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

Izaziso ngokubanzi
(Ph Eur monograph 1511)
C30H46O4 470.7 471-53-4
Isenzo kunye nokusetyenziswa
Unyango lwesifo se-benign peptic ulcer.
Ph Eur
INGCACISO
(20β) -3β-Hydroxy-11-oxo-olean-12-en-29-oic acid.
Umxholo
98.0 ekhulwini ukuya kwi-101.0 yeepesenti (into eyomileyo).
ABAlinganiswa
Imbonakalo
Umgubo omhlophe okanye ophantse umhlophe wekristale.
Ukunyibilika
Ayinyibiliki kakhulu emanzini, inyibilika kwi-ethanol, inyibilika kancinci kwi-methylene chloride.
Ibonisa i-polymorphism (5.9).
UKUCHAZA
Isazisi sokuqala A.
Isazisi sesibini B, C.
A. Jonga nge-infrared absorption spectrophotometry (2.2.24).
Uthelekiso Enoxolone CRS.
Ukuba i-spectra efunyenwe kwisimo esiqinileyo ibonisa umahluko, nyibilikisa i-0.2 g yezinto eziza kuhlolwa kunye ne-0.2 g ye-reference substance ngokwahlukileyo kwi-6 ml ye-ethanol R. Bilisa ngaphantsi
i-reflux condenser ye-1 h kwaye yongeza i-6 ml yamanzi R. I-precipitate yenziwe.Ukuphola ukuya malunga ne-10℃ kwaye hluza ngoncedo lwevacuum.Geza i-precipitate nge-10 ml yotywala R, yomise kwi-oven kwi-80 ℃ kwaye urekhode i-spectra entsha.
B. I-chromatography ye-Thin-layer (2.2.27).
Isisombululo sovavanyo Dissolve i-10 mg yezinto eziza kuhlolwa kwi-methylene chloride R kwaye udibanise kwi-10 ml kunye ne-solvent efanayo.
Isisombululo sereferensi Nciba i-10 mg ye-enoxolone CRS kwi-methylene chloride R kwaye udibanise kwi-10 ml kunye ne-solvent efanayo.
Ipleyiti ye-TLC ye-silica gel plate R.
Isigaba seselula se-glacial acetic acid R, i-acetone R, i-methylene chloride R (5:10:90 V/V/V).
Usetyenziso 5 µl.
Uphuhliso Ngaphezu kwe-2/3 yepleyiti.
Ukomisa emoyeni kwi-5 min.
Ukufumanisa Ukutshiza ngesisombululo se-anisaldehyde R kunye nobushushu kwi-100-105 ℃ kwi-10 min.Iziphumo Indawo ephambili kwichromatogram efunyenwe ngesisombululo sovavanyo iyafana kwindawo, umbala kunye nobukhulu kwindawo ephambili kwichromatogram efunyenwe ngereferensi.
isisombululo.
C. Dissolve 50 mg kwi-10 ml ye-methylene chloride R. Kwi-2 ml yesi sisombululo, yongeza i-1 ml ye-acetic anhydride R kunye ne-0.3 ml ye-sulfuric acid R. Umbala opinki uveliswa.
UVAVANYO
Ukubonakala kwesisombululo
Isisombululo sicacile (2.2.1) kwaye singabi nombala ogqithiseleyo kunesisombululo sereferensi ye-Y6 (2.2.2, i-Method II).
Dissolve 0.1 g kwi-ethanol R kwaye udibanise kwi-10 ml kunye ne-solvent efanayo.
Ukujikeleza okucacileyo kwe-optical (2.2.7) + 145 ukuya + 154 (into eyomileyo).
Dissolve 0.50 g kwi-dioxan R kwaye udibanise kwi-50.0 ml kunye ne-solvent efanayo.
Izinto ezinxulumeneyo
Ichromatography yolwelo (2.2.29).
Isisombululo sovavanyo Chitha i-0.10 g yezinto eziza kuhlolwa kwisigaba esihambahambayo kwaye udibanise kwi-100.0 ml kunye nesigaba esihambayo.
Isisombululo sereferensi (a) Nciphisa i-2.0 ml yesisombululo sovavanyo kwi-100.0 ml kunye nesigaba esihambayo.
Isisombululo sereferensi (b) Nciphisa i-5.0 ml yesisombululo sereferensi (a) ukuya kwi-100.0 ml kunye nesigaba esihambayo.
Isisombululo sereferensi (c) Dissolve 0.1 g ye-18α-glycyrrhetinic acid R kwi-tetrahydrofuran R kwaye udibanise kwi-100.0 ml kunye ne-solvent efanayo.Kwi-2.0 ml yesisombululo, yongeza i-2.0 ml yesisombululo sovavanyo kwaye uhlambulule kwi-100.0 ml kunye nesigaba seselula.
Uluhlu:
-ubungakanani: l = 0.25 m, Ø = 4.6 mm,
-isigaba sokumisa: i-octadecylsilyl silica gel yechromatography R (5 µm),
-ubushushu: 30℃.
Isigaba seselula Xuba imiqulu ye-430 ye-tetrahydrofuran R kunye ne-570 imiqulu ye-1.36 g / l isisombululo se-sodium acetate R elungiswe kwi-pH 4.8 kunye ne-glacial acetic acid R.
Isantya sokuhamba 0.8 ml / min.
Ukufunyanwa kweSpectrophotometer kwi-250 nm.
Isitofu ngama-20 µl isitofu selophu;tofa isisombululo sovavanyo kunye nezisombululo zereferensi.
Ixesha lokubaleka 4 ixesha lokugcinwa kuka Enoxolone.
Ukufaneleka kwenkqubo:
-isisombululo: ubuncinane be-2.0 phakathi kweencopho ngenxa ye-enoxolone kunye ne-18α-glycyrrhetinic acid kwi-chromatogram efunyenwe ngesisombululo sereferensi (c).
Imida:
-nakuphi na ukungcola: akukho ngaphezu kwexesha le-7 indawo yenqununu yenqununu kwi-chromatogram efunyenwe ngesisombululo sokubhekisela (b) (ipesenti ze-0.7),
-itotali: hayi ngaphezu kwendawo yencopho eyintloko kwichromatogram efunyenwe ngesisombululo sereferensi (a) (2.0 pesenti),
-ukungahoyi umda: amaxesha e-0.5 indawo yenqununu yenqununu kwi-chromatogram efunyenwe ngesisombululo sokubhekisela (b) (ipesenti ze-0.05).
Iintsimbi ezinzima (2.4.8) Ubuninzi be-20 ppm.
I-1.0 g ihambelana novavanyo lomda F. Lungiselela umgangatho usebenzisa i-2 ml yesisombululo esiqhelekileyo se-lead (10 ppm Pb) R.
Ilahleko ekomisweni (2.2.32) Ubuninzi beepesenti ze-0.5, kunqunywe kwi-1.000 g ngokumisa kwi-oven kwi-105 ℃ nge-4 h.
Uthuthu lwe-Sulphated (2.4.14) Ubuninzi beepesenti ze-0.2, bunqunywe kwi-1.0 g.
UVAVANYO
Dissolve 0.330 g kwi-40 ml ye-dimethylformamide R. I-Titrate kunye ne-0.1 M tetrabutylammonium hydroxide, ukugqiba i-potent-point point (2.2.20).Yenza ititration engenanto.I-1 ml ye-0.1 M tetrabutylammonium hydroxide ilingana ne-47.07 mg ye-C30H46O4
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UKUGCINA
Ikhuselwe ekukhanyeni.
UBUNGCOLA
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