Glycyrrhetic Acid (Enoxolone) CAS 471-53-4 Kev Ntsuam Xyuas 98.0 ~ 101.0% (Potentiometry)

Daim Ntawv Ceeb Toom
(Ph Eur monograph 1511)
C30H46O4 470.7 471-53-4
Kev ua thiab siv
Kev kho mob ntawm benign peptic ulcer kab mob.
Ph Eur
DEFINITION
(20β)-3β-Hydroxy-11-oxo-olean-12-en-29-oic acid.
Cov ntsiab lus
98.0 feem pua ​​​​rau 101.0 feem pua ​​(cov khoom qhuav).
CEEB TOOM
Qhov tshwm sim
Dawb los yog yuav luag dawb crystalline hmoov.
Solubility
Xyaum insoluble hauv dej, soluble hauv ethanol, sparingly soluble hauv methylene chloride.
Nws qhia txog polymorphism (5.9).
IDENTIFICATION
Thawj daim ID A.
II ID B, C.
A. Tshawb xyuas los ntawm infrared absorption spectrophotometric (2.2.24).
Sib piv Enoxolone CRS.
Yog hais tias lub spectrum tau txais nyob rau hauv lub xeev cov khoom muaj qhov sib txawv, yaj 0.2 g ntawm cov tshuaj yuav tsum tau kuaj thiab 0.2 g ntawm cov ntaub ntawv siv cais nyob rau hauv 6 ml ntawm ethanol R. Boil nyob rau hauv
reflux condenser rau 1 h thiab ntxiv 6 ml dej R. A precipitate yog tsim.Txias mus txog 10 ℃ thiab lim nrog kev pab ntawm lub tshuab nqus tsev.Ntxuav lub precipitate nrog 10 ml ntawm cawv R, qhuav nyob rau hauv ib lub qhov cub ntawm 80 ℃ thiab sau tshiab spectra.
B. Nyias-txheej chromatography (2.2.27).
Kuaj cov tshuaj Dissolve 10 mg ntawm cov tshuaj yuav tsum tau kuaj nyob rau hauv methylene chloride R thiab dilute mus rau 10 ml nrog tib hnyav.
Kev siv tshuaj Dissolve 10 mg ntawm enoxolone CRS hauv methylene chloride R thiab dilute mus rau 10 ml nrog tib cov kuab tshuaj.
Phaj TLC silica gel phaj R.
Mobile theem glacial acetic acid R, acetone R, methylene chloride R (5: 10: 90 V / V / V).
Daim ntawv thov 5 µl.
Kev loj hlob tshaj 2/3 ntawm lub phaj.
Qhuav hauv huab cua rau 5 min.
Kev Tshawb Fawb Txau nrog cov tshuaj anisaldehyde R thiab cua sov ntawm 100-105 ℃ rau 10 min.Cov txiaj ntsig Qhov chaw tseem ceeb hauv chromatogram tau txais nrog cov tshuaj ntsuam xyuas yog qhov zoo sib xws hauv txoj hauj lwm, xim thiab qhov loj me rau qhov chaw tseem ceeb hauv chromatogram tau nrog kev siv
daws.
C. Dissolve 50 mg nyob rau hauv 10 ml ntawm methylene chloride R. Rau 2 ml ntawm cov tshuaj no, ntxiv 1 ml ntawm acetic anhydride R thiab 0.3 ml ntawm sulfuric acid R. Ib tug liab xim yog tsim.
KEV KAWM
Qhov tshwm sim ntawm kev daws teeb meem
Cov tshuaj yog qhov tseeb (2.2.1) thiab tsis muaj xim ntau dua li siv tshuaj Y6 (2.2.2, Txoj Kev II).
Dissolve 0.1 g hauv ethanol R thiab dilute mus rau 10 ml nrog tib cov kuab tshuaj.
Kev sib hloov kho qhov muag tshwj xeeb (2.2.7) + 145 txog + 154 (cov khoom qhuav).
