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

General Notices
(Ph Eur monograph 1511)
C30H46O4 470.7 471-53-4
Chiito uye kushandiswa
Kurapa kwe benign peptic ulcer chirwere.
Ph Eur
DEFINITION
(20β) -3β-Hydroxy-11-oxo-olean-12-en-29-oic acid.
Content
98.0 muzana kusvika 101.0 muzana (yakaomeswa zvinhu).
VANHU
Chitarisiko
Ichena kana inenge yakachena crystalline powder.
Solubility
Inenge isinganyungudike mumvura, inonyungudika mu ethanol, inonyungudika zvishoma mumethylene chloride.
Inoratidza polymorphism (5.9).
KUZIVA
Chiziviso chekutanga A.
Chechipiri kuzivikanwa B, C.
A. Ongorora ne infrared absorption spectrophotometry (2.2.24).
Kuenzanisa Enoxolone CRS.
Kana iyo spectra yakawanikwa mumamiriro akasimba ichiratidza misiyano, nyungudutsa 0.2 g yechinhu chinofanira kuongororwa uye 0.2 g yechinhu chinotaridzirwa zvakasiyana mu 6 ml ye ethanol R. Birisa pasi
reflux condenser ye1 h uye kuwedzera 6 ml yemvura R. A precipitate inoumbwa.Kutonhorera kusvika ku10 ℃ uye sefa nerubatsiro rwevacuum.Geza mvura ine 10 ml yedoro R, yakaoma muchoto pa80 ℃ uye rekodha mitsva.
B. Thin-layer chromatography (2.2.27).
Test solution Dissolve 10 mg yechinhu chinofanirwa kuongororwa mumethylene chloride R uye dilute kusvika ku10 ml nemusanganiswa wakafanana.
Reference solution Dissolve 10 mg ye enoxolone CRS mu methylene chloride R uye dilute kusvika 10 ml nemusanganiswa wakafanana.
Plate TLC silica gel ndiro R.
Mobile phase glacial acetic acid R, acetone R, methylene chloride R (5:10:90 V/V/V).
Kushandisa 5µl.
Kuvandudza Kupfuura 2/3 yeplate.
Kuomesa Mumhepo kwe5 min.
Detection Spray ne anisaldehyde solution R uye kupisa pa100-105 ℃ kwemaminetsi gumi.Mhinduro Nzvimbo huru muchromatogram yakawanikwa nemhinduro yebvunzo yakafanana pachinzvimbo, ruvara uye saizi kunzvimbo huru muchromatogram yakawanikwa nereferensi.
mhinduro.
C. Dissolve 50 mg mu 10 ml ye methylene chloride R. Ku 2 ml yemhinduro iyi, wedzera 1 ml yeacetic anhydride R uye 0.3 ml ye sulfuric acid R. Muvara wepinki unogadzirwa.
ZVIYEDZO
Kuonekwa kwemhinduro
Mushonga wacho wakajeka (2.2.1) uye kwete zvakanyanya ruvara kupfuura referensi mhinduro Y6 (2.2.2, Method II).
Dissolve 0.1 g mu ethanol R uye shandura kusvika 10 ml neine solvent yakafanana.
Yakananga optical rotation (2.2.7) + 145 kusvika + 154 (yakaomeswa zvinhu).
Dissolve 0.50 g mu dioxan R uye shandura kusvika ku 50.0 ml neine solvent yakafanana.
Zvinhu zvinoenderana
Liquid chromatography (2.2.29).
Muedzo mhinduro Dissolve 0.10 g yechinhu kuti chiongororwe muchikamu chenhare uye wedzera kusvika ku100.0 ml nechikamu chenhare.
Reference solution (a) Dilute 2.0 ml yebvunzo mhinduro ku100.0 ml nechikamu chenhare.
Reference solution (b) Dilute 5.0 ml yereferensi solution (a) kusvika 100.0 ml nechikamu chenhare.
Reference solution (c) Dissolve 0.1 g ye 18α-glycyrrhetinic acid R mu tetrahydrofuran R uye shandura kusvika ku100.0 ml neine solvent yakafanana.Ku 2.0 ml yemhinduro, wedzera 2.0 ml yemhinduro yekuyedza uye deredza kusvika ku100.0 ml nechikamu chenhare.
Column:
-saizi: l = 0.25 m, Ø = 4.6 mm,
-stationary phase: octadecylsilyl silica gel yechromatography R (5 µm),
-tembiricha: 30 ℃.
Mobile phase Mix 430 mavhoriyamu etetrahydrofuran R uye 570 mavhoriyamu e1.36 g/l mhinduro yesodium acetate R yakagadziridzwa kuita pH 4.8 ine glacial acetic acid R.
Kuyerera kwe 0.8 ml / min.
Detection Spectrophotometer pa250 nm.
Jekiseni 20 µl loop jekiseni;jekiseni mhinduro yebvunzo uye mhinduro dzekutarisa.
Mhanyai nguva 4 nguva yekuchengeta Enoxolone.
Kukodzera kweSystem:
-resolution: shoma ye2.0 pakati pepamusoro nekuda kweenoxolone uye ku18α-glycyrrhetinic acid muchromatogram yakawanikwa nereferensi mhinduro (c).
Miganhu:
-chero kusachena: kwete kupfuura 7 nguva yenzvimbo yepamusoro peak muchromatogram yakawanikwa nereferensi mhinduro (b) (0.7 muzana),
-total: isingasviki nzvimbo yepamusoro peak muchromatogram yakawanikwa nereferensi mhinduro (a) (2.0 muzana),
-kuregeredza muganho: 0.5 nguva yenzvimbo yepamusoro peak muchromatogram yakawanikwa nereferensi mhinduro (b) (0.05 muzana).
Heavy metals (2.4.8) Maximum 20 ppm.
1.0 g inowirirana nemuganhu bvunzo F. Gadzirira mwero uchishandisa 2 ml yemutobvu yakajairwa mhinduro (10 ppm Pb) R.
Kurasikirwa pakuomeswa (2.2.32) Maximum 0.5 per cent, yakatarwa pa1.000 g nekuomesa muchoto pa105 ℃ kwe4 h.
Sulphated ash (2.4.14) Maximum 0.2 per cent, yakatarwa pa 1.0 g.
ASSAY
Dissolve 0.330 g mu 40 ml ye dimethylformamide R. Titrate ne 0.1 M tetrabutylammonium hydroxide, inotarisa kuguma-kunogoneka (2.2.20).Ita titration isina chinhu.1 ml ye0.1 M tetrabutylammonium hydroxide yakaenzana ne47.07 mg yeC30H46O4
Crown Copyright 2006 330 46 4
STORAGE
Kudzivirirwa kubva kuchiedza.
KUSIRIRA
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