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

Abubuwan da aka bayar na URSODEOXYCHOLIC
C24H40O4 Mr 392.6[128-13-2]
BAYANI
3α,7β-Dihydroxy-5β-cholan-24-oic acid.
Abun ciki: 99.0 bisa dari zuwa 101.0 bisa dari (bushewar abu).
HALAYE
Bayyanar: fari ko kusan fari foda.
Solubility: kusan wanda ba a iya narkewa a cikin ruwa, mai narkewa cikin yardar kaina a cikin ethanol (kashi 96), mai narkewa kaɗan a cikin acetone, kusan maras narkewa a cikin methylene chloride.
mp: kusan 202 ℃.
GANO
Alamar farko: A.
Na biyu ganewa: B, C.
A. Infrared spectrophotometry (2.2.24).
Kwatanta: Ursodeoxycholic Acid CRS.
B. Bincika chromatograms da aka samu a gwaji don rashin tsarki C.
Sakamako: babban tabo a cikin chromatogram da aka samu tare da maganin gwaji (b) yayi kama da matsayi, launi da girma zuwa babban tabo a cikin chromatogram da aka samu tare da bayani na tunani (a).
C. Narke game da 10 MG a cikin 1 ml na sulfuric acid R. Ƙara 0.1 ml na formaldehyde bayani R kuma ba da damar tsayawa na 5 min.Ƙara 5 ml na ruwa R. Dakatar da aka samu shine kore-shuɗi.
GWAJI
Takamaiman jujjuyawar gani (2.2.7): + 58.0 zuwa + 62.0 (bushewar abu).
Narkar da 0.500 g a cikin anhydrous ethanol R kuma tsarma zuwa 25.0 ml tare da sauran ƙarfi iri ɗaya.
Najasa C. chromatography na bakin ciki (2.2.27).
Cakuda mai narkewa: ruwa R, acetone R (10:90 V/V).
Maganin gwaji (a).Narke 0.40 g na abun da za a bincika a cikin cakuda mai narkewa kuma a tsarma zuwa 10 ml tare da cakuda mai narkewa.
Maganin gwaji (b).Tsarma 1 ml na maganin gwajin (a) zuwa 10 ml tare da cakuda mai narkewa.
Maganin Magana (a).Narkar da 40 MG na ursodeoxycholic acid CRS a cikin cakuda mai narkewa kuma a tsoma shi zuwa 10 ml tare da cakuda mai narkewa.
Maganin Magana (b).Narkar da 20 MG na lithocholic acid CRS (najasa C) a cikin cakuda mai narkewa kuma a tsarma zuwa 10.0 ml tare da cakuda mai narkewa (maganin A).Tsarma 2.0 ml na wannan maganin zuwa 100.0 ml tare da cakuda mai narkewa.
Maganin Magana (c).Zuwa 5 ml na bayani A ƙara 10 MG na chenodeoxycholic acid CRS (najasa A) da kuma tsarma zuwa 50 ml tare da cakuda mai narkewa.
Plate: TLC silica gel farantin R.
Lokacin wayar hannu: glacial acetic acid R, acetone R, methylenechloride R (1:30:60 V/V/V).
Saukewa: 5μL.
Ci gaba: sama da 2/3 na farantin.
Bushewa: a 120 ℃ na 10 min.
Ganewa: fesa nan da nan tare da maganin 47.6 g/L na phosphomolybdic acid R a cikin cakuduwar 1 girma na sulfuric acid R da 20 juzu'i na glacial acetic acid R da zafi a 120 ℃ har sai launin shuɗi ya bayyana akan bango mai haske.
Dacewar tsarin: Magani (c):
- chromatogram yana nuna 2 a sarari rabe manyan aibobi.
Iyaka: maganin gwaji (a):
- rashin tsarki C: duk wani tabo saboda rashin tsarkin C bai fi tsanani ba fiye da babban tabo a cikin chromatogram da aka samu tare da bayani (b) (0.1%).
Abubuwan da ke da alaƙa.Liquid chromatography (2.2.29).
Cakuda mai narkewa: methanol R, lokacin wayar hannu (10:90 V/V).
Maganin gwaji.Narkar da 60 MG na abun da za a bincika a cikin cakuda mai narkewa kuma a tsarma zuwa 20.0 ml tare da cakuda mai narkewa.
Maganin Magana (a).Narkar da abin da ke cikin kwano na Ursodeoxycholic Acid don dacewa da tsarin CRS (mai ɗauke da datti A da H) a cikin 1.0 ml na cakuda mai narkewa.
