Ursodeoxycholic Acid (UDCA) CAS 128-13-2 Assay 99.0~101.0%

URSODEOXYCHOLIC ACID
C24H40O4 Mr 392.6[128-13-2]
WHAKAMAHI
3α,7β-Dihydroxy-5β-cholan-24-oic acid.
Ihirangi: 99.0 ōrau ki te 101.0 ōrau (matū maroke).
KAUPAPA
Te ahua: paura ma, tata ma ranei.
Te memehatanga: karekau e rewa ki te wai, te wairewa noa ki te waiwaro (96 paiheneti), paku whakarewa ki te acetone, tata kore ki te methylene chloride.
mp: āhua 202℃.
WHAKATAUTANGA
Te tohu tuatahi: A.
Tautuhi tuarua: B, C.
A. A. Infrared absorption spectrophotometry (2.2.24).
Whakatauritenga: Ursodeoxycholic Acid CRS.
B. Tirohia nga chromatograms i whiwhi i te whakamatautau mo te poke C.
Hua: Ko te waahi matua o te chromatogram i whiwhi ki te otinga whakamatautau (b) he rite te tuunga, te tae me te rahi ki te waahi matua o te chromatogram i whiwhi ki te otinga tohutoro (a).
C. Whakarewahia te 10 mg ki te 1 mL o te waikawa pungatara R. Tāpirihia te 0.1 mL o te wairewa formaldehyde R ka waiho kia tu mo te 5 meneti.Tāpirihia te 5 mL wai R. Ko te whakatārewatanga he kākāriki-puru.
WHAKAMAHI
Te hurihanga whatu motuhake (2.2.7): + 58.0 ki + 62.0 (matū maroke).
Whakarewahia te 0.500 g ki te waiwaro R ka waimeha ki te 25.0 mL me te whakarewa ano.
Te poke C. Thin-layer chromatography (2.2.27).
Te ranunga whakarewa: wai R, acetone R (10:90 V/V).
Te otinga whakamatautau (a).Whakarewahia te 0.40 g o te matū ka tirohia i roto i te ranunga whakarewa ka waimeha ki te 10 mL me te ranunga whakarewa.
Te otinga whakamatautau (b).Ringihia te 1 mL o te wairewa whakamatautau (a) ki te 10 mL ki te ranunga whakarewa.
Te otinga tohutoro (a).Whakarewahia te 40 mg o te waikawa ursodeoxycholic CRS i roto i te ranunga whakarewa ka waimeha ki te 10 mL me te ranunga whakarewa.
Te otinga tohutoro (b).Whakarewahia te 20 mg o te waikawa lithocholic CRS (te poke C) i roto i te ranunga whakarewa ka waimeha ki te 10.0 mL me te ranunga whakarewa (wairewa A).Ringihia te 2.0 mL o tenei otinga ki te 100.0 mL me te ranunga whakarewa.
Te otinga tohutoro (c).Ki te 5 mL o te otinga A tāpirihia te 10 mg o te waikawa chenodeoxycholic CRS (te poke A) ka waimeha ki te 50 mL me te ranunga whakarewa.
Pereti: TLC silica gel plate R.
Wāhanga pūkoro: waikawa ahetiki huka R, acetone R, methylenepūhaumāota R (1:30:60 V/V/V).
Taupānga: 5μL.
Whanaketanga: neke atu i te 2/3 o te pereti.
Te whakamaroke: i te 120 ℃ mo te 10 min.
Raputanga: rehu tonu ki te wairewa 47.6 g/L o te waikawa phosphomolybdic R i roto i te ranunga o te 1 rōrahi o te waikawa pungatara R me te 20 rōrahi o te waikawa ahetiki glacial R me te whakamahana i te 120 ℃ tae noa ki te puta mai o nga wahi kikorangi ki runga i te papamuri mama.
Te pai o te punaha: otinga tohutoro (c):
- e whakaatu ana te chromatogram i nga waahi matua e 2 kua wehea.
Tepe: otinga whakamatautau (a):
-te poke C: tetahi wahi na te poke C kaore i te kaha ake i te waahi matua o te chromatogram i whiwhi ki te otinga tohutoro (b) (0.1 paiheneti).
Matū whai pānga.Koromatography wai (2.2.29).
Te ranunga whakarewa: mewaro R, te wahanga pūkoro (10:90 V/V).
Te otinga whakamatautau.Whakarewahia te 60 mg o te matū ka tirohia i roto i te ranunga whakarewa ka waimeha ki te 20.0 mL me te ranunga whakarewa.
Te otinga tohutoro (a).Whakarewahia nga mea o roto o te ipu Ursodeoxycholic Acid kia pai ai te punaha CRS (kei roto nga poke A me te H) ki te 1.0 mL o te ranunga whakarewa.
