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

URSODEOXYCHOLIC ACID
C24H40O4 Mnu 392.6[128-13-2]
INGCACISO
3α,7β-Dihydroxy-5β-cholan-24-oic acid.
Umxholo: i-99.0 ipesenti ukuya kwi-101.0 ipesenti (into eyomileyo).
ABAlinganiswa
Ukubonakala: umhlophe okanye phantse umgubo omhlophe.
Ukunyibilika: ngokwenyani akunyibiliki emanzini, kunyibilika ngokukhululekileyo kwi-ethanol (ipesenti ezingama-96), ukunyibilika kancinane kwi-acetone, ayinyibiliki kwi-methylene chloride.
mp: malunga 202℃.
UKUCHAZA
Isazisi sokuqala: A.
Isazisi sesibini: B, C.
A. I-Infrared absorption spectrophotometry (2.2.24).
Uthelekiso: Ursodeoxycholic Acid CRS.
B. Hlola iichromatograms ezifunyenwe kuvavanyo lokungacoceki C.
Iziphumo: indawo ephambili kwichromatogram efunyenwe ngesisombululo sovavanyo (b) iyafana kwindawo, umbala kunye nobukhulu kwindawo ephambili kwichromatogram efunyenwe ngesisombululo sereferensi (a).
C. Dissolve malunga ne-10 mg kwi-1 mL ye-sulfuric acid R. Yongeza i-0.1 mL yesisombululo se-formaldehyde R kwaye uvumele ukuma i-5 min.Yongeza i-5 mL yamanzi R. Ukumiswa okufunyenweyo kuluhlaza-blue.
UVAVANYO
Ukujikeleza okuthe ngqo kwe-optical (2.2.7): + 58.0 ukuya + 62.0 (into eyomileyo).
Chitha i-0.500 g kwi-ethanol R e-anhydrous kwaye udibanise kwi-25.0 mL kunye ne-solvent efanayo.
Ukungcola C. Thin-layer chromatography (2.2.27).
Umxube wokunyibilikisa: amanzi R, i-acetone R (10:90 V/V).
Isisombululo sovavanyo (a).Chitha i-0.40 g yezinto eziza kuhlolwa kumxube we-solvent kwaye udibanise kwi-10 mL kunye nomxube we-solvent.
Isisombululo sovavanyo (b).Nciphisa i-1 mL yesisombululo sovavanyo (a) ukuya kwi-10 mL ngomxube we-solvent.
Isisombululo seReferensi (a).Dissolve 40 mg ye-ursodeoxycholic acid CRS kumxube we-solvent kwaye uhlambulule kwi-10 mL ngomxube we-solvent.
Isisombululo seReferensi (b).Dissolve i-20 mg ye-lithocholic acid CRS (ukungcola C) kumxube we-solvent kwaye udibanise kwi-10.0 mL kunye nomxube we-solvent (isisombululo A).Nciphisa i-2.0 mL yesi sisombululo kwi-100.0 mL kunye nomxube we-solvent.
Isisombululo seReferensi (c).Kwi-5 mL yesisombululo A yongeza i-10 mg ye-chenodeoxycholic acid CRS (ukungcola A) kwaye uhlambulule kwi-50 mL ngomxube we-solvent.
Icwecwe: TLC silica gel plate R.
Isigaba seselula: i-glacial acetic acid R, i-acetone R, i-methyleneikloridi R (1:30:60 V/V/V).
Isicelo: 5μL.
Uphuhliso: ngaphezu kwe-2/3 yepleyiti.
Ukomisa: kwi-120 ℃ nge-10 min.
Ukufumanisa: fafaza ngokukhawuleza ngesisombululo se-47.6 g / L se-phosphomolybdic acid R kumxube we-1 umthamo we-sulfuric acid R kunye ne-20 ye-glacial acetic acid R kunye nobushushu kwi-120 ℃ kude kube amabala aluhlaza avela kwimvelaphi ekhanyayo.
Ukufaneleka kwenkqubo: isisombululo sesalathiso (c):
- ichromatogram ibonisa amabala enqununu ama-2 ahluke ngokucacileyo.
Umda: isisombululo sovavanyo (a):
-ukungcola C: nayiphi na indawo ngenxa yokungcola C ayinamandla ngaphezu kwendawo eyintloko kwichromatogram efunyenwe ngesisombululo sokubhekisela (b) (ipesenti ze-0.1).
Izinto ezinxulumeneyo.Ichromatography yolwelo (2.2.29).
Umxube wokunyibilikisa: i-methanol R, isigaba esihambayo (10:90 V / V).
Isisombululo sovavanyo.Dissolve i-60 mg yezinto eziza kuhlolwa kumxube we-solvent kwaye udibanise kwi-20.0 mL ngomxube we-solvent.
Isisombululo seReferensi (a).Dissolve imixholo ye-vial ye-Ursodeoxycholic Acid yokufaneleka kwe-CRS (equlethe ukungcola A kunye ne-H) kwi-1.0 mL yomxube we-solvent.
