Ursodeoxycholic Acid (UDCA) CAS 128-13-2 Kev Ntsuam Xyuas 99.0 ~ 101.0%

URSODEOXYCHOLIC ACID
C24H40O4 Mr 392.6[128-13-2]
DEFINITION
3a,7β-Dihydroxy-5β-cholan-24-oic acid.
Cov ntsiab lus: 99.0 feem pua ​​​​rau 101.0 feem pua ​​(cov khoom qhuav).
CEEB TOOM
Qhov tsos: dawb los yog yuav luag dawb hmoov.
Solubility: xyaum insoluble nyob rau hauv dej, dawb do soluble nyob rau hauv ethanol (96 feem pua), me ntsis soluble nyob rau hauv acetone, xyaum insoluble nyob rau hauv methylene chloride.
mp: txog 202 ℃.
IDENTIFICATION
Kev txheeb xyuas thawj zaug: A.
Kev txheeb xyuas thib ob: B, C.
A. Infrared absorption spectrophotometry (2.2.24).
Sib piv: Ursodeoxycholic Acid CRS.
B. Tshawb xyuas cov chromatograms tau txais hauv kev sim rau impurity C.
Cov txiaj ntsig: qhov chaw tseem ceeb hauv chromatogram tau txais nrog cov tshuaj ntsuam xyuas (b) zoo ib yam hauv txoj hauj lwm, xim thiab qhov loj me rau qhov chaw tseem ceeb hauv chromatogram tau nrog kev siv tshuaj (a).
C. Dissolve txog 10 mg hauv 1 mL ntawm sulfuric acid R. Ntxiv 0.1 mL ntawm formaldehyde tov R thiab cia sawv ntsug rau 5 feeb.Ntxiv 5 mL dej R. Qhov kev ncua tau txais yog ntsuab-xiav.
KEV KAWM
Kev sib hloov kho qhov muag tshwj xeeb (2.2.7): + 58.0 txog + 62.0 (cov khoom qhuav).
Dissolve 0.500 g hauv anhydrous ethanol R thiab dilute mus rau 25.0 mL nrog tib cov kuab tshuaj.
Impurity C. Nyias-txheej chromatography (2.2.27).
Cov kuab tshuaj sib tov: dej R, acetone R (10: 90 V / V).
Test daws (a).Dissolve 0.40 g ntawm cov tshuaj yuav tsum tau soj ntsuam nyob rau hauv cov kuab tshuaj tov thiab dilute mus rau 10 mL nrog cov kuab tshuaj tov.
Test daws (b).Dilute 1 mL ntawm cov tshuaj ntsuam xyuas (a) mus rau 10 mL nrog cov kuab tshuaj sib tov.
Kev daws teeb meem (a).Dissolve 40 mg ntawm ursodeoxycholic acid CRS hauv cov kuab tshuaj sib tov thiab dilute mus rau 10 mL nrog cov kuab tshuaj sib tov.
Kev daws teeb meem (b).Dissolve 20 mg ntawm lithocholic acid CRS (impurity C) nyob rau hauv cov kuab tshuaj sib tov thiab dilute mus rau 10.0 mL nrog cov kuab tshuaj tov (solution A).Dilute 2.0 mL ntawm cov tshuaj no rau 100.0 mL nrog cov kuab tshuaj sib tov.
Kev daws teeb meem (c).Rau 5 mL ntawm kev daws A ntxiv 10 mg ntawm chenodeoxycholic acid CRS (impurity A) thiab dilute mus rau 50 mL nrog cov kuab tshuaj sib tov.
Phaj: TLC silica gel phaj R.
Mobile theem: glacial acetic acid R, acetone R, methyleneChloride R (1: 30: 60 V / V / V).
Daim ntawv thov: 5μL.
Kev loj hlob: tshaj 2/3 ntawm lub phaj.
Qhuav: ntawm 120 ℃ rau 10 min.
Kev kuaj pom: tsuag tam sim ntawd nrog 47.6 g / L tov ntawm phosphomolybdic acid R nyob rau hauv ib tug sib tov ntawm 1 ntim ntawm sulfuric acid R thiab 20 ntim ntawm glacial acetic acid R thiab tshav kub ntawm 120 ℃ kom txog thaum xiav me ntsis tshwm nyob rau hauv ib tug sib dua keeb kwm yav dhau.
System suitability: reference solution (c):
- lub chromatogram qhia tau hais tias 2 qhov chaw tseem ceeb sib cais.
Limit: test solution (a):
- impurity C: txhua qhov chaw vim impurity C tsis khaus ntau dua li qhov chaw tseem ceeb hauv chromatogram tau nrog kev siv tshuaj (b) (0.1 ib xees).
Cov khoom muaj feem xyuam.Ua kua chromatography (2.2.29).
