Ursodeoxycholic acid (UDCA) CAS 128-13-2 nyocha 99.0 ~ 101.0%

USODEOXYCHOLIC Acid
C24H40O4 Mr 392.6[128-13-2]
Nkọwa
3α,7β-Dihydroxy-5β-cholan-24-oic acid.
Ọdịnaya: 99.0 pasent ruo 101.0 pasent (ihe akpọnwụwo).
ÀMÀ
Ọdịdị: ọcha ma ọ bụ ihe fọrọ nke nta ka ọ bụrụ ntụ ntụ.
Solubility: ihe fọrọ nke nta ka ọ bụrụ ihe a na-adịghị ahụkebe na mmiri, na-agbaze na ethanol (pasent 96), soluble ntakịrị na acetone, ọ fọrọ nke nta ka ọ ghara ịsolu na methylene chloride.
mp: ihe dị ka 202 ℃.
Nchọpụta
njirimara mbụ: A.
njirimara nke abụọ: B, C.
A. spectrophotometry absorption infrared (2.2.24).
Ntụnyere: Ursodeoxycholic Acid CRS.
B. Nyochaa chromatograms enwetara n'ule maka adịghị ọcha C.
Nsonaazụ: isi ntụpọ na chromatogram enwetara na ngwọta nnwale (b) yiri n'ọnọdụ, agba na nha na isi ebe dị na chromatogram nwetara site na ntụnye ntụaka (a).
C. Gbarie ihe dịka 10 mg na 1 ml nke sulfuric acid R. Tinye 0.1 ml nke formaldehyde ngwọta R ma kwe ka guzoro maka 5 min.Tinye 5 ml mmiri R. Nkwusioru enwetara bụ akwụkwọ ndụ akwụkwọ ndụ-acha anụnụ anụnụ.
Nnwale
Ntụgharị anya pụrụ iche (2.2.7): + 58.0 ruo + 62.0 (ihe akpọnwụwo).
Gbari 0.500 g na ethanol R anhydrous wee jiri otu ihe mgbaze mee ka ọ bụrụ 25.0 ml.
Adịghị ọcha C. chromatography nke dị obere (2.2.27).
Ngwakọta ihe mgbaze: mmiri R, acetone R (10:90 V/V).
Ngwọta ule (a).Gbanyụọ 0.40 g nke ihe a ga-enyocha na ngwakọta ihe mgbaze ma gbanye 10 ml na ngwakọta ihe mgbaze.
Ngwọta ule (b).Ghichaa 1 ml nke ngwọta ule (a) na 10 ml na ngwakọta ihe mgbaze.
Ngwọta ntụaka (a).Gbarie 40 mg nke ursodeoxycholic acid CRS n'ime ngwakọta ihe mgbaze wee tụba ya na 10 ml na ngwakọta ihe mgbaze.
Ngwọta ntụaka (b).Gbari 20 mg nke lithocholic acid CRS (adịghị ọcha C) na ngwakọta ihe mgbaze wee gbanye 10.0 ml na ngwakọta ihe mgbaze (ngwọta A).Ghichaa 2.0 ml nke ngwọta a na 100.0 ml na ngwakọta ihe mgbaze.
Ngwọta ntụaka (c).Na 5 ml nke ngwọta, tinye 10 mg nke chenodeoxycholic acid CRS (adịghị ọcha A) wee gbanye 50 ml na ngwakọta ihe mgbaze.
Efere: TLC silica gel plate R.
Usoro mkpanaka: glacial acetic acid R, acetone R, methylenechloride R (1:30:60 V/V/V).
Ngwa: 5μL.
Mmepe: karịa 2/3 nke efere.
Nhicha: na 120 ℃ maka 10 min.
Nchọpụta: fesa ozugbo na 47.6 g/L ngwọta nke phosphomolybdic acid R na ngwakọta nke 1 olu sulfuric acid R na 20 mpịakọta glacial acetic acid R na okpomọkụ na 120 ℃ ruo mgbe ntụpọ na-acha anụnụ anụnụ pụtara na ọkụ ọkụ ndabere.
Ndabara sistemu: ngwọta ntụaka (c):
- chromatogram na-egosi ntụpọ isi abụọ kewapụrụ nke ọma.
Oke: ngwọta nnwale (a):
-adịghị ọcha C: ntụpọ ọ bụla n'ihi adịghị ọcha C adịghị ike karịa ebe bụ isi na chromatogram nwetara site na ntụnye ntụaka (b) (0.1%).
Ihe ndị metụtara ya.chromatography nke mmiri mmiri (2.2.29).
Ngwakọta mgbaze: methanol R, usoro mkpanaka (10:90 V/V).
Ngwọta ule.Gbanyụọ 60 mg nke ihe a ga-enyocha na ngwakọta ihe mgbaze wee gbasaa na 20.0 ml na ngwakọta ihe mgbaze.
Ngwọta ntụaka (a).Gbarie ọdịnaya nke vial nke Ursodeoxycholic Acid maka sistemu sistemu CRS (nwere adịghị ọcha A na H) na 1.0 ml nke ngwakọta ihe mgbaze.
