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

Ọkwa n'ozuzu
(Ph Eur monograph 1511)
C30H46O4 470.7 471-53-4
Action na ojiji
Ọgwụgwọ ọrịa ọnyá afọ peptic.
Ph Euro
Nkọwa
(20β) -3β-Hydroxy-11-oxo-olean-12-en-29-oic acid.
Ọdịnaya
98.0 pasent ruo 101.0 pasent (ihe akpọnwụwo).
ÀMÀ
Ọdịdị
Ọcha ma ọ bụ ọ fọrọ nke nta ka ọ bụrụ ntụ ntụ crystalline ọcha.
Solubility
Ihe na-adịghị ahụkebe n'ime mmiri, soluble na ethanol, na-agbaze obere na methylene chloride.
Ọ na-egosi polymorphism (5.9).
Nchọpụta
njirimara mbụ A.
Nchọpụta nke abụọ B, C.
A. Nyochaa site na infrared absorption spectrophotometry (2.2.24).
Tụnyere Enoxolone CRS.
Ọ bụrụ na ụdịdị dị iche iche enwetara na steeti siri ike na-egosi ọdịiche, gbarie 0.2 g nke ihe a ga-enyocha yana 0.2 g nke ihe ntụaka dị iche na 6 ml nke ethanol R. Obụpde n'okpuru.
a reflux condenser maka 1 h ma tinye 6 ml nke mmiri R. A na-akpụ akpụ.Jụụ ruo ihe dị ka 10 ℃ ma jiri enyemaka nke oghere na-enyocha ya.Jiri 10 ml mmanya R na-asa mmiri ahụ, kpochaa na oven na 80 ℃ ma dekọọ ụdị ọhụrụ.
B. chromatography nke dị obere (2.2.27).
Ngwọta ule gbazee 10 mg nke ihe a ga-enyocha na methylene chloride R wee jiri otu ihe mgbaze mee ka ọ bụrụ 10 ml.
Ngwọta ntụaka gbazee 10 mg nke enoxolone CRS na methylene chloride R wee gbasaa na 10 ml na otu ihe mgbaze.
Plate TLC silica gel plate R.
Akụkụ mkpanaka glacial acetic acid R, acetone R, methylene chloride R (5:10:90 V/V/V).
Ngwa 5 µl.
Mmepe Karịrị 2/3 nke efere.
Ịkpọ nkụ na ikuku maka 5 min.
Nchọpụta fesa na anisaldehyde ngwọta R na okpomọkụ na 100-105 ℃ maka 10 min.Nsonaazụ Ebe bụ isi na chromatogram nke enwetara na ngwọta nnwale yiri n'ọnọdụ, agba na nha ya na ebe bụ isi na chromatogram enwetara na ntụaka.
ngwọta.
C. Gbari 50 mg na 10 ml nke methylene chloride R. Na 2 ml nke ngwọta a, tinye 1 ml acetic anhydride R na 0.3 ml nke sulfuric acid R. A na-emepụta agba pink.
Nnwale
Ọdịdị nke ngwọta
Ihe ngwọta doro anya (2.2.1) na ọ bụghị karịa agba agba karịa ntụaka ngwọta Y6 (2.2.2, Method II).
Gbari 0.1 g na ethanol R wee gbasaa na 10 ml na otu ihe mgbaze.
Ntụgharị anya pụrụ iche (2.2.7) + 145 ruo + 154 (ihe akpọnwụwo).
Gbari 0.50 g na dioxan R wee gbasaa na 50.0 ml na otu ihe mgbaze.
Ihe ndị metụtara ya
chromatography nke mmiri mmiri (2.2.29).
Ngwọta ule gbazee 0.10 g nke ihe a ga-enyocha na usoro mkpanaka wee gbanye 100.0 ml na usoro mkpanaka.
Ngwọta ntụaka (a) Jiri usoro mkpanaka gbanye 2.0 ml nke ngwọta nnwale na 100.0 ml.
Ngwọta ntụaka (b) Jiri usoro mkpanaka gbanye 5.0 ml nke ihe ntụaka (a) ruo 100.0 ml.
Ngwọta ntụaka (c) Gbarie 0.1 g nke 18α-glycyrrhetinic acid R na tetrahydrofuran R wee gbasaa na 100.0 ml na otu ihe mgbaze.Na 2.0 ml nke ngwọta, gbakwunye 2.0 ml nke ngwọta ule ma gbanye 100.0 ml na usoro mkpanaka.
Ogidi:
- nha: l = 0.25 m, Ø = 4.6 mm,
- nkeji oge: octadecylsilyl silica gel maka chromatography R (5 µm),
- okpomọkụ: 30 ℃.
Ngwa mkpanaka Ngwakọta mpịakọta 430 nke tetrahydrofuran R na mpịakọta 570 nke ngwọta 1.36 g / l nke sodium acetate R gbanwere pH 4.8 na glacial acetic acid R.
Ọnụego 0.8 ml / min.
Nchọpụta Spectrophotometer na 250 nm.
Injector loop nke 20 µl;gbanye ngwọta ule na ntụnye aka.
Gbaa oge 4 ugboro oge njigide nke Enoxolone.
Kwesịrị ekwesị sistemụ:
-mkpebi: opekempe nke 2.0 n'etiti ọnụ ọgụgụ kasị elu n'ihi enoxolone na 18a-glycyrrhetinic acid na chromatogram nwetara na ntụ ntụ ntụ ntụ (c).
Oke:
-adịghị ọcha ọ bụla: ọ bụghị ihe karịrị ugboro 7 mpaghara nke isi kacha elu na chromatogram nwetara site na ngwọta ntụaka (b) (0.7%).
-mkpokọta: ọ bụghị karịa mpaghara nke isi kacha elu na chromatogram nwetara site na ntụnye ntụaka (a) (2.0%)
-nleghara oke: 0,5 ugboro mpaghara nke isi elu na chromatogram nwetara na ntụaka ngwọta (b) (0.05 pasent).
Ọla dị arọ (2.4.8) Kachasị 20 ppm.
1.0 g na-akwado ule oke F. Kwadebe ọkọlọtọ site na iji 2 ml nke ngwọta ọkọlọtọ ụzọ (10ppm Pb) R.
Ọnwụ na ihicha (2.2.32) kacha 0.5 pasent, kpebisiri ike na 1.000 g site na ihicha na oven na 105 ℃ maka 4 h.
Sulfated ash (2.4.14) Kachasị 0.2 pasent, kpebisiri ike na 1.0 g.
ASSAY
Gbari 0.330 g na 40 ml nke dimethylformamide R. Titrate na 0.1 M tetrabutylammonium hydroxide, na-ekpebi njedebe njedebe nke ike (2.2.20).Mepụta titration efu.1 ml nke 0.1 m tetrabutylammonium hydroxide bụ 47.07 mg nke C30H46O4.
Okpueze nwebiisinka 2006 330 46 4
Nchekwa
Echebere na ìhè.
IHE adịghị ọcha
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