Isisombululo seReferensi (b).Nciphisa i-1.0 mL yesisombululo sovavanyo kwi-100.0 mL kunye nomxube we-solvent.Nciphisa i-1.0 mL yesi sisombululo kwi-10.0 mL kunye nomxube we-solvent.
Uluhlu:
-ubungakanani: l = 0.25 m, Ø = 4.6 mm;
-isigaba sokumisa: i-end-capped octadecylsilyl silica gel yeikromatografi R (5 μm);
- iqondo lobushushu: 40℃ ± 1℃.
Isigaba seselula: xuba imiqulu ye-30 ye-acetonitrile R, imiqulu ye-37 ye-0.78 g / L isisombululo se-sodium dihydrogen phosphate R elungiswe kwi-pH 3 kunye ne-phosphoric acid R, kunye ne-40 imiqulu ye-methanol R.
Izinga lokuhamba: 0.8 mL / min.
Ukufunyanwa: i-refractometer kwi-35 ± 1℃.
Isitofu: 150 μL.
Ixesha lokugijima: amaxesha ama-4 ixesha lokugcinwa kwe-Ursodeoxycholic Acid.
Ukuchongwa kokungcola: sebenzisa ichromatogram ebonelelwe nge-ursodeoxycholic acid yokufaneleka kwenkqubo iCRS kunye nechromatogram efunyenwe ngesisombululo sereferensi (a) ukuchonga iincopho ngenxa yobumdaka A kunye no-H.
Ukugcinwa okuhambelanayo ngokubhekiselele kwi-ursodeoxycholic acid (ixesha lokugcinwa = malunga ne-14 min): ukungcola H = malunga ne-0.9;ukungcola A = malunga ne-2.8.
Ukufaneleka kwenkqubo: isisombululo sesalathiso (a):
-isisombululo: ubuncinci be-1.5 phakathi kweencopho ngenxa yokungcola H kunye ne-ursodeoxycholic acid.
Imida:
- ukungcola A: akukho ngaphezu kwamaxesha e-10 indawo yenqununu yenqununu kwi-chromatogram efunyenwe ngesisombululo sokubhekisela (b) (i-1.0 ekhulwini);
-ukungcola okungachazwanga: kukungcola ngalunye, kungabi ngaphezu kwendawo yenqununu yenqununu kwichromatogram efunyenwe ngesisombululo sokubhekisela (b) (0.10 ekhulwini);
- iyonke: ingabi ngaphezu kwe-15 amaxesha kwindawo yenqununu yenqununu kwi-chromatogram efunyenwe ngesisombululo sokubhekisela (b) (i-1.5 ekhulwini);
-ukungahoyi umda: amaxesha e-0.5 indawo yenqununu yenqununu kwi-chromatogram efunyenwe ngesisombululo sokubhekisela (b) (i-0.05 ekhulwini).
Iintsimbi ezinzima (2.4.8): ubuninzi be-20 ppm.
I-1.0 g ihambelana novavanyo C. Lungiselela isisombululo sereferensi usebenzisa i-2 mL yesisombululo esiqhelekileyo se-lead (10 ppm Pb) R.
Ilahleko ekomisweni (2.2.32): ubuninzi beepesenti ze-1.0, kunqunywe kwi-1.000 g ngokumisa kwi-oven kwi-105 ℃.
Uthuthu lwe-Sulfated (2.4.14): ubuninzi beepesenti ze-0.1, kunqunywe kwi-1.0 g.
UVAVANYO
Dlulisa i-0.350 g kwi-50 mL ye-ethanol (ipesenti ezingama-96) R, ngaphambili ingathathi hlangothi kwi-0.2 mL yesisombululo se-phenolphthalein R. Yongeza i-50 mL yamanzi R kunye ne-titrate kunye ne-0.1 M i-sodium hydroxide kuze kufumaneke umbala opinki.
I-1 mL ye-0.1 M i-sodium hydroxide ilingana ne-39.26 mg ye-C24H40O4.
UBUNGCOLA
Ukungcola okuchaziweyo: A, C.
Olunye ukungcola okubonakalayo (ezi zinto zilandelayo ziyakuthi, ukuba zikho kwinqanaba elaneleyo, zibhaqwe ngolunye okanye ezinye iimvavanyo kwi-monograph. Zithintelwe ngumqathango wokwamkelwa ngokubanzi kwezinye / ukungcola okungachazwanga kunye / okanye nge-monograph yezinto ngokubanzi. kusetyenziso lwamayeza (ngo-2034) ke ngoko akuyomfuneko ukuchonga obu kungcola ukubonisa ukuthotyelwa.Bona naku-5.10.
Ukulawulwa kokungcola kwizinto zokusetyenziswa kweyeza): B, D, E, F, G, H, I.
A. 3α, 7α-dihydroxy-5β-cholan-24-oic acid (i-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.