Ngwọta ntụaka (b).Ghichaa 1.0 ml nke ngwọta ule na 100.0 ml na ngwakọta ihe mgbaze.Ghichaa 1.0 ml nke ngwọta a na 10.0 ml na ngwakọta ihe mgbaze.
Ogidi:
- nha: l = 0.25 m, Ø = 4.6 mm;
-Agba ọsọ: njedebe-capped octadecylsilyl silica gel makachromatography R (5 μm);
- okpomọkụ: 40 ℃ ± 1 ℃.
Usoro mkpanaka: gwakọta mpịakọta 30 nke acetonitrile R, mpịakọta 37 nke ngwọta 0.78 g / L nke sodium dihydrogen phosphate R gbanwee na pH 3 na phosphoric acid R, na 40 mpịakọta methanol R.
Ọnụego mmiri: 0.8ml/min.
Nchọpụta: refractometer na 35 ± 1 ℃.
Nri: 150 μL.
Oge ịgba ọsọ: oge ​​4 nke Ursodeoxycholic acid.
Nchọpụta adịghị ọcha: jiri chromatogram nyere ursodeoxycholic acid maka ịdị mma sistemu CRS yana chromatogram enwetara na ntụzịaka ntụaka (a) iji chọpụta ọnụ ọgụgụ kachasị elu n'ihi adịghị ọcha A na H.
Njide njikọ na ntụnyere ursodeoxycholic acid (oge njide = ihe dịka 14 min): adịghị ọcha H = banyere 0.9;adịghị ọcha A = ihe dịka 2.8.
Ndabara sistemu: ngwọta ntụaka (a):
-mkpebi: opekempe 1.5 n'etiti ọnụ ọnụ n'ihi adịghị ọcha H na ursodeoxycholic acid.
Oke:
- adịghị ọcha A: ọ bụghị ihe karịrị ugboro 10 mpaghara nke isi ihe dị na chromatogram nwetara na ngwọta ntụaka (b) (1.0%);
-adịghị ọcha na-akọwapụtaghị: maka adịghị ọcha ọ bụla, ọ bụghị karịa mpaghara nke isi elu na chromatogram nwetara na ngwọta ntụaka (b) (0.10 pasent);
- mkpokọta: ọ bụghị ihe karịrị ugboro 15 mpaghara nke isi ọnụ ọgụgụ dị elu na chromatogram nwetara na ngwọta ntụaka (b) (1.5%);
-nleghara oke: 0,5 ugboro mpaghara nke isi elu na chromatogram nwetara na ntụaka ngwọta (b) (0.05 percent).
Ọla dị arọ (2.4.8): kacha 20 ppm.
1.0 g na-akwado ule C. Kwadebe ntụaka ntụaka site na iji 2 mL nke ngwọta ọkọlọtọ ụzọ (10ppm Pb) R.
Ọnwụ na ihicha (2.2.32): kacha 1.0 pasent, kpebisiri ike na 1.000 g site na ihicha na oven na 105 ℃.
Sulfated ash (2.4.14): kacha 0.1 pasent, kpebisiri ike na 1.0 g.
ASSAY
Gbari 0.350 g na 50 ml nke ethanol (pasent 96) R, na mbụ neutralized ka 0.2 mL nke phenolphthalein ngwọta R. Tinye 50 mL mmiri R na titrate na 0.1 M sodium hydroxide ruo mgbe a pink agba.
1 ml nke 0.1 M sodium hydroxide bụ 39.26 mg nke C24H40O4.
IHE adịghị ọcha
Ihe adịghị ọcha akọwapụtara: A, C.
Ihe adịghị ọcha ndị ọzọ a na-achọpụta (ihe ndị na-esonụ ga-, ma ọ bụrụ na ọ dị na ọkwa zuru oke, otu ma ọ bụ ọzọ nke ule dị na monograph. A na-ejedebe ha site na njedebe nnabata n'ozuzu maka adịghị ọcha ndị ọzọ/akọwapụtaghị na / ma ọ bụ site na mkpokọta monograph ihe. maka iji ọgwụ eme ihe (2034) Ya mere ọ dịghị mkpa ka a chọpụta adịghị ọcha ndị a maka ngosipụta nke nnabata. Leekwa 5.10.
Njikwa adịghị ọcha na ihe maka iji ọgwụ eme ihe): B, D, E, F, G, H, I.
A. 3α,7a-dihydroxy-5β-cholan-24-oic acid (chenodeoxycholic acid),
B. 3α,7α,12a-trihydroxy-5β-cholan-24-oic acid (cholic acid),
C. 3a-hydroxy-5β-cholan-24-oic acid (lithocholic acid),
D. 3α,7β,12a-trihydroxy-5β-cholan-24-oic acid (ursocholic acid),
E. 3α,12α-dihydroxy-5β-cholan-24-oic acid (deoxycholic acid),
F. 3a-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.