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

Izaziso Ezijwayelekile
(i-Ph Eur monograph 1511)
C30H46O4 470.7 471-53-4
Isenzo nokusetshenziswa
Ukwelashwa kwesifo se-benign peptic ulcer.
Ph Eur
INCAZELO
(20β)-3β-Hydroxy-11-oxo-olean-12-en-29-oic acid.
Okuqukethwe
98.0% ukuya ku-101.0% (into eyomisiwe).
ABALINGISI
Ukubukeka
Impushana emhlophe emhlophe noma ecishe ibe mhlophe.
Ukuncibilika
Ayincibiliki emanzini, incibilika ku-ethanol, incibilika kancane ku-methylene chloride.
Ibonisa i-polymorphism (5.9).
UKUKHOMBA
Umazisi wokuqala u-A.
Umazisi wesibili B, C.
A. Hlola nge-infrared absorption spectrophotometry (2.2.24).
Ukuqhathanisa Enoxolone CRS.
Uma i-spectra etholwe esimweni esiqinile sibonisa umehluko, ncibilikisa u-0.2 g wento ezohlolwa kanye no-0.2 g wento eyisethenjwa ngokuhlukana ku-6 ml we-ethanol R. Bilisa ngaphansi
i-condenser ye-reflux ye-1 h bese wengeza u-6 ml wamanzi R. I-precipitate yenziwa.Kuphole ku-10℃ bese uhlunga ngosizo lwe-vacuum.Geza imvula ngo-10 ml wotshwala R, womise kuhhavini ongu-80℃ bese urekhoda isibuko esisha.
B. I-chromatography yongqimba oluncane (2.2.27).
Isixazululo sokuhlola Chaza u-10 mg wento ezohlolwa ku-methylene chloride R bese unciphisa ibe ngu-10 ml nge-solvent efanayo.
Isixazululo sereferensi Chaza u-10 mg we-enoxolone CRS ku-methylene chloride R bese unciphisa ku-10 ml nge-solvent efanayo.
Ipuleti le-TLC silica gel plate R.
Isigaba seselula i-glacial acetic acid R, i-acetone R, i-methylene chloride R (5:10:90 V/V/V).
Uhlelo lokusebenza 5 µl.
Ukuthuthukiswa Ngaphezulu kwe-2/3 yepuleti.
Ukomisa Emoyeni imizuzu emi-5.
Ukuthola Futha ngesisombululo se-anisaldehyde R bese ushisa ku-100-105℃ imizuzu eyi-10.Imiphumela Indawo eyinhloko kuchromatogram etholwe ngesixazululo sokuhlola iyafana ngesimo, umbala nosayizi nendawo eyinhloko kuchromatogram etholwe nereferensi.
isisombululo.
C. Chaza u-50 mg ku-10 ml we-methylene chloride R. Ku-2 ml walesi sixazululo, engeza u-1 ml we-acetic anhydride R kanye no-0.3 ml we-sulfuric acid R. Umbala ophinki uyakhiqizwa.
IZIVIVINYO
Ukubukeka kwesixazululo
Isixazululo sicacile (2.2.1) futhi asinawo umbala ogqamile kunesixazululo sereferensi Y6 (2.2.2, Indlela II).
Chaza u-0.1 g ku-ethanol R bese unciphisa ku-10 ml nge-solvent efanayo.
Ukujikeleza okuqondile kwe-optical (2.2.7) + 145 kuya ku- + 154 (into eyomile).
Chaza u-0.50 g ku-dioxan R bese unciphisa ku-50.0 ml nge-solvent efanayo.
Izinto ezihlobene
I-chromatography yoketshezi (2.2.29).
Isixazululo sokuhlola Chaza u-0.10 g wento ezohlolwa esigabeni esihambayo bese unciphisa ibe ngu-100.0 ml ngesigaba seselula.
Isixazululo sereferensi (a) Nciphisa u-2.0 ml wesixazululo sokuhlola sibe ngu-100.0 ml ngesigaba esihambayo.
Isixazululo sereferensi (b) Nciphisa u-5.0 ml wesixazululo sereferensi (a) sibe ngu-100.0 ml ngesigaba esihambayo.
Isixazululo sereferensi (c) Chaza u-0.1 g we-18α-glycyrrhetinic acid R ku-tetrahydrofuran R bese unciphisa ku-100.0 ml nge-solvent efanayo.Ku-2.0 ml wesisombululo, engeza u-2.0 ml wesisombululo sokuhlola bese unciphisa ku-100.0 ml ngesigaba seselula.
Ikholomu:
-usayizi: l = 0.25 m, Ø = 4.6 mm,
-isigaba sokuma: ijeli ye-silica ye-octadecylsilyl ye-chromatography R (5 µm),
- izinga lokushisa: 30 ℃.
Isigaba seselula Hlanganisa amavolumu angu-430 we-tetrahydrofuran R kanye namavolumu angu-570 wesisombululo esingu-1.36 g/l se-sodium acetate R elungiswe ku-pH 4.8 nge-glacial acetic acid R.
Izinga lokugeleza 0.8 ml/min.
I-Detection Spectrophotometer ku-250 nm.
Umjovo 20 µl loop injector;faka isisombululo sokuhlola kanye nezixazululo zereferensi.
Isikhathi sokugijima izikhathi ezi-4 kunesikhathi sokugcina sika-Enoxolone.
Ukufaneleka kwesistimu:
-ukulungiswa: ubuncane obungu-2.0 phakathi kweziqongo ngenxa ye-enoxolone kanye no-18α-glycyrrhetinic acid kuchromatogram etholwe ngesisombululo sereferensi (c).
Imikhawulo:
-noma yikuphi ukungcola: hhayi izikhathi ezingaphezu kwezingu-7 endaweni yokuphakama okuyinhloko ku-chromatogram etholwe ngesisombululo sereferensi (b) (amaphesenti angu-0.7),
-ingqikithi: hhayi ngaphezu kwendawo yenani eliphakeme eliyinhloko kuchromatogram etholwe ngesixazululo sereferensi (a) (2.0 per cent),
-umkhawulo wokunganaki: izikhathi ezingu-0.5 indawo yokuphakama okuyinhloko ku-chromatogram etholwe ngesixazululo sereferensi (b) (amaphesenti angu-0.05).
Izinsimbi ezinzima (2.4.8) Ubukhulu obungu-20 ppm.
1.0 g ithobelana nokuhlolwa komkhawulo F. Lungiselela indinganiso usebenzisa u-2 ml wesisombululo esijwayelekile somthofu (10 ppm Pb) R.
Ukulahlekelwa ekomisweni (2.2.32) Ubukhulu obungamaphesenti angu-0.5, obunqunywa ku-1.000 g ngokomiswa kuhhavini ongu-105℃ amahora angu-4.
Umlotha one-sulphated (2.4.14) Ubukhulu obungamaphesenti angu-0.2, bunqunywe ku-1.0 g.
ISIVIVINYO
Chaza u-0.330 g ku-40 ml we-dimethylformamide R. Titrate nge-0.1 M tetrabutylammonium hydroxide, enquma iphuzu lokugcina potentiometrically (2.2.20).Yenza ititration engenalutho.I-1 ml ye-0.1 M tetrabutylammonium hydroxide ilingana no-47.07 mg we-C30H46O4
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ISITOREJI
Ivikelwe ekukhanyeni.
UKUNGCOLA
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