Te otinga tohutoro (b).Ringihia te 1.0 mL o te otinga whakamatautau ki te 100.0 mL me te ranunga whakarewa.Ringihia te 1.0 mL o tenei otinga ki te 10.0 mL me te ranunga whakarewa.
Tīwae:
-rahi: l = 0.25 m, Ø = 4.6 mm;
-waahanga paho: octadecylsilyl silica gel kapi-mutunga mochromatography R (5 μm);
- te pāmahana: 40℃ ± 1℃.
Wāhanga pūkoro: uruhia te 30 rōrahi acetonitrile R, 37 rōrahi o te otinga 0.78 g/L o te konutai dihydrogen phosphate R kua whakaritea ki te pH 3 me te waikawa ūkuikui R, me te 40 rōrahi mewaro R.
Rere rere: 0.8 mL/min.
Te kitenga: te refractometer i te 35 ± 1 ℃.
Werohanga: 150 μL.
Te wa oma: 4 wa te wa pupuri o Ursodeoxycholic Acid.
Te tautuhi i nga poke: whakamahia te chromatogram i homai ki te waikawa ursodeoxycholic mo te pai o te punaha CRS me te chromatogram i whiwhi me te otinga tohutoro (a) hei tautuhi i nga tihi na te poke A me H.
Te pupuri whanaunga me te tohutoro ki te waikawa ursodeoxycholic (wa pupuri = tata ki te 14 min): poke H = tata ki te 0.9;poke A = āhua 2.8.
Te pai o te punaha: otinga tohutoro (a):
-taumira: iti rawa 1.5 i waenganui i nga tihi na te poke H me te waikawa ursodeoxycholic.
Tepe:
- poke A: kaua e neke ake i te 10 whakarea te horahanga o te tihi matua o te chromatogram i whiwhi ki te otinga tohutoro (b) (1.0 ōrau);
-nga poke kore i tohua: mo ia poke, kaua e neke ake i te waahi o te tihi matua o te chromatogram i whiwhi ki te otinga tohutoro (b) (0.10 paiheneti);
- tapeke: kaua e neke ake i te 15 whakarea te horahanga o te tihi matua o te chromatogram i whiwhi ki te otinga tohutoro (b) (1.5 ōrau);
-kaore e aro: 0.5 whakarea te horahanga o te tihi matua o te chromatogram i whiwhi ki te otinga tohutoro (b) (0.05 ōrau).
Nga konganuku taumaha (2.4.8): teitei 20 ppm.
1.0 g e tutuki ana ki te whakamatautau C. Whakaritea te otinga tohutoro ma te whakamahi i te 2 mL o te wairewa paerewa mata (10 ppm Pb) R.
Ngaronga i runga i te whakamaroke (2.2.32): 1.0 paiheneti te nui, ka whakatauhia ki te 1.000 g ma te whakamaroke i roto i te oumu i te 105 ℃.
Te pungarehu ngongo (2.4.14): 0.1 paiheneti teitei, kua whakatauhia ki te 1.0 g.
WHAKAMAHI
Whakarewahia te 0.350 g ki te 50 mL o te waihano (96 paiheneti) R, i whakakorea i mua ki te 0.2 mL o te wairewa phenolphthalein R. Tāpirihia te 50 mL wai R ka whakatitahia ki te 0.1 M konutai waihā kia tae ra ano he tae mawhero.
Ko te 1 mL o te 0.1 M konutai waikawa he rite ki te 39.26 mg o C24H40O4.
NGA POKE
Ko nga poke kua tohua: A, C.
Ko etahi atu poke ka kitea (ko nga matū e whai ake nei, mena he rawaka te taumata, ka kitea e tetahi, etahi atu ranei o nga whakamatautau kei roto i te monograph. Ka whakawhäitihia e te paearu whakaae whänui mo etahi atu poke/kaore i whakaingoatia, e te monograph whanui Matanga. mo te whakamahi rongoa (2034) No reira kaore e tika kia tautuhia enei poke hei whakaatu i te tutukitanga. Tirohia hoki 5.10.
Te whakahaere i nga poke i roto i nga matū mo te whakamahi rongoa): B, D, E, F, G, H, I.
A. 3α,7α-dihydroxy-5β-cholan-24-oic acid (waikawa chenodeoxycholic),
B. 3α,7α,12α-trihydroxy-5β-cholan-24-oic waikawa (waikawa cholic),
C. 3α-hydroxy-5β-cholan-24-oic acid (waikawa lithocholic),
D. 3α,7β,12α-trihydroxy-5β-cholan-24-oic acid (waikawa ursocholic),
E. 3α,12α-dihydroxy-5β-cholan-24-oic acid (waikawa deoxycholic),
F. 3α-hydroxy-7-oxo-5β-cholan-24-oic acid,
G. methyl 3α,7β-dihydroxy-5β-cholan-24-oate,
H. 3β,7β-dihydroxy-5β-cholan-24-oic acid,
I. 5β-cholane-3α,7β,24-triol.