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

URSODEOXYCHOLIC ACID
C24H40O4 Mr 392.6[128-13-2]
DEFINITION
3α,7β-Dihydroxy-5β-cholan-24-oic acid.
Zvemukati: 99.0 muzana kusvika 101.0 muzana (yakaomeswa zvinhu).
VANHU
Kuonekwa: chena kana inenge chena poda.
Solubility: inenge isinganyungudike mumvura, inonyungudika zvakasununguka mu ethanol (96 muzana), inonyungudika zvishoma muacetone, isinganyungudika mumethylene chloride.
mp: inenge 202 ℃.
KUZIVA
Kuzivikanwa kwekutanga: A.
Kuzivikanwa kwechipiri: B, C.
A. Infrared absorption spectrophotometry (2.2.24).
Kuenzanisa: Ursodeoxycholic Acid CRS.
B. Ongorora machromatograms akawanikwa mukuedzwa kwekusachena C.
Mibairo: nzvimbo huru muchromatogram yakawanikwa nebvunzo mhinduro (b) yakafanana pachinzvimbo, ruvara uye saizi kunzvimbo huru muchromatogram yakawanikwa nereferensi mhinduro (a).
C. Dissolve nezve 10 mg mu 1 mL ye sulfuric acid R. Wedzera 0.1 mL ye formaldehyde solution R uye bvumira kumira kwemaminitsi mashanu.Wedzera 5 mL yemvura R. Kumiswa kunowanikwa kune greenish-blue.
ZVIYEDZO
Yakananga optical rotation (2.2.7): + 58.0 kusvika + 62.0 (yakaomeswa zvinhu).
Dissolve 0.500 g mu anhydrous ethanol R uye diluted kusvika 25.0 mL neine solvent yakafanana.
Kusachena C. Thin-layer chromatography (2.2.27).
Solvent musanganiswa: mvura R, acetone R (10:90 V/V).
Muedzo mhinduro (a).Dissolve 0.40 g yechinhu chinofanirwa kuongororwa mumusanganiswa wekunyungudutsa uye diluted kusvika 10 mL nemusanganiswa wekunyungudutsa.
Mhinduro yekuedza (b).Dilute 1 mL yebvunzo mhinduro (a) kusvika 10 mL nemusanganiswa wekunyungudutsa.
Reference solution (a).Dissolve 40 mg yeursodeoxycholic acid CRS mumusanganiswa wekunyungudutsa uye wedzera kusvika ku10 mL nemusanganiswa wekunyungudutsa.
Reference solution (b).Dissolve 20 mg ye lithocholic acid CRS (kusvibiswa C) mumusanganiswa wekunyungudutsa uye dilute kusvika ku10.0 mL nemusanganiswa wekunyungudutsa (mhinduro A).Dilute 2.0 mL yemhinduro iyi kusvika ku100.0 mL nemusanganiswa wekunyungudutsa.
Reference solution (c).Ku 5 mL yemhinduro A wedzera 10 mg ye chenodeoxycholic acid CRS (kusvibiswa A) uye dilute kusvika ku50 mL nemusanganiswa wekunyungudutsa.
Plate: TLC silica gel ndiro R.
Nharembozha: glacial acetic acid R, acetone R, methylenechloride R (1:30:60 V/V/V).
Kushandisa: 5μL.
Kubudirira: pamusoro pe2/3 yeplate.
Kuomesa: pa 120 ℃ ye 10 min.
Kuona: pfapfaidza nekukasika ne47.6 g/L solution yephosphomolybdic acid R mumusanganiswa we1 volume ye sulfuric acid R uye 20 mavhoriyamu eglacial acetic acid R uye kupisa pa120 ℃ kusvika makwapa eblue aonekwa kuseri kwakareruka.
Kukodzera kweSystem: Reference solution (c):
- chromatogram inoratidza 2 akaparadzaniswa zvakajeka makwapa makuru.
Limit: bvunzo mhinduro (a):
-kusachena C: chero nzvimbo nekuda kwekusachena C haina kunyanyisa kupfuura nzvimbo huru muchromatogram yakawanikwa nereferensi mhinduro (b) (0.1 muzana).
Zvinoenderana zvinhu.Liquid chromatography (2.2.29).
Solvent musanganiswa: methanol R, mobile phase (10:90 V/V).
Test mhinduro.Dissolve 60 mg yechinhu chinofanirwa kuongororwa mumusanganiswa wekunyungudutsa uye diluted kusvika 20.0 mL nemusanganiswa wekunyungudutsa.
Reference solution (a).Dissolve zviri mubhodhoro reUrsodeoxycholic Acid yekukodzera system CRS (ine tsvina A uye H) mu1.0 mL yemusanganiswa wekunyungudutsa.