Maganin Magana (b).Tsarma 1.0 ml na maganin gwajin zuwa 100.0 ml tare da cakuda mai narkewa.Tsarma 1.0 ml na wannan maganin zuwa 10.0 ml tare da cakuda mai narkewa.
Rukunin:
- girman: l = 0.25 m, Ø = 4.6 mm;
-tsayin lokaci: ƙarshen-capped octadecylsilyl silica gel donchromatography R (5 μm);
- zazzabi: 40 ℃ ± 1 ℃.
Lokacin wayar hannu: haxa nau'ikan 30 na acetonitrile R, juzu'i 37 na 0.78 g/L bayani na sodium dihydrogen phosphate R daidaitawa zuwa pH 3 tare da phosphoric acid R, da 40 juzu'i na methanol R.
Yawan gudu: 0.8ml/min.
Ganewa: refractometer a 35 ± 1 ℃.
Allura: 150 μL.
Lokacin gudu: sau 4 lokacin riƙewar Ursodeoxycholic acid.
Gane ƙazanta: yi amfani da chromatogram ɗin da aka kawo tare da ursodeoxycholic acid don dacewa da tsarin CRS da chromatogram da aka samu tare da maganin tunani (a) don gano kololuwa saboda ƙazanta A da H.
Dangantakar da ke da dangantaka da ursodeoxycholic acid (lokacin riƙewa = game da 14 min): ƙazanta H = game da 0.9;rashin tsarki A = kusan 2.8.
Dacewar tsarin: Magani na tunani (a):
-ƙuduri: ƙaramar 1.5 tsakanin kololuwa saboda ƙazanta H da ursodeoxycholic acid.
Iyaka:
- ƙazanta A: ba fiye da sau 10 na yanki na babba mafi girma a cikin chromatogram da aka samu tare da bayani na tunani (b) (1.0 bisa dari);
- ƙazantar da ba a bayyana ba: ga kowane ƙazanta, ba fiye da yanki na babba mafi girma a cikin chromatogram da aka samu tare da bayani mai mahimmanci (b) (0.10 bisa dari);
- jimlar: ba fiye da sau 15 na yanki na babba mafi girma a cikin chromatogram da aka samu tare da bayani na tunani (b) (1.5 bisa dari);
- rashin kula da iyaka: 0.5 sau yanki na babban kololuwa a cikin chromatogram da aka samu tare da bayani na tunani (b) (0.05 bisa dari).
Karfe masu nauyi (2.4.8): matsakaicin 20 ppm.
1.0 g ya bi gwajin C. Shirya maganin tunani ta amfani da 2 ml na daidaitaccen maganin gubar (10 ppm Pb) R.
Asarar bushewa (2.2.32): matsakaicin 1.0 bisa dari, ƙaddara akan 1.000 g ta bushewa a cikin tanda a 105 ℃.
Sulfated ash (2.4.14): matsakaicin 0.1 bisa dari, ƙaddara akan 1.0 g.
ASSAY
Narkar da 0.350 g a cikin 50 ml na ethanol (96 bisa dari) R, a baya an cire shi zuwa 0.2 ml na maganin phenolphthalein R. Ƙara 50 ml na ruwa R da titrate tare da 0.1 M sodium hydroxide har sai an sami launin ruwan hoda.
1 ml na 0.1 M sodium hydroxide yayi daidai da 39.26 MG na C24H40O4.
RASHIN ZUCIYA
ƙayyadaddun ƙazanta: A, C.
Sauran ƙazantattun abubuwan da za a iya ganowa (waɗannan abubuwa masu zuwa, idan sun kasance a isassun matakin, ɗaya ko wasu gwaje-gwajen da ke cikin monograph ɗin za su iya gano su. An iyakance su ta hanyar ma'aunin karɓuwa gabaɗaya don wasu ƙazantattun ƙazanta da / ko ta hanyar abubuwan da ke gaba ɗaya. Don yin amfani da magunguna (2034) Don haka ba lallai ba ne a gano waɗannan ƙazanta don nuna yarda. Duba kuma 5.10.
Gudanar da ƙazanta a cikin abubuwa don amfani da magunguna): B, D, E, F, G, H, I.
A. 3α,7a-dihydroxy-5β-cholan-24-oic acid (chenodeoxycholic acid),
B. 3α,7α,12a-trihydroxy-5β-cholan-24-oic acid (cholic acid),
C. 3a-hydroxy-5β-cholan-24-oic acid (lithocholic acid),
D. 3α,7β,12a-trihydroxy-5β-cholan-24-oic acid (ursocholic acid),
E. 3a,12a-dihydroxy-5β-cholan-24-oic acid (deoxycholic acid),
F. 3a-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.