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

Gabaɗaya Sanarwa
(Ph Eur monograph 1511)
C30H46O4 470.7 471-53-4
Aiki da amfani
Maganin cutar gyambon ciki.
Ph Yuro
BAYANI
(20β) -3β-Hydroxy-11-oxo-olean-12-en-29-oic acid.
Abun ciki
Kashi 98.0 zuwa kashi 101.0 (bushewar abu).
HALAYE
Bayyanar
Fari ko kusan fari crystalline foda.
Solubility
A zahiri maras narkewa a cikin ruwa, mai narkewa a cikin ethanol, mai narkewa a cikin methylene chloride.
Yana nuna polymorphism (5.9).
GANO
Farkon ganewa A.
Na biyu ganewa B, C.
A. Bincika ta infrared absorption spectrophotometry (2.2.24).
Kwatanta Enoxolone CRS.
Idan bakan da aka samu a cikin ƙasa mai ƙarfi ya nuna bambance-bambance, narkar da 0.2 g na abubuwan da za a bincika da 0.2 g na abubuwan tunani daban a cikin 6 ml na ethanol R. Tafasa ƙarƙashin
reflux condenser na 1 h kuma ƙara 6 ml na ruwa R. An kafa hazo.Yi sanyi zuwa kusan 10 ℃ kuma tace tare da taimakon vacuum.A wanke hazo tare da 10 ml na barasa R, bushe a cikin tanda a 80 ℃ kuma yi rikodin sabon bakan.
B. chromatography na bakin ciki (2.2.27).
Maganin gwajin Narkar da MG 10 na abun da za a bincika a cikin methylene chloride R kuma a tsoma shi zuwa 10 ml tare da sauran ƙarfi iri ɗaya.
Maganin Magana Narke 10 MG na enoxolone CRS a cikin methylene chloride R kuma a tsarma zuwa 10 ml tare da sauran ƙarfi iri ɗaya.
Plate TLC silica gel farantin R.
Wayar hannu lokaci glacial acetic acid R, acetone R, methylene chloride R (5:10:90 V/V/V).
Aikace-aikace 5 µl.
Ci gaba Sama da 2/3 na farantin.
Bushewa A cikin iska na 5 min.
Gano Fesa tare da maganin anisaldehyde R da zafi a 100-105 ℃ na 10 min.Sakamako Babban tabo a cikin chromatogram da aka samu tare da maganin gwajin yayi kama da matsayi, launi da girma zuwa babban tabo a cikin chromatogram da aka samu tare da tunani.
mafita.
C. Narke 50 MG a cikin 10 ml na methylene chloride R. Zuwa 2 ml na wannan maganin, ƙara 1 ml na acetic anhydride R da 0.3 ml na sulfuric acid R. Ana samar da launin ruwan hoda.
GWAJI
Bayyanar mafita
Maganin a bayyane yake (2.2.1) kuma bai fi tsananin launi ba fiye da maganin tunani Y6 (2.2.2, Hanyar II).
Narke 0.1 g a cikin ethanol R kuma tsarma zuwa 10 ml tare da sauran ƙarfi iri ɗaya.
Takamaiman jujjuyawar gani (2.2.7) + 145 zuwa + 154 (bushewar abu).
Narke 0.50 g a cikin dioxan R kuma a tsarma zuwa 50.0 ml tare da sauran ƙarfi iri ɗaya.
Abubuwan da ke da alaƙa
Liquid chromatography (2.2.29).
Maganin gwaji Narkar da 0.10 g na abun da za a bincika a cikin tsarin wayar hannu kuma a tsoma shi zuwa 100.0 ml tare da lokacin wayar hannu.
Maganin Magana (a) Tsarma 2.0 ml na maganin gwajin zuwa 100.0 ml tare da lokacin wayar hannu.
Maganin Magana (b) Tsarma 5.0 ml na maganin tunani (a) zuwa 100.0 ml tare da lokacin wayar hannu.
Maganin Magana (c) Narke 0.1 g na 18a-glycyrrhetinic acid R a cikin tetrahydrofuran R kuma a tsarma zuwa 100.0 ml tare da sauran ƙarfi iri ɗaya.Zuwa 2.0 ml na maganin, ƙara 2.0 ml na maganin gwajin kuma tsarma zuwa 100.0 ml tare da lokacin wayar hannu.
Rukunin:
- girman: l = 0.25 m, Ø = 4.6 mm,
lokaci na tsaye: octadecylsilyl silica gel don chromatography R (5 µm),
- zazzabi: 30 ℃.
Lokacin wayar hannu Mix 430 juzu'i na tetrahydrofuran R da 570 juzu'i na 1.36 g/l bayani na sodium acetate R wanda aka daidaita zuwa pH 4.8 tare da glacial acetic acid R.
Yawan gudu 0.8 ml/min.
Gano Spectrophotometer a 250 nm.
Allurar madauki 20 µl injector;allurar maganin gwajin da hanyoyin magancewa.
Gudun lokaci sau 4 na lokacin riƙewa na Enoxolone.
Dacewar tsarin:
-ƙuduri: mafi ƙarancin 2.0 tsakanin kololuwa saboda enoxolone da zuwa 18a-glycyrrhetinic acid a cikin chromatogram da aka samu tare da bayani na tunani (c).
Iyaka:
-duk wani ƙazanta: bai fi sau 7 yanki na babban kololuwa a cikin chromatogram da aka samu tare da bayani na tunani (b) (0.7%).
- jimlar: bai wuce yankin babban kololuwa a cikin chromatogram da aka samu tare da bayani na tunani (a) (2.0 bisa dari),
- rashin kula da iyaka: 0.5 sau yanki na babban kololuwa a cikin chromatogram da aka samu tare da bayani na tunani (b) (0.05 bisa dari).
Karfe masu nauyi (2.4.8) Matsakaicin 20 ppm.
1.0 g ya bi gwajin iyaka F. Shirya ma'auni ta amfani da 2 ml na daidaitaccen maganin gubar (10 ppm Pb) R.
Asarar bushewa (2.2.32) Matsakaicin 0.5 bisa dari, ƙaddara akan 1.000 g ta bushewa a cikin tanda a 105 ℃ na 4 h.
Sulphated ash (2.4.14) Matsakaicin 0.2 bisa dari, an ƙaddara akan 1.0 g.
ASSAY
Narkar da 0.330 g a cikin 40 ml na dimethylformamide R. Titrate tare da 0.1 M tetrabutylammonium hydroxide, ƙayyade ƙarshen-ma'ana potentiometrically (2.2.20).Gudanar da titration mara kyau.1 ml na 0.1 m tetrabutylammonium hydroxide yayi daidai da 47.07 MG na C30H46O4
Haƙƙin mallaka na Crown 2006 330 46 4
AJIYA
An kare shi daga haske.
RASHIN ZUCIYA
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 Yuro