rokiroki: Whakaorangia i roto i nga ipu kua kati pai i waenga i te 2 me te 8 ℃.
• Paerewa Tohutoro USP <11>
USP Orlistat RS
USP Orlistat Related Compound A RS
USP Orlistat Related Compound B RS
USP Orlistat Related Compound C RS
USP Orlistat Related Compound D RS
USP Orlistat Related Compound E RS
USP35