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

I-URSODEOXYCHOLIC ACID
C24H40O4 Mnu 392.6[128-13-2]
INCAZELO
I-3α,7β-Dihydroxy-5β-cholan-24-oic acid.
Okuqukethwe: 99.0% ukuya ku-101.0% (into eyomisiwe).
ABALINGISI
Ukubukeka: impushana emhlophe noma cishe emhlophe.
Ukunyibilika: cishe akuncibiliki emanzini, kuncibilika ngokukhululeka ku-ethanol (amaphesenti angama-96), kuncibilika kancane ku-acetone, cishe okungancibiliki ku-methylene chloride.
mp: mayelana ne-202℃.
UKUKHOMBA
Umazisi wokuqala: A.
Ukuhlonza okwesibili: B, C.
A. I-spectrophotometry yokumuncwa kwe-infrared (2.2.24).
Ukuqhathanisa: Ursodeoxycholic Acid CRS.
B. Hlola ama-chromatogram atholwe ekuhlolweni kokungcola C.
Imiphumela: indawo eyinhloko kuchromatogram etholwe ngesixazululo sokuhlola (b) iyafana ngokuma, umbala nosayizi nendawo eyinhloko kuchromatogram etholwe ngesixazululo sereferensi (a).
C. Chaza cishe u-10 mg ku-1 mL ye-sulfuric acid R. Engeza u-0.1 mL wesisombululo se-formaldehyde R bese uvumela ukuthi ume imizuzu emi-5.Engeza u-5 mL wamanzi R. Ukumiswa okutholiwe kuluhlaza okwesibhakabhaka.
IZIVIVINYO
Ukujikeleza okuqondile kwe-optical (2.2.7): + 58.0 kuya ku- + 62.0 (into eyomisiwe).
Chaza u-0.500 g ku-ethanol R engamanzi bese uncibilikisa ibe ngu-25.0 mL nge-solvent efanayo.
Ukungcola C. I-chromatography yongqimba oluncane (2.2.27).
Ingxube ye-solvent: amanzi R, i-acetone R (10:90 V/V).
Isixazululo sokuhlola (a).Chaza u-0.40 g wento ezohlolwa engxubeni ye-solvent bese unciphisa ibe ngu-10 ml ngengxube ye-solvent.
Isixazululo sokuhlola (b).Nciphisa i-1 mL yesisombululo sokuhlola (a) kuya ku-10 mL ngengxube ye-solvent.
Isixazululo sereferensi (a).Chaza u-40 mg we-ursodeoxycholic acid CRS kungxube ye-solvent bese unciphisa ku-10 mL ngengxube ye-solvent.
Isixazululo sereferensi (b).Chaza u-20 mg we-lithocholic acid CRS (ukungcola C) kungxube ye-solvent bese unciphisa ku-10.0 mL ngengxube ye-solvent (isixazululo A).Nciphisa u-2.0 mL walesi sixazululo sibe ngu-100.0 mL ngengxube ye-solvent.
Isixazululo sereferensi (c).Ku-5 mL wesixazululo A engeza u-10 mg we-chenodeoxycholic acid CRS (ukungcola A) bese unciphisa ku-50 mL ngengxube ye-solvent.
Ipuleti: TLC silica gel plate R.
Isigaba seselula: i-glacial acetic acid R, i-acetone R, i-methylenei-chloride R (1:30:60 V/V/V).
Isicelo: 5μL.
Ukuthuthukiswa: ngaphezu kwe-2/3 yepuleti.
Ukomisa: ku-120 ℃ imizuzu engu-10.
Ukutholwa: fafaza ngokushesha ngesixazululo esingu-47.6 g/L se-phosphomolybdic acid R enhlanganisweni engu-1 yevolumu ye-sulfuric acid R kanye nevolumu engu-20 ye-glacial acetic acid R kanye nokushisa ku-120℃ kuze kuvele amachashaza aluhlaza kungemuva elilula.
Ukufaneleka kwesistimu: isixazululo sereferensi (c):
- ichromatogram ikhombisa izindawo eziyinhloko ezihlukene ezi-2.
Umkhawulo: isixazululo sokuhlola (a):
-ukungcola C: noma iyiphi indawo ngenxa yokungcola C ayinamandla kakhulu kunendawo eyinhloko ku-chromatogram etholwe ngesisombululo sereferensi (b) (amaphesenti angu-0.1).
Izinto ezihlobene.I-chromatography yoketshezi (2.2.29).
Ingxube ye-solvent: i-methanol R, isigaba seselula (10:90 V/V).
Isixazululo sokuhlola.Chaza u-60 mg wento ezohlolwa engxubeni ye-solvent bese unciphisa ibe ngu-20.0 mL ngengxube ye-solvent.
