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

URSODEOXYCHOLIC ACID
C24H40O4 Mong 392.6[128-13-2]
TLHALOSO
3α,7β-Dihydroxy-5β-cholan-24-oic acid.
Litaba: liperesente tse 99.0 ho isa ho liperesente tse 101.0 (lintho tse omisitsoeng).
LIEKETSENG
Ponahalo: phofo e tšoeu kapa e batlang e le tšoeu.
Solubility: hoo e batlang e sa qhibilihe ka metsing, e qhibiliha ka bolokolohi ka har'a ethanol (96 lekholong), e qhibiliha hanyenyane ka acetone, hoo e batlang e sa qhibilihe ka har'a methylene chloride.
mp: hoo e ka bang 202 ℃.
TS'ELISO TS'OANE
Boitsebiso ba pele: A.
Boitsebiso ba bobeli: B, C.
A. Infrared absorption spectrophotometry (2.2.24).
Papiso: Ursodeoxycholic Acid CRS.
B. Hlahloba li-chromatogram tse fumanoeng tekong bakeng sa ho se hloeke C.
Liphetho: sebaka sa mantlha sa chromatogram se fumanoeng ka tharollo ea tlhahlobo (b) se tšoana ka boemo, 'mala le boholo le sebaka sa mantlha sa chromatogram se fumanoeng ka tharollo ea litšupiso (a).
C. Qhala hoo e ka bang 10 mg ho 1 mL ea sulfuric acid R. Eketsa 0.1 mL ea tharollo ea formaldehyde R mme u lumelle ho ema metsotso e 5.Kenya 5 mL ea metsi R. Ho emisoa ho fumanoeng ke botala bo botala.
LITEKO
Potoloho e khethehileng ea optical (2.2.7): + 58.0 ho + 62.0 (ntho e omisitsoeng).
Qhala 0.500 g ka anhydrous ethanol R 'me u hlapolle ho 25.0 mL ka solvent e tšoanang.
Tšilafalo C. Thin-layer chromatography (2.2.27).
Motsoako oa solvent: metsi R, acetone R (10:90 V / V).
Tharollo ea teko (a).Qhala 0.40 g ea ntho e lokelang ho hlahlobjoa ka har'a motsoako oa solvent mme o hlapolle ho 10 ml ka motsoako oa solvent.
Tharollo ea teko (b).Hlakola 1 mL ea tharollo ea teko (a) ho 10 ml ka motsoako oa solvent.
Tharollo ea litšupiso (a).Qhala 40 mg ea ursodeoxycholic acid CRS ka har'a motsoako oa solvent 'me u hlapolle ho 10 ml ka motsoako oa solvent.
Tharollo ea litšupiso (b).Qhala 20 mg ea lithocholic acid CRS (ho se hloeke C) motsoakong oa motsoako 'me u hlapolle ho 10.0 mL ka motsoako oa motsoako (tharollo A).Hlakola 2.0 mL ea tharollo ena ho 100.0 mL ka motsoako oa solvent.
Tharollo ea litšupiso (c).Ho 5 mL ea tharollo A eketsa 10 mg ea chenodeoxycholic acid CRS (litšila A) 'me u hlapolle ho 50 mL ka motsoako oa solvent.
Plate: TLC silica gel plate R.
Mobile phase: glacial acetic acid R, acetone R, methylenechloride R (1:30:60 V/V/V).
Kopo: 5μL.
Nts'etsopele: ho feta 2/3 ea poleiti.
Ho omisa: ka 120 ℃ bakeng sa 10 min.
Ho lemoha: fafatsa hang-hang ka tharollo ea 47.6 g/L ea phosphomolybdic acid R ka motsoako oa 1 volume ea sulfuric acid R le li-volume tse 20 tsa glacial acetic acid R le mocheso ho 120 ℃ ho fihlela matheba a maputsoa a hlaha mokokotlong o bobebe.
Ho tšoaneleha ha sistimi: tharollo ea litšupiso (c):
- chromatogram e bonts'a matheba a mantlha a 2 a arohaneng ka ho hlaka.
Moeli: tharollo ea teko (a):
-tšila C: sebaka sefe kapa sefe ka lebaka la ho se hloeke C ha se matla ho feta sebaka se ka sehloohong sa chromatogram se fumanoeng ka tharollo ea litšupiso (b) (0.1 lekholong).
Lintho tse amanang.Mokelikeli oa chromatography (2.2.29).
Motsoako oa solvent: methanol R, mobile phase (10: 90 V / V).
Tharollo ea teko.Qhala 60 mg ea ntho e lokelang ho hlahlojoa motsoakong oa solvent ebe o hlapolla ho 20.0 mL ka motsoako oa solvent.
