Glycyrrhetic Acid (Enoxolone) CAS 471-53-4 Assay 98.0~101.0% (Potentiometry)

Litsebiso tse akaretsang
(Monograph oa Ph Eur 1511)
C30H46O4 470.7 471-53-4
Ts'ebetso le tšebeliso
Phekolo ea lefu la benign peptic ulcer.
Ph Eur
TLHALOSO
(20β) -3β-Hydroxy-11-oxo-olean-12-en-29-oic acid.
Litaba
98.0 lekholong ho isa ho 101.0 lekholong (ntho e omisitsoeng).
LIEKETSENG
Ponahalo
Phofo ea kristale e tšoeu kapa e batlang e le tšoeu.
Solubility
Ha e khone ho qhibiliha ka metsing, e qhibiliha ka har'a ethanol, e qhibiliha hanyenyane ka methylene chloride.
E bontša polymorphism (5.9).
TS'ELISO TS'OANE
Boitsebiso ba pele A.
Boitsebiso ba bobeli B, C.
A. Hlahloba ka infrared absorption spectrophotometry (2.2.24).
Papiso Enoxolone CRS.
Haeba ponahalo e fumanoeng boemong bo tiileng e bontša phapang, qhala 0.2 g ea ntho e lokelang ho hlahlojoa le 0.2 g ea ntho ea litšupiso ka thoko ho 6 ml ea ethanol R. Beha ka tlas'a
reflux condenser bakeng sa 1 h 'me u kenye 6 ml ea metsi R. Ho thehoa precipitate.Pholile ho isa ho 10 ℃ 'me u sefa ka thuso ea vacuum.Hlatsoa metsi ka 10 ml ea joala R, e omelle ka ontong ea 80 ℃ 'me u rekote ponahalo e ncha.
B. Thin-layer chromatography (2.2.27).
Tharollo ea teko Qhala 10 mg ea ntho e lokelang ho hlahlojoa ka methylene chloride R 'me u hlapolle ho 10 ml ka solvent e tšoanang.
Tharollo ea Reference Hlakola 10 mg ea enoxolone CRS ka methylene chloride R 'me u hlapolle ho 10 ml ka solvent e tšoanang.
Plate TLC silica gel poleiti R.
Mobile phase glacial acetic acid R, acetone R, methylene chloride R (5:10:90 V/V/V).
Tšebeliso ea 5µl.
Nts'etsopele Ho feta 2/3 ea poleiti.
Ho omisa moeeng bakeng sa 5 min.
Ho lemoha Spray ka tharollo ea anisaldehyde R le mocheso ho 100-105 ℃ bakeng sa 10 min.Liphetho Sebaka sa mantlha sa chromatogram se fumanoeng ka tharollo ea tlhahlobo se tšoana ka boemo, 'mala le boholo le sebaka sa mantlha ho chromatogram e fumanoeng ka referense.
tharollo.
C. Hlakola 50 mg ka 10 ml ea methylene chloride R. Ho 2 ml ea tharollo ena, eketsa 1 ml ea acetic anhydride R le 0,3 ml ea sulfuric acid R. Ho hlahisoa 'mala o pinki.
LITEKO
Ponahalo ea tharollo
Tharollo e hlakile (2.2.1) mme ha e na mebala e matla ho feta tharollo ea Y6 (2.2.2, Method II).
Qhala 0.1 g ka ethanol R 'me u hlapolle ho 10 ml ka solvent e tšoanang.
Potoloho e khethehileng ea optical (2.2.7) + 145 ho + 154 (ntho e omisitsoeng).
Hlakola 0.50 g ka dioxan R 'me u hlapolle ho 50.0 ml ka solvent e tšoanang.
Lintho tse amanang
Mokelikeli oa chromatography (2.2.29).
Tharollo ea liteko Hlakola 0.10 g ea ntho e tla hlahlojoa mohatong oa selefouno ebe o hlapolla ho 100.0 ml ka mohato oa mohala.
Tharollo ea litšupiso (a) Hlakola 2.0 ml ea tharollo ea teko ho 100.0 ml ka mohato oa selefouno.
Tharollo ea litšupiso (b) Hlakola 5.0 ml ea tharollo ea litšupiso (a) ho 100.0 ml ka mohato oa mohala.
Tharollo ea litšupiso (c) Hlakola 0.1 g ea 18α-glycyrrhetinic acid R ka tetrahydrofuran R 'me u hlapolle ho 100.0 ml ka solvent e tšoanang.Ho 2.0 ml ea tharollo, eketsa 2.0 ml ea tharollo ea teko 'me u hlapolle ho 100.0 ml ka mohato oa selefouno.
Kholomo:
- boholo: l = 0.25 m, Ø = 4.6 limilimithara,
-mohato o emeng: octadecylsilyl silica gel bakeng sa chromatography R (5 µm),
- mocheso: 30 ℃.
Mobile phase Mix 430 volumes ea tetrahydrofuran R le 570 volumes ea 1.36 g/l solution ea sodium acetate R e fetotsoeng ho pH 4.8 le glacial acetic acid R.
Sekhahla sa phallo 0.8 ml / min.
Spectrophotometer ea ho lemoha ho 250 nm.
Ente ea 20 µl loop ente;enta tharollo ea teko le litharollo tsa litšupiso.
Nako ea ho matha makhetlo a 4 ho feta nako ea Enoxolone.
Ho nepahala ha sistimi:
-resolution: bonyane ba 2.0 lipakeng tsa litlhoro ka lebaka la enoxolone le 18α-glycyrrhetinic acid ka har'a chromatogram e fumanoeng ka tharollo ea litšupiso (c).
Meeli:
- litšila leha e le life: ha ho makhetlo a fetang 7 sebaka sa tlhoro e ka sehloohong ea chromatogram e fumanoeng ka tharollo ea litšupiso (b) (0.7 lekholong),
-kakaretso: eseng ho feta sebaka sa tlhoro ea mantlha ea chromatogram e fumanoeng ka tharollo ea litšupiso (a) (2.0 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 dumellana le teko ya moedi F. Lokisetsa maemo o sebedisa 2 ml ya tharollo e tlwaelehileng ya loto (10 ppm Pb) R.
Tahlehelo nakong ea ho omisa (2.2.32) Boholo ba 0.5 peresente, bo lekantsoeng ho 1.000 g ka ho omisa ka ontong ka 105 ℃ bakeng sa 4 h.
Molora o nang le sulphated (2.4.14) Boholo ba karolo ea 0,2 lekholong, e ikemiselitseng ho 1.0 g.
TLHOKOMELO
Hlakola 0.330 g ka 40 ml ea dimethylformamide R. Titrate le 0.1 M tetrabutylammonium hydroxide, ho khetholla ntlha ea ho qetela ea potentiometrically (2.2.20).Etsa titration e se nang letho.1 ml ea 0.1 M tetrabutylammonium hydroxide e lekana le 47.07 mg ea C30H46O4
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POLOKO
Sireletsoa kganya.
LITŠILA
A. (20β) -3β-hydroxy-11-oxo-18α-olean-12-en-29-oic acid,
B. (4β,20β) -3β,23-dihydroxy-11-oxo-olean-12-en-29-oic acid.
Ph Eur