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

Zidziwitso Zonse
(ph Eur monograph 1511)
C30H46O4 470.7 471-53-4
Zochita ndi kugwiritsa ntchito
Chithandizo cha chosaopsa chironda chachikulu matenda.
Ph Eur
TANTHAUZO
(20β) -3β-Hydroxy-11-oxo-olean-12-en-29-oic acid.
Zamkatimu
98.0 peresenti mpaka 101.0 peresenti (zouma).
AKALE
Maonekedwe
White kapena pafupifupi woyera crystalline ufa.
Kusungunuka
Pafupifupi sungunuka m'madzi, sungunuka mu Mowa, sungunuka pang'ono mu methylene chloride.
Ikuwonetsa polymorphism (5.9).
CHIZINDIKIRO
Chidziwitso choyamba A.
Chizindikiritso chachiwiri B, C.
A. Unikani ndi infuraredi mayamwidwe spectrophotometry (2.2.24).
Kuyerekeza Enoxolone CRS.
Ngati mawonekedwe owoneka bwino olimba akuwonetsa kusiyana, sungunulani 0,2 g wa zinthu zomwe zikuyenera kufufuzidwa ndi 0,2 g wazinthu zofananira payokha mu 6 ml ya ethanol R. Wiritsani pansi.
reflux condenser kwa 1 h ndikuwonjezera 6 ml ya madzi R. A precipitate amapangidwa.Kuzizira mpaka 10 ℃ ndikusefa mothandizidwa ndi vacuum.Sambani madziwo ndi 10 ml ya mowa R, yowumitsani mu uvuni pa 80 ℃ ndikujambula mawonekedwe atsopano.
B. Thin-wosanjikiza chromatography (2.2.27).
Njira yoyesera Sungunulani 10 mg ya zinthu zomwe ziyenera kuyesedwa mu methylene chloride R ndi kusungunula mpaka 10 ml ndi zosungunulira zomwezo.
Sungunulani 10 mg wa enoxolone CRS mu methylene chloride R ndi kusungunula mpaka 10 ml ndi zosungunulira zomwezo.
Plate TLC silika gel mbale R.
Mobile gawo glacial acetic asidi R, acetone R, methylene kolorayidi R (5:10:90 V/V/V).
Ntchito 5µl.
Kupititsa patsogolo 2/3 ya mbale.
Kuyanika Mumlengalenga kwa 5 min.
Kuzindikira Utsi ndi anisaldehyde yankho R ndi kutentha pa 100-105 ℃ kwa 10 min.Zotsatira Malo ofunika kwambiri mu chromatogram yopezedwa ndi yankho la mayeso ndi ofanana m'malo, mtundu ndi kukula kwa malo oyambira mu chromatogram yopezedwa ndi mawu
yankho.
C. Sungunulani 50 mg mu 10 ml ya methylene chloride R. Kwa 2 ml ya yankho ili, onjezerani 1 ml ya acetic anhydride R ndi 0,3 ml ya sulfuric acid R. Mtundu wa pinki umapangidwa.
MAYESO
Mawonekedwe a yankho
Yankho lake ndi lomveka (2.2.1) komanso losawoneka bwino kwambiri kuposa yankho la Y6 (2.2.2, Method II).
Sungunulani 0,1 g mu Mowa R ndi kuchepetsa 10 ml ndi zosungunulira yemweyo.
Kuzungulira kwapadera kwa kuwala (2.2.7) + 145 mpaka + 154 (zinthu zouma).
Sungunulani 0,50 g mu dioxan R ndi kuchepetsa 50.0 ml ndi zosungunulira yemweyo.
Zogwirizana nazo
Chromatography yamadzimadzi (2.2.29).
Yankho loyesa Sungunulani 0,10 g ya chinthucho kuti chiwunikidwe mu gawo la mafoni ndikuchepetsa mpaka 100.0 ml ndi gawo la mafoni.
Yankho lolozera (a) Sungunulani 2.0 ml ya yankho la mayeso ku 100.0 ml ndi gawo la mafoni.
Njira yolozera (b) Sungunulani 5.0 ml ya yankho lolozera (a) mpaka 100.0 ml ndi gawo la mafoni.
Reference solution (c) Sungunulani 0.1 g wa 18α-glycyrrhetinic acid R mu tetrahydrofuran R ndi kuchepetsa ku 100.0 ml ndi zosungunulira zomwezo.Pa 2.0 ml ya yankho, onjezerani 2.0 ml ya yankho la mayeso ndikuchepetsa mpaka 100.0 ml ndi gawo la mafoni.
Mzere:
kukula: l = 0.25 m, Ø = 4.6 mm,
-gawo loyima: gel octadecylsilyl silica chromatography R (5 µm),
-kutentha: 30 ℃.
Mobile phase Mix 430 voliyumu ya tetrahydrofuran R ndi 570 voliyumu ya 1.36 g/l solution ya sodium acetate R yosinthidwa kukhala pH 4.8 ndi glacial acetic acid R.
Kuthamanga kwa 0.8 ml / min.
Kuzindikira Spectrophotometer pa 250 nm.
jakisoni 20 µl loop injector;jekeseni njira yothetsera mayesero ndi mayankho ofotokozera.
Nthawi yothamanga 4 nthawi yosungira Enoxolone.
Kuyenerera kwadongosolo:
-kutsimikiza: osachepera 2.0 pakati pa nsonga chifukwa cha enoxolone ndi 18α-glycyrrhetinic acid mu chromatogram yopezedwa ndi yankho lachidziwitso (c).
Malire:
-chidetso chilichonse: osapitilira ka 7 gawo la pachimake chachikulu mu chromatogram yopezedwa ndi yankho lolozera (b) (0.7 peresenti),
-chiwerengero: osaposa gawo lachimake chachikulu mu chromatogram yomwe idapezedwa ndi yankho (a) (2.0 peresenti),
-kunyalanyaza malire: 0.5 nthawi za nsonga yayikulu mu chromatogram yopezedwa ndi yankho lolozera (b) (0.05 peresenti).
Zitsulo zolemera (2.4.8) Zolemba malire 20 ppm.
1.0 g imagwirizana ndi mayeso a malire F. Konzani muyeso pogwiritsa ntchito 2 ml ya njira yokhazikika ya lead (10 ppm Pb) R.
Kutaya pakuyanika (2.2.32) Kuchuluka kwa 0.5 peresenti, kutsimikiziridwa pa 1.000 g mwa kuyanika mu uvuni pa 105 ℃ kwa 4 h.
Phulusa la Sulphated (2.4.14) Kuchuluka kwa 0.2 peresenti, kutsimikiziridwa pa 1.0 g.
ZOYESA
Sungunulani 0.330 g mu 40 ml ya dimethylformamide R. Titrate ndi 0.1 M tetrabutylammonium hydroxide, kudziwa mapeto a potentiometrically (2.2.20).Chitani mawu opanda kanthu.1 ml ya 0.1 M tetrabutylammonium hydroxide ndi ofanana ndi 47.07 mg wa C30H46O4
Korona Copyright 2006 330 46 4
KUSINTHA
Kutetezedwa ku kuwala.
ZOCHITSA
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