Tharollo ea litšupiso (a).Hlakola likahare tsa vial ea Ursodeoxycholic Acid bakeng sa tsamaiso ea CRS e loketseng (e nang le litšila A le H) ka 1.0 mL ea motsoako oa solvent.
Tharollo ea litšupiso (b).Hlakola 1.0 mL ea tharollo ea teko ho 100.0 mL ka motsoako oa solvent.Hlakola 1.0 mL ea tharollo ena ho 10.0 mL ka motsoako oa solvent.
Kholomo:
-boholo: l = 0,25 m, Ø = 4,6 limilimithara;
-stationary phase: end-capped octadecylsilyl silica gel bakeng sachromatography R (5 μm);
- mocheso: 40 ℃ ± 1℃.
Mohato oa selefouno: kopanya li-volumes tse 30 tsa acetonitrile R, li-volumes tse 37 tsa 0.78 g/L tharollo ea sodium dihydrogen phosphate R e fetotsoeng ho pH 3 le phosphoric acid R, le methanol e 40 ea methanol R.
Sekhahla sa phallo: 0.8 mL / min.
Ho lemoha: refractometer ho 35 ± 1 ℃.
Ente: 150 μL.
Nako ea ho matha: makhetlo a 4 nako ea ho boloka Ursodeoxycholic Acid.
Ho tsebahatsa litšila: sebelisa chromatogram e fanoeng ka ursodeoxycholic acid bakeng sa ho nepahala ha sistimi ea CRS le chromatogram e fumanoeng ka tharollo ea litšupiso (a) ho supa litlhoro ka lebaka la litšila A le H.
Ho boloka kamano e amanang le ursodeoxycholic acid (nako ea ho boloka = hoo e ka bang 14 min): ho se hloeke H = hoo e ka bang 0.9;ho se hloeke A = hoo e ka bang 2,8.
Ho tšoaneleha ha sistimi: tharollo ea litšupiso (a):
-qeto: bonyane 1.5 pakeng tsa litlhōrō ka lebaka la ho se hloeke H le ursodeoxycholic acid.
Meeli:
- ho se hloeke A: ha ho makhetlo a fetang 10 sebaka sa tlhōrō e ka sehloohong ea chromatogram e fumanoang ka tharollo ea litšupiso (b) (1.0 lekholong);
- litšila tse sa hlalosoang: bakeng sa ho se hloeke ka 'ngoe, eseng ho feta sebaka sa tlhōrō e ka sehloohong ea chromatogram e fumanoang ka tharollo ea litšupiso (b) (0.10 lekholong);
- kakaretso: eseng makhetlo a fetang 15 sebaka sa tlhōrō e ka sehloohong ea chromatogram e fumanoeng ka tharollo ea litšupiso (b) (1,5 lekholong);
- ho hlokomoloha moeli: makhetlo a 0.5 sebaka sa tlhōrō e ka sehloohong ea chromatogram e fumanoang ka tharollo ea litšupiso (b) (0.05 lekholong).
Litšepe tse boima (2.4.8): boholo ba 20 ppm.
1.0 g e lumellana le teko C. Lokisetsa tharollo ea litšupiso u sebelisa 2 mL ea tharollo e tloaelehileng ea loto (10 ppm Pb) R.
Tahlehelo ka ho omisa (2.2.32): boholo ba 1.0 peresente, e ikemiselitseng ho 1.000 g ka ho omisa ka ontong ho 105 ℃.
Sulfated molora (2.4.14): boholo ba karolo ea 0,1 lekholong, e ikemiselitseng ho 1.0 g.
TLHOKOMELO
Qhala 0.350 g ka 50 mL ea ethanol (96 lekholong) R, pele e ne e sa sebetse ho 0.2 mL ea phenolphthalein tharollo R. Eketsa 50 mL ea metsi R le titrate ka 0.1 M sodium hydroxide ho fihlela 'mala o pinki o fumanoa.
1 mL ea 0.1 M sodium hydroxide e lekana le 39.26 mg ea C24H40O4.
LITŠILA
Litšila tse boletsoeng: A, C.
Litšila tse ling tse ka bonoang (lintho tse latelang, haeba li le maemong a lekaneng, li ka bonoa ke tlhahlobo e le 'ngoe kapa tse ling ho monograph. Li lekantsoe ke mokhoa oa ho amohela ka kakaretso bakeng sa litšila tse ling/tse sa hlalosoang le/kapa ke monograph Kakaretso. bakeng sa tšebeliso ea meriana (2034) Ka hona ha ho hlokahale ho tsebahatsa litšila tsena bakeng sa pontšo ea ho lumellana le melao.Sheba hape 5.10.
Taolo ea litšila linthong bakeng sa tšebeliso ea meriana): 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.