Cov kuab tshuaj tov: methanol R, mobile theem (10:90 V / V).
Test daws.Dissolve 60 mg ntawm cov tshuaj yuav tsum tau soj ntsuam nyob rau hauv cov kuab tshuaj tov thiab dilute mus rau 20.0 mL nrog cov kuab tshuaj tov.
Kev daws teeb meem (a).Dissolve cov ntsiab lus ntawm lub vial ntawm Ursodeoxycholic Acid rau qhov system haum CRS (muaj impurities A thiab H) hauv 1.0 mL ntawm cov kuab tshuaj sib tov.
Kev daws teeb meem (b).Dilute 1.0 mL ntawm cov tshuaj ntsuam xyuas rau 100.0 mL nrog cov kuab tshuaj sib tov.Dilute 1.0 mL ntawm cov tshuaj no rau 10.0 mL nrog cov kuab tshuaj sib tov.
Kem:
Luas = 0.25 m, Ø 4.6 mm.
-stationary theem: kawg-capped octadecylsilyl silica gel rauchromatography R (5 μm);
- Kub: 40 ℃ ± 1 ℃.
Txawb theem: sib tov 30 ntim ntawm acetonitrile R, 37 ntim ntawm 0.78 g / L tov ntawm sodium dihydrogen phosphate R hloov mus rau pH 3 nrog phosphoric acid R, thiab 40 ntim ntawm methanol R.
Tus nqi ntws: 0.8 mL / min.
Kev kuaj pom: refractometer ntawm 35 ± 1 ℃.
Kev txhaj tshuaj: 150 μL.
Lub sijhawm ua haujlwm: 4 zaug lub sijhawm khaws cia ntawm Ursodeoxycholic Acid.
Kev txheeb xyuas cov impurities: siv cov chromatogram muab nrog ursodeoxycholic acid rau qhov system haum CRS thiab cov chromatogram tau txais nrog kev siv tshuaj (a) txhawm rau txheeb xyuas cov peaks vim impurities A thiab H.
Cov txheeb ze tuav nrog siv rau ursodeoxycholic acid (lub sij hawm tuav = txog 14 min): impurity H = txog 0.9;impurity A = txog 2.8.
System suitability: reference solution (a):
-kev daws teeb meem: yam tsawg kawg 1.5 ntawm lub ncov vim impurity H thiab ursodeoxycholic acid.
txwv:
- impurity A: tsis pub ntau tshaj 10 npaug ntawm thaj tsam ntawm lub hauv paus ncov hauv chromatogram tau nrog kev siv tshuaj (b) (1.0 feem pua);
-unspecified impurities: rau txhua impurity, tsis ntau tshaj qhov chaw ntawm lub hauv paus ncov nyob rau hauv lub chromatogram tau nrog siv tshuaj (b) (0.10 ib xees);
- tag nrho: tsis pub ntau tshaj 15 npaug ntawm thaj tsam ntawm lub hauv paus ncov hauv chromatogram tau nrog kev siv tshuaj (b) (1.5 feem pua);
-tsis quav ntsej txwv: 0.5 npaug ntawm thaj tsam ntawm lub hauv paus ncov hauv chromatogram tau nrog kev siv tshuaj (b) (0.05 feem pua).
Cov hlau hnyav (2.4.8): siab tshaj 20 ppm.
1.0 g ua raws li kev xeem C. Npaj cov kev siv tshuaj siv 2 mL ntawm cov tshuaj txhuas txhuas (10 ppm Pb) R.
Poob ntawm ziab (2.2.32): siab tshaj 1.0 feem pua, txiav txim siab ntawm 1.000 g los ntawm ziab hauv qhov cub ntawm 105 ℃.
Sulfated tshauv (2.4.14): siab tshaj 0.1 feem pua, txiav txim siab ntawm 1.0 g.
QHIA
Dissolve 0.350 g nyob rau hauv 50 mL ntawm ethanol (96 ib xees) R, yav tas los neutralized rau 0.2 mL ntawm phenolphthalein tov R. Ntxiv 50 mL dej R thiab titrate nrog 0.1 M sodium hydroxide kom txog thaum ib tug liab xim.
1 mL ntawm 0.1 M sodium hydroxide yog sib npaug rau 39.26 mg ntawm C24H40O4.
IMPURITIES
Specified impurities: A, C.
Lwm yam impurities kuaj tau (cov tshuaj hauv qab no yuav, yog tias muaj nyob rau theem txaus, raug kuaj pom los ntawm ib lossis lwm qhov ntawm cov kev sim hauv monograph. rau kev siv tshuaj (2034) Yog li tsis tas yuav tsum txheeb xyuas cov impurities no rau kev ua kom pom kev ua raws cai. Saib ntxiv 5.10.
Tswj cov impurities hauv cov tshuaj siv tshuaj): 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.