Dissolve 0.50 g hauv dioxan R thiab dilute mus rau 50.0 ml nrog tib cov kuab tshuaj.
Cov khoom muaj feem xyuam
Ua kua chromatography (2.2.29).
Kuaj cov tshuaj Dissolve 0.10 g ntawm cov tshuaj yuav tsum tau kuaj nyob rau hauv lub mobile theem thiab dilute mus rau 100.0 ml nrog rau lub mobile theem.
Kev siv tshuaj (a) Dilute 2.0 ml ntawm cov tshuaj ntsuam xyuas rau 100.0 ml nrog rau theem mobile.
Kev siv tshuaj (b) Dilute 5.0 ml ntawm kev siv tshuaj (a) rau 100.0 ml nrog rau theem mobile.
Kev siv tshuaj (c) Dissolve 0.1 g ntawm 18α-glycyrrhetinic acid R hauv tetrahydrofuran R thiab dilute mus rau 100.0 ml nrog tib cov kuab tshuaj.Rau 2.0 ml ntawm cov tshuaj, ntxiv 2.0 ml ntawm cov tshuaj ntsuam xyuas thiab dilute mus rau 100.0 ml nrog rau theem mobile.
Kem:
Luas = 0.25 m, Ø 4.6 mm.
-stationary theem: octadecylsilyl silica gel rau chromatography R (5 µm),
- Kub: 30 ℃.
Txawb theem Sib tov 430 ntim ntawm tetrahydrofuran R thiab 570 ntim ntawm 1.36 g / l tov ntawm sodium acetate R hloov mus rau pH 4.8 nrog glacial acetic acid R.
Flow tus nqi 0.8 ml / min
Detection Spectrophotometer ntawm 250 nm.
Txhaj 20 µl voj injector;txhaj tshuaj ntsuam xyuas thiab cov kev daws teeb meem.
Lub sijhawm ua haujlwm 4 npaug ntawm lub sijhawm khaws cia ntawm Enoxolone.
System haum:
-kev daws teeb meem: yam tsawg kawg nkaus ntawm 2.0 ntawm lub ncov vim yog enoxolone thiab mus rau 18α-glycyrrhetinic acid nyob rau hauv lub chromatogram tau nrog siv tshuaj (c).
txwv:
-Txhua yam impurity: tsis pub ntau tshaj 7 npaug ntawm thaj tsam ntawm lub hauv paus ncov hauv chromatogram tau txais nrog kev siv tshuaj (b) (0.7 feem pua),
-tag nrho: tsis pub ntau tshaj qhov chaw ntawm lub hauv paus ncov nyob rau hauv lub chromatogram tau nrog kev siv tshuaj (a) (2.0 ib xees),
-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 ib xees).
Cov hlau hnyav (2.4.8) siab tshaj 20 ppm.
1.0 g ua raws li kev txwv kev xeem F. Npaj tus qauv siv 2 ml ntawm cov tshuaj txhuas txhuas (10 ppm Pb) R.
Poob ntawm ziab (2.2.32) Qhov siab tshaj plaws 0.5 feem pua, txiav txim siab ntawm 1.000 g los ntawm ziab hauv qhov cub ntawm 105 ℃ rau 4 h.
Sulfated tshauv (2.4.14) Qhov siab tshaj plaws 0.2 feem pua, txiav txim siab ntawm 1.0 g.
QHIA
Dissolve 0.330 g hauv 40 ml ntawm dimethylformamide R. Titrate nrog 0.1 M tetrabutylammonium hydroxide, txiav txim siab qhov kawg-point potentiometrically (2.2.20).Ua ib qho titration dawb paug.1 ml ntawm 0.1 M tetrabutylammonium hydroxide yog sib npaug rau 47.07 mg ntawm C30H46O4
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KHOOM
Tiv thaiv los ntawm lub teeb.
IMPURITIES
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