Reference solution (b).Dilute 1.0 mL yemubvunzo wemhinduro ku100.0 mL nemusanganiswa wekunyungudutsa.Dilute 1.0 mL yemhinduro iyi kusvika 10.0 mL nemusanganiswa we solvent.
Column:
-kukura: l = 0.25 m, Ø = 4.6 mm;
-stationary phase: end-capped octadecylsilyl silica gel yechromatography R (5 μm);
-tembiricha: 40℃ ± 1℃.
Nharembozha: sanganisa makumi matatu mavhoriyamu eacetonitrile R, 37 mavhoriyamu e0.78 g/L mhinduro ye sodium dihydrogen phosphate R yakagadziridzwa kuita pH 3 ine phosphoric acid R, uye makumi mana mavhoriyamu emethanol R.
Kuyerera kweyero: 0.8 mL/min.
Kuonekwa: refractometer pa 35 ± 1 ℃.
Jekiseni: 150 μL.
Nguva yekumhanya: 4 nguva yekuchengeta nguva yeUrsodeoxycholic Acid.
Kuzivikanwa kwetsvina: shandisa chromatogram yakapihwa ursodeoxycholic acid yekukodzera system CRS uye chromatogram yakawanikwa ine referensi mhinduro (a) kuona makwiriro nekuda kwetsvina A uye H.
Kuchengetwa kwehukama maererano neursodeoxycholic acid (nguva yekuchengetedza = inenge 14 min): tsvina H = inenge 0.9;kusachena A = anenge 2.8.
Kukodzera kweSystem: Reference solution (a):
-resolution: zvishoma 1.5 pakati pepamusoro nekuda kwekusachena H uye ursodeoxycholic acid.
Miganhu:
- kusachena A: kwete kupfuura 10 nguva nzvimbo yepamusoro peak muchromatogram yakawanikwa nereferensi mhinduro (b) (1.0 muzana);
-kusvibiswa kusingazivikanwe: kune imwe neimwe kusachena, kwete kupfuura nzvimbo yepamusoro peak muchromatogram yakawanikwa nereferensi mhinduro (b) (0.10 muzana);
- yakazara: isingasviki ka15 nzvimbo yenzvimbo yepamusoro muchromatogram yakawanikwa nereferensi mhinduro (b) (1.5 muzana);
-kuregeredza muganhu: 0.5 nguva yenzvimbo yepamusoro peak muchromatogram yakawanikwa nereferensi mhinduro (b) (0.05 muzana).
Heavy metals (2.4.8): yakawanda 20 ppm.
1.0 g inopindirana nemuedzo C. Gadzirira mhinduro yereferensi uchishandisa 2 mL ye lead standard solution (10 ppm Pb) R.
Kurasikirwa pakuomeswa (2.2.32): yakakura 1.0 muzana, yakatarwa pa1.000 g nekuomesa muchoto pa105 ℃.
Sulfated ash (2.4.14): yakawanda 0.1 muzana, yakatarwa pa 1.0 g.
ASSAY
Dissolve 0.350 g mu 50 mL ye ethanol (96 per cent) R, yakambogadziriswa kusvika 0.2 mL ye phenolphthalein solution R. Wedzera 50 mL yemvura R uye titrate ne 0.1 M sodium hydroxide kusvikira ruvara rwepinki rwawanikwa.
1 mL ye0.1 M sodium hydroxide yakaenzana ne 39.26 mg yeC24H40O4.
KUSIRIRA
Kusachena kwaitaurwa: A, C.
Kumwe kusachena kunoonekwa (zvinhu zvinotevera, kana zviripo pamwero wakakwana, zvinoonekwa neimwe kana imwe yebvunzo mumonograph. Zvinoganhurirwa nechiyero chekugamuchira kune zvimwe/zvisina kutaurwa uye/kana negeneral monograph Substances. yekushandiswa kwemishonga (2034) Naizvozvo hazvina kufanira kuzivisa tsvina iyi kuratidza kutevedza.Onawo 5.10.
Kudzora kusvibiswa muzvinhu zvekushandiswa kwemishonga): B, D, E, F, G, H, I.
A. 3α,7α-dihydroxy-5β-cholan-24-oic acid (chenodeoxycholic acid),
B. 3α, 7α, 12α-trihydroxy-5β-cholan-24-oic acid (cholic acid),
C. 3α-hydroxy-5β-cholan-24-oic acid (lithocholic acid),
D. 3α,7β,12α-trihydroxy-5β-cholan-24-oic acid (ursocholic acid),
E. 3α,12α-dihydroxy-5β-cholan-24-oic acid (deoxycholic acid),
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.