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

Panui Nui
(Ph Eur monograph 1511)
C30H46O4 470.7 471-53-4
Mahi me te whakamahi
Te maimoatanga o te mate whewhe peptic ngawari.
Ph Eur
WHAKAMAHI
(20β)-3β-Hydroxy-11-oxo-olean-12-en-29-oic acid.
Ihirangi
98.0 ōrau ki te 101.0 ōrau (matū maroke).
KAUPAPA
Te ahua
Te paura tioata ma, tata ma ranei.
Wairewa
Kare e rewa ki te wai, ka whakarewahia ki te waihano, he iti te whakarewa ki te methylene chloride.
E whakaatu ana i te polymorphism (5.9).
WHAKATAUTANGA
Ko te tohu tuatahi A.
Tautuhinga tuarua B, C.
A. Te tirotiro ma te infrared absorption spectrophotometry (2.2.24).
Whakatauritenga Enoxolone CRS.
Mēnā he rerekē te tūāwhiorangi i roto i te āhua mārō, memeha 0.2 g o te matū ka tirohia me te 0.2 g o te matū tohutoro motuhake ki te 6 ml o te waihā R. Kohuatia ki raro.
he whakapoauau mo te 1 haora ka tapirihia te 6 ml o te wai R. Ka puta he rerenga.Matao ki te 10 ℃ me te tātari me te korehau.Horoihia te waipara ki te 10 ml o te waipiro R, whakamaroke i roto i te oumu i te 80 ℃ me te tuhi i te hiranga hou.
B. Koromatography papa angiangi (2.2.27).
Wairewa whakamatautau Whakarewahia te 10 mg o te matū ka tirohia ki te methylene chloride R ka waimeha ki te 10 ml me te whakarewa ano.
Wairewa tohutoro Whakarewahia te 10 mg o te enoxolone CRS ki te methylene chloride R ka waimeha ki te 10 ml me te whakarewa ano.
Te pereti TLC pereti kirika kirika R.
Wāhanga pūkoro waikawa ahetiki huka R, acetone R, methylene pūhaumāota R (5:10:90 V/V/V).
Tono 5 µl.
Whanaketanga Neke atu i te 2/3 o te pereti.
Te whakamaroke I te hau mo te 5 min.
Mapuhia ki te wairewa anisaldehyde R me te wera i te 100-105 ℃ mo te 10 meneti.Hua Ko te waahi matua o te chromatogram i whiwhi me te otinga whakamatautau he rite te tuunga, te tae me te rahi ki te waahi matua o te chromatogram i whiwhi ma te tohutoro
otinga.
C. Whakarewahia te 50 mg ki te 10 ml o te methylene chloride R. Ki te 2 ml o tenei wairewa, taapirihia te 1 ml o te anhydride acetic R me te 0.3 ml o te waikawa pungatara R. Ka puta he tae mawhero.
WHAKAMAHI
Te ahua o te otinga
He maamaa te otinga (2.2.1) me te kore e kaha ake te tae i te otinga tohutoro Y6 (2.2.2, Tikanga II).
Whakarewahia te 0.1 g ki te waiwaro R ka waimeha ki te 10 ml me te whakarewa ano.
Te hurihanga whatu motuhake (2.2.7) + 145 ki + 154 (matū maroke).
Whakarewahia te 0.50 g ki te dioxan R ka waimeha ki te 50.0 ml me te whakarewa ano.
Matū whai pānga
Koromatography wai (2.2.29).
Te otinga whakamatautau Whakarewahia te 0.10 g o te matū ka tirotirohia i roto i te wahanga pūkoro ka waimeha ki te 100.0 ml me te wahanga pūkoro.
Wairewa tohutoro (a) Whakarihia te 2.0 ml o te wairewa whakamatautau ki te 100.0 ml me te wahanga pūkoro.
Wairewa tohutoro (b) Whakarihia te 5.0 ml o te wairewa tohutoro (a) ki te 100.0 ml me te wahanga pūkoro.
Wairewa tohutoro (c) Whakarewahia te 0.1 g o te waikawa 18α-glycyrrhetinic R i te tetrahydrofuran R ka waimeha ki te 100.0 ml me te whakarewa ano.Ki te 2.0 ml o te otinga, taapirihia te 2.0 ml o te otinga whakamatautau me te waimeha ki te 100.0 ml me te wahanga pūkoro.
Tīwae:
-rahi: l = 0.25 m, Ø = 4.6 mm,
-waahanga noho: octadecylsilyl silica gel mo te chromatography R (5 µm),
-mahana: 30 ℃.
Wāhanga pūkoro Whakaranuhia te 430 rōrahi tetrahydrofuran R me te 570 rōrahi o te wairewa 1.36 g/l o te konutai acetate R kua whakaritea ki te pH 4.8 me te waikawa ahetiki huka R.
Rere rere 0.8 ml/min.
Irirangi Tirohanga i te 250 nm.
Werohanga 20 µl injector koropiko;werohia te otinga whakamatautau me nga otinga tohutoro.
Te wa oma 4 nga wa te wa pupuri o Enoxolone.
Te pai o te punaha:
-taumira: te iti rawa o te 2.0 i waenga i nga tihi na te enoxolone me te waikawa 18α-glycyrrhetinic i roto i te chromatogram i whiwhi me te otinga tohutoro (c).
Tepe:
-tetahi poke: kaua e neke ake i te 7 whakareatanga te horahanga o te tihi matua o te chromatogram i whiwhi ki te otinga tohutoro (b) (0.7 paiheneti),
-tapeke: kaua e neke ake i te horahanga o te tihi matua o te chromatogram i whiwhi ki te otinga tohutoro (a) (2.0 paiheneti),
-whakarerea tepe: 0.5 whakarea te horahanga o te tihi matua o te chromatogram i whiwhi ki te otinga tohutoro (b) (0.05 paiheneti).
Nga konganuku taumaha (2.4.8) Morahi 20 ppm.
1.0 g e tutuki ana ki te whakamatautau tepe F. Whakaritea te paerewa ma te whakamahi i te 2 ml o te wairewa paerewa mata (10 ppm Pb) R.
Ngaronga i runga i te whakamaroke (2.2.32) Morahi 0.5 paiheneti, ka whakatauhia ki te 1.000 g ma te whakamaroke i roto i te oumu i te 105 ℃ mo te 4 haora.
Te pungarehu ngongo (2.4.14) Morahi 0.2 paiheneti, kua whakatauhia ki te 1.0 g.
WHAKAMAHI
Whakarewahia te 0.330 g ki te 40 ml o te dimethylformamide R. Titrate ki te 0.1 M tetrabutylammonium hydroxide, te whakatau i te pito-mutunga potentiometrically (2.2.20).Whakahaerehia he titration patea.1 ml o te 0.1 M tetrabutylammonium hydroxide he rite ki te 47.07 mg o C30H46O4
Mana pupuri Karauna 2006 330 46 4
PUTANGA
Ka parea i te marama.
NGA POKE
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