Ursodeoxycholic Acid (UDCA) CAS 128-13-2 Mayeso 99.0~101.0%

URSODEOXYCHOLIC ACID
Chithunzi cha C24H40O4 Chithunzi cha 392.6[128-13-2]
TANTHAUZO
3α,7β-Dihydroxy-5β-cholan-24-oic acid.
Zomwe zili: 99.0 peresenti mpaka 101.0 peresenti (zouma).
AKALE
Maonekedwe: ufa woyera kapena pafupifupi woyera.
Kusungunuka: pafupifupi kosasungunuka m'madzi, kusungunuka momasuka mu ethanol (96 peresenti), kusungunuka pang'ono mu acetone, pafupifupi osasungunuka mu methylene chloride.
mp: pafupifupi 202 ℃.
CHIZINDIKIRO
Chidziwitso choyamba: A.
Chizindikiritso Chachiwiri: B, C.
A. Infuraredi mayamwidwe spectrophotometry (2.2.24).
Kuyerekeza: Ursodeoxycholic Acid CRS.
B. Yang'anani ma chromatogram omwe adapezeka poyesa zonyansa C.
Zotsatira: malo ofunikira mu chromatogram yopezedwa ndi yankho loyesa (b) ndi ofanana ndi malo, mtundu ndi kukula kwa malo oyambira mu chromatogram yopezedwa ndi yankho lolozera (a).
C. Sungunulani pafupifupi 10 mg mu 1 mL ya sulfuric acid R. Onjezerani 0.1 mL ya yankho la formaldehyde R ndipo mulole kuyimirira kwa 5 min.Onjezani 5 ml ya madzi R. Kuyimitsidwa komwe kumapezeka ndi kobiriwira-buluu.
MAYESO
Kuzungulira kwapadera kwa kuwala (2.2.7): + 58.0 mpaka + 62.0 (zinthu zouma).
Sungunulani 0,500 g mu anhydrous ethanol R ndi kuchepetsa 25.0 mL ndi zosungunulira chomwecho.
Chidetso C. Thin-wosanjikiza chromatography (2.2.27).
Kusakaniza kosungunulira: madzi R, acetone R (10:90 V/V).
Njira yothetsera mayeso (a).Sungunulani 0,40 g wa zinthu kuti afufuzidwe mu zosungunulira osakaniza ndi kuchepetsa 10 mL ndi zosungunulira osakaniza.
Njira yothetsera mayeso (b).Sungunulani 1 ml ya njira yoyesera (a) mpaka 10 mL ndi zosungunulira zosakaniza.
Yankho lolozera (a).Sungunulani 40 mg wa ursodeoxycholic acid CRS mu zosungunulira zosakaniza ndi kuchepetsa 10 mL ndi zosungunulira osakaniza.
Yankho lolozera (b).Sungunulani 20 mg wa lithocholic acid CRS (zonyansa C) mu zosungunulira osakaniza ndi kuchepetsa 10.0 mL ndi zosungunulira osakaniza (njira A).Sungunulani 2.0 ml ya njira iyi ku 100.0 mL ndi zosungunulira zosakaniza.
Yankho lolozera (c).Pa 5 ml ya yankho A onjezerani 10 mg wa chenodeoxycholic acid CRS (zosayera A) ndi kusungunula mpaka 50 mL ndi zosungunulira zosakaniza.
Plate: TLC silika gel mbale R.
Gawo la mafoni: glacial acetic acid R, acetone R, methylenekloridi R ( 1:30:60 V/V/V).
Kugwiritsa ntchito: 5μL.
Kukula: kupitilira 2/3 ya mbale.
Kuyanika: pa 120 ℃ kwa 10 min.
Kuzindikira: ponyani nthawi yomweyo ndi yankho la 47.6 g/L la phosphomolybdic acid R mu osakaniza 1 voliyumu ya sulfuric acid R ndi voliyumu 20 ya glacial acetic acid R ndi kutentha pa 120 ℃ mpaka mawanga abuluu awonekere kumbuyo kopepuka.
Kuyenerera kwadongosolo: yankho lolozera (c):
- Chromatogram imawonetsa mawanga awiri olekanitsidwa bwino.
Malire: kuyesa njira (a):
-Kudetsedwa C: malo aliwonse chifukwa cha chidetso C sali ochuluka kuposa malo oyamba mu chromatogram yopezedwa ndi yankho lolozera (b) (0.1 peresenti).
Zogwirizana nazo.Chromatography yamadzimadzi (2.2.29).
Zosungunulira osakaniza: methanol R, mafoni gawo (10:90 V/V).
Njira yothetsera mayeso.Sungunulani 60 mg wa mankhwala kuti afufuzidwe mu zosungunulira osakaniza ndi kuchepetsa 20.0 mL ndi zosungunulira osakaniza.
Yankho lolozera (a).Sungunulani zomwe zili mu botolo la Ursodeoxycholic Acid kuti mugwirizane ndi CRS (yokhala ndi zonyansa A ndi H) mu 1.0 mL ya zosungunulira zosakaniza.
