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

Ogeysiisyada Guud
(Ph Eur monograph 1511)
C30H46O4 470.7 471-53-4
Ficil iyo isticmaal
Daawaynta cudurka boogaha ba'an.
Ph Euro
Qeexitaan
(20β) -3β-Hydroxy-11-oxo-olean-12-en-29-oic acid.
Nuxurka
98.0 boqolkiiba ilaa 101.0 boqolkiiba (walaxda qalalan).
MEESHA
Muuqashada
Caddaan ama ku dhawaad ​​cad budo crystalline.
Solubility
Dhab ahaantii aan biyo ku milmin, ku milmin ethanol, si yar ugu milmi kara methylene chloride.
Waxay muujinaysaa polymorphism (5.9).
AQOONSIGA
Aqoonsiga koowaad A.
Aqoonsiga labaad B, C.
A. Ku baadh nuugista infrared spectrophotometry (2.2.24).
Isbarbardhigga Enoxolone CRS.
Haddii spectra ee laga helay gobolka adag ay muujiyaan kala duwanaansho, milaan 0.2 g walaxda la baaro iyo 0.2 g oo ah walaxda tixraaca si gooni gooni ah 6 ml ethanol R. Karkari hoos
qaboojiyaha reflux muddo 1 saac ah kuna dar 6 ml oo biyo ah R. Da'da ayaa la sameeyay.Qabooji ilaa 10 ℃ oo ku shaandhee adigoo isticmaalaya faakuum.Ku dhaq daadad soo daadatay 10 ml oo aalkolo ah, ku qallaji foornada 80℃ oo qor muuqaal cusub.
B. chromatography oo khafiif ah (2.2.27).
Xalka tijaabada Ku mil 10 mg oo walax ah oo lagu baaro methylene chloride R oo ku mil 10 ml oo isku mid ah dareere.
Xalka tixraaca Ku mil 10 mg ee enoxolone CRS ee methylene chloride R oo ku mil 10 ml oo leh dareere isku mid ah.
Plate TLC silica jel saxan R.
Marxaladda wareega ee glacial acetic acid R, acetone R, methylene chloride R (5:10:90 V/V/V).
Codsiga 5 µl.
Horumarinta In ka badan 2/3 ee saxanka.
Ku qallajinta hawada 5 daqiiqo.
Ogaanshaha ku buufi xal anisaldehyde R oo kuleyl 100-105℃ 10 daqiiqo.Natiijooyinka Meesha ugu muhiimsan ee chromatogram-ka ee lagu helay xalka tijaabada waxay la mid tahay booska, midabka iyo cabbirka meesha ugu muhiimsan ee chromatogram-ka laga helay tixraaca.
xal.
C. Ku milmo 50 mg 10 ml methylene chloride R. Ilaa 2 ml ee xalkan, ku dar 1 ml oo acetic anhydride R ah iyo 0.3 ml sulfuric acid R. Midab casaan ah ayaa la soo saaray.
IMTIXAANKA
Muuqashada xalka
Xalku waa cad yahay (2.2.1) oo aan ka midab badan ahayn xalka tixraaca Y6 (2.2.2, Habka II).
Ku mil 0.1 g ethanol R oo ku mil 10 ml oo isku mid ah dareere.
Wareegga indhaha ee gaarka ah (2.2.7) + 145 ilaa + 154 (walxaha qallalan).
Ku mil 0.50 g dioxan R oo ku mil 50.0 ml oo isku mid ah dareere.
Walxaha la xidhiidha
chromatography dareere ah (2.2.29).
Xalka tijaabada Mila 0.10 g oo ah walaxda lagu baaro wareega wareega oo ku mil 100.0 ml wajiga mobaylka.
Xalka tixraaca (a) Ku mil 2.0 ml ee xalka tijaabada ilaa 100.0 ml wajiga wareega.
Xalka tixraaca (b) Ku mil 5.0 ml oo xal tixraac ah (a) ilaa 100.0 ml wajiga wareega
Xalka tixraaca (c) Ku mil 0.1 g oo ah 18a-glycyrrhetinic acid R ee tetrahydrofuran R oo ku milo 100.0 ml oo leh dareere isku mid ah.Ku dar 2.0 ml oo ah xalka, ku dar 2.0 ml ee xalka tijaabada oo ku milo 100.0 ml oo leh wajiga wareega.
Tiirka:
-xajmiga: l = 0.25 m, Ø = 4.6 mm,
Marxaladda taagan: octadecylsilyl silica gel for chromatography R (5 µm),
- heerkulka: 30 ℃.
Wajiga moobilka Isku qas 430 mugga tetrahydrofuran R iyo 570 mugga 1.36 g/l ee sodium acetate R oo lagu hagaajiyay pH 4.8 oo leh glacial acetic acid R.
Heerka socodka 0.8 ml/min.
Xakamaynta Spectrophotometer ee 250 nm.
Mudista 20 µl loop;duraa xalalka tijaabada iyo xalalka tixraaca.
Wakhtiga wad 4 jeer wakhtiga haynta Enoxolone.
Ku habboonaanta nidaamka:
-xarka: ugu yaraan 2.0 inta u dhaxaysa meelaha ugu sarreeya sababtoo ah enoxolone iyo ilaa 18a-glycyrrhetinic acid ee chromatogram-ka ee lagu helay xal tixraaceed (c).
Xaddid:
wasakh kasta: aan ka badnayn 7 jeer meesha ugu sarraysa ee chromatogram-ka ee lagu helay xal tixraaceed (b) (0.7 boqolkiiba),
-wadarta: aan ka badnayn aagga ugu sarreeya ee chromatogram-ka ee lagu helay xal tixraaceed (a) (2.0 boqolkiiba),
Xadid la'aanta: 0.5 jeer bedka ugu sarreeya ee chromatogram-ka ee lagu helay xal tixraaceed (b) (0.05 boqolkiiba).
Biraha culus (2.4.8) Ugu badnaan 20 ppm.
1.0 g ayaa u hogaansama tijaabada xadka F. U diyaari heerka adigoo isticmaalaya 2 ml oo ah xalalka sunta rasaasta (10ppm Pb) R.
Luminta qalajinta (2.2.32) Ugu badnaan 0.5 boqolkiiba, waxaa lagu go'aamiyay 1.000 g iyadoo lagu qallajinayo foornada 105 ℃ 4 saac.
Dambaska sulfateed (2.4.14) Ugu badnaan 0.2 boqolkiiba, oo lagu go'aamiyay 1.0 g.
ASSAY
Ku milmi 0.330 g ee 40 ml dimethylformamide R. Titrate leh 0.1 M tetrabutylammonium hydroxide, go'aaminta barta-dhamaadka ee awood ahaan (2.2.20).Samee titration maran.1 ml oo ah 0.1 m tetrabutylammonium hydroxide waxay u dhigantaa 47.07 mg ee C30H46O4
Xuquuqda daabacaadda Crown 2006 330 46 4
KAYDINTA
Ilays laga ilaaliyo.
XANUUNKA
A. (20β) -3β-hydroxy-11-oxo-18a-olean-12-en-29-oic acid,
B. (4β,20β) -3β,23-dihydroxy-11-oxo-olean-12-en-29-oic acid.
Ph Euro