Isixazululo sereferensi (a).Chaza okuqukethwe kwe-vial ye-Ursodeoxycholic Acid yokufaneleka kwesistimu ye-CRS (equkethe ukungcola A no-H) ngo-1.0 mL wengxube ye-solvent.
Isixazululo sereferensi (b).Nciphisa u-1.0 mL wesixazululo sokuhlola sibe ngu-100.0 mL ngengxube ye-solvent.Nciphisa u-1.0 mL walesi sixazululo sibe ngu-10.0 mL ngengxube ye-solvent.
Ikholomu:
-usayizi: l = 0.25 m, Ø = 4.6 mm;
-isigaba sokumisa: ijeli ye-silica ye-octadecylsilyl evaliwei-chromatography R (5 μm);
- izinga lokushisa: 40℃ ± 1℃.
Isigaba seselula: hlanganisa imiqulu engu-30 ye-acetonitrile R, imiqulu engama-37 yesisombululo esingu-0.78 g/L se-sodium dihydrogen phosphate R elungiswe yaba yi-pH 3 ne-phosphoric acid R, kanye namavolumu angu-40 e-methanol R.
Izinga lokugeleza: 0.8 mL/min.
Ukutholwa: i-refractometer ku-35 ± 1℃.
Umjovo: 150 μL.
Isikhathi sokuqalisa: izikhathi ezi-4 kunesikhathi sokugcinwa kwe-Ursodeoxycholic Acid.
Ukuhlonza ukungcola: sebenzisa i-chromatogram ehlinzekwe nge-ursodeoxycholic acid ukuze uthole uhlelo lwe-CRS olufaneleka kanye ne-chromatogram etholwe ngesixazululo sereferensi (a) ukuze uhlonze iziqongo ngenxa yokungcola A no-H.
Ukugcinwa okuhlobene ngokubhekisela ku-ursodeoxycholic acid (isikhathi sokugcina = mayelana ne-14 min): ukungcola H = mayelana ne-0.9;ukungcola A = cishe 2.8.
Ukufaneleka kwesistimu: isixazululo sereferensi (a):
-ukulungiswa: ubuncane be-1.5 phakathi kweziqongo ngenxa yokungcola H kanye ne-ursodeoxycholic acid.
Imikhawulo:
- ukungcola A: hhayi izikhathi ezingaphezu kwezingu-10 endaweni yokuphakama okuyinhloko ku-chromatogram etholwe ngesixazululo sereferensi (b) (amaphesenti angu-1.0);
-ukungcola okungacacisiwe: ngokungcola ngakunye, kungabi ngaphezu kwendawo yokuphakama okuyinhloko kuchromatogram etholwe ngesixazululo sereferensi (b) (0.10 per cent);
- inani: izikhathi ezingeqile kwezingu-15 indawo yokuphakama okuyinhloko kuchromatogram etholwe ngesixazululo sereferensi (b) (amaphesenti angu-1.5);
-umkhawulo wokunganaki: izikhathi ezingu-0.5 indawo yokuphakama okuyinhloko ku-chromatogram etholwe ngesixazululo sereferensi (b) (amaphesenti angu-0.05).
Izinsimbi ezinzima (2.4.8): umkhawulo ongu-20 ppm.
I-1.0 g ithobelana nokuhlola C. Lungiselela isisombululo sereferensi usebenzisa u-2 mL wesisombululo esijwayelekile somthofu (10 ppm Pb) R.
Ukulahlekelwa ekumisweni (2.2.32): ubuningi bamaphesenti angu-1.0, kunqunywa ku-1.000 g ngokomiswa kuhhavini ngo-105℃.
Umlotha one-sulfated (2.4.14): ubuningi bamaphesenti angu-0.1, bunqunywe ku-1.0 g.
ISIVIVINYO
Chaza u-0.350 g ku-50 mL we-ethanol (amaphesenti angu-96) R, ngaphambilini ayengashintshiwe waba ngu-0.2 mL wesisombululo se-phenolphthalein R. Engeza u-50 mL wamanzi R bese u-titrate ngo-0.1 M sodium hydroxide kuze kutholakale umbala ophinki.
I-1 mL ka-0.1 M i-sodium hydroxide ilingana no-39.26 mg we-C24H40O4.
UKUNGCOLA
Ukungcola okucacisiwe: A, C.
Okunye ukungcola okuqaphelekayo (izinto ezilandelayo, uma zikhona ezingeni elanele, zizotholwa ngokukodwa noma okunye kokuhlola ku-monograph. Zinqunyelwe indinganiso evamile yokwamukela kokunye/ukungcola okungashiwongo kanye/noma ngezinto ezivamile ze-monograph. ukuze kusetshenziswe imithi (2034) Ngakho-ke akudingekile ukukhomba lokhu kungcola ukuze kuboniswe ukuthobelana. Bheka futhi 5.10.
Ukulawulwa kokungcola ezintweni ezisetshenziselwa ukwenza imithi): 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,
I-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.