Yankho lolozera (b).Sungunulani 1.0 mL ya njira yothetsera 100.0 mL ndi zosungunulira zosakaniza.Sungunulani 1.0 mL ya njira iyi ku 10.0 mL ndi zosungunulira zosakaniza.
Mzere:
-kukula: l = 0,25 m, Ø = 4.6 mm;
-gawo loyima: gel octadecylsilyl silica gel omalizachromatography R (5 μm);
- Kutentha: 40 ℃ ± 1 ℃.
Gawo la mafoni: sakanizani ma voliyumu 30 a acetonitrile R, ma volume 37 a 0.78 g/L solution ya sodium dihydrogen phosphate R yosinthidwa kukhala pH 3 ndi phosphoric acid R, ndi ma voliyumu 40 a methanol R.
Kuthamanga: 0.8 mL / min.
Kuzindikira: refractometer pa 35 ± 1 ℃.
Jekeseni: 150 μL.
Nthawi yothamanga: nthawi 4 nthawi yosungira Ursodeoxycholic Acid.
Kuzindikiritsa zodetsedwa: gwiritsani ntchito chromatogram yoperekedwa ndi ursodeoxycholic acid kuti igwirizane ndi dongosolo la CRS ndi chromatogram yopezedwa ndi yankho lolozera (a) kuti muzindikire nsonga chifukwa cha zonyansa A ndi H.
Kusungidwa kwachibale ponena za ursodeoxycholic acid (nthawi yosungira = pafupifupi 14 min): zonyansa H = pafupifupi 0.9;chodetsedwa A = pafupifupi 2.8.
Kuyenerera kwadongosolo: yankho lolozera (a):
-kusamvana: osachepera 1.5 pakati pa nsonga chifukwa cha zonyansa H ndi ursodeoxycholic acid.
Malire:
- Kudetsedwa A: osapitirira ka 10 malo omwe ali pachimake chachikulu mu chromatogram yopezedwa ndi yankho lolozera (b) (1.0 peresenti);
-zodetsa zosadziwika: pachidetso chilichonse, chosaposa gawo la pachimake chachikulu mu chromatogram yopezedwa ndi yankho lachidziwitso (b) (0.10 peresenti);
- chiwopsezo: osapitilira ka 15 gawo la pachimake chachikulu mu chromatogram yomwe idapezedwa ndi yankho lolozera (b) (1.5 peresenti);
-kunyalanyaza malire: 0.5 nthawi za malo omwe ali pachimake chachikulu mu chromatogram yopezedwa ndi yankho lolozera (b) (0.05 peresenti).
Zitsulo zolemera (2.4.8): pazipita 20 ppm.
1.0 g imagwirizana ndi mayeso C. Konzani yankho lolozera pogwiritsa ntchito 2 mL ya lead standard solution (10 ppm Pb) R.
Kutaya pa kuyanika (2.2.32): pazipita 1.0 peresenti, anatsimikiza pa 1.000 ga kuyanika mu uvuni pa 105 ℃.
Phulusa la Sulfated (2.4.14): pazipita 0,1 peresenti, yotsimikizika pa 1.0 g.
ZOYESA
Sungunulani 0,350 g mu 50 mL wa Mowa (96 peresenti) R, kale neutralized kwa 0,2 mL wa phenolphthalein njira R. Onjezerani 50 mL madzi R ndi titrate ndi 0.1 M sodium hydroxide mpaka pinki mtundu analandira.
1 mL ya 0.1 M sodium hydroxide ndi yofanana ndi 39.26 mg ya C24H40O4.
ZOCHITSA
Zodetsedwa zotchulidwa: A, C.
Zonyansa zina zozindikirika (zinthu zotsatirazi, ngati zilipo pamlingo wokwanira, zitha kuzindikirika ndi mayeso amodzi kapena ena omwe ali mu monograph. Amachepetsedwa ndi mulingo wovomerezeka wa zonyansa zina/zosadziwika bwino ndi/kapena ndi zinthu zonse kuti agwiritse ntchito mankhwala (2034) Choncho sikoyenera kuzindikira zonyansazi kuti ziwonetsere kutsatiridwa.Onaninso 5.10.
Kuwongolera zonyansa muzinthu zogwiritsidwa ntchito ngati mankhwala): B, D, E, F, G, H, I.
A. 3α,7α-dihydroxy-5β-cholan-24-oic acid (chenodeoxycholic acid),
B. 3α, 7α, 12α-trihydroxy-5β-cholan-24-oic acid (cholic acid),
C. 3α-hydroxy-5β-cholan-24-oic acid (lithocholic acid),
D. 3α,7β,12α-trihydroxy-5β-cholan-24-oic acid (ursocholic acid),
E. 3α, 12α-dihydroxy-5β-cholan-24-oic acid (deoxycholic acid),
F. 3α-hydroxy-7-oxo-5β-cholan-24-oic acid,
G. methyl 3α,7β-dihydroxy-5β-cholan-24-oate,
H. 3β,7β-dihydroxy-5β-cholan-24-oic acid,
I. 5β-cholane-3α,7β,24-triol.