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

URSODEOXYCHOLIC AID
C24H40O4 Mr 392.6[128-13-2]
Qeexitaan
3α,7β-Dihydroxy-5β-cholan-24-oic acid.
Waxa ku jira: 99.0 boqolkiiba ilaa 101.0 boqolkiiba (walaxda qalalan).
MEESHA
Muuqaal: cad ama ku dhawaad ​​budo cad.
Solubility: ficil ahaan aan biyo ku milmin, si xor ah ugu milmi kara ethanol (96 boqolkiiba), in yar oo ku milma acetone, ficil ahaan aan milmi karin methylene chloride.
mp: qiyaastii 202 ℃.
AQOONSIGA
Aqoonsiga koowaad: A.
Aqoonsiga labaad: B, C.
A. spectrophotometry nuugista infrared (2.2.24).
Isbarbardhigga: Ursodeoxycholic Acid CRS.
B. Ka baadh chromatogram-yada lagu helay baaritaanka wasakhnimada C.
Natiijooyinka: meesha ugu muhiimsan ee chromatogram-ka ee lagu helay xalka tijaabada (b) waxay la mid tahay booska, midabka iyo cabbirka meesha ugu muhiimsan ee chromatogram-ka ee lagu helay xal tixraaceed (a).
C. Ku mil ilaa 10 mg 1 ml oo sulfuric acid R. Ku dar 0.1 mL oo xal formaldehyde R una ogolow inaad istaagto 5 min.Ku dar 5 ml oo biyo ah R. Ka joojinta la helay waa cagaar-buluug.
IMTIXAANKA
Wareegga indhaha ee gaarka ah (2.2.7): + 58.0 ilaa + 62.0 (walxaha qallalan).
Ku mil 0.500 g ethanol R anhydrous oo ku mil 25.0 mL oo leh dareere isku mid ah.
Nijaasnimo C. chromatography khafiif ah (2.2.27).
Isku darka dareeraha: biyaha R, acetone R (10:90 V/V).
Xalka tijaabada (a).Kala dir 0.40 g oo ah walaxda lagu baaro isku dhafka dareeraha oo ku milo 10 mL isku darka dareeraha.
Xalka tijaabada (b).Ku qas 1 ml oo xal tijaabo ah (a) ilaa 10 mL isku darka dareeraha.
Xalka tixraaca (a).Ku mil 40 mg ee ursodeoxycholic acid CRS ee isku darka dareeraha oo ku milo 10 mL isku darka dareeraha.
Xalka tixraaca (b).Ku mil 20 mg ee lithocholic acid CRS (nijaasta C) isku darka dareeraha oo ku mil 10.0 ml isku dar ah dareeraha (xalka A).Ku qas 2.0 ml ee xalkan ilaa 100.0 ml isku dar ah dareeraha.
Xalka tixraaca (c).Ilaa 5 mL oo xal ah ku dar 10 mg oo chenodeoxycholic acid CRS ( wasakh A) oo ku mil 50 mL isku darka dareeraha ah.
Saxan: TLC silica gel saxan R.
Marxaladda wareega: glacial acetic acid R, acetone R, methylenechloride R (1:30:60 V/V/V).
Codsiga: 5μL.
Horumarinta: in ka badan 2/3 ee saxanka.
Qallajinta: at 120 ℃ 10 daqiiqo.
Ogaanshaha: ku buufin isla markiiba 47.6 g/L xal fosphomolybdic acid R isku dar ah 1 mug ah sulfuric acid R iyo 20 mugga glacial acetic acid R iyo kulayl 120 ℃ ilaa dhibco buluug ahi ka soo baxaan asal khafiif ah.
Ku habboonaanta nidaamka: xallinta tixraaca (c):
- chromatogram-ku waxa uu muujinayaa 2 dhibcood oo waaweyn oo si cad u kala soocan.
Xadka: xalka tijaabada (a):
-nijaasnimo C: meel kasta oo ay ugu wacan tahay wasakhda C kama badna meesha ugu muhiimsan ee chromatogramka ee lagu helay xal tixraaceed (b) (0.1 boqolkiiba).
Walxaha la xidhiidha.chromatography dareere ah (2.2.29).
Isku darka dareeraha: methanol R, wajiga wareega (10:90 V/V).
Xalka tijaabada.Kala dir 60 mg ee walaxda lagu baaro isku darka dareeraha oo ku milo 20.0 mL isku darka dareeraha.
Xalka tixraaca (a).Kala dir waxa ku jira fiilo Ursodeoxycholic Acid ee ku habboonaanta nidaamka CRS (ka kooban wasakh A iyo H) 1.0 mL ee isku dhafka dareeraha ah.
Xalka tixraaca (b).Ku qas 1.0 mL ee xalka tijaabada ilaa 100.0 mL isku darka dareeraha.Ku qas 1.0 mL ee xalkan ilaa 10.0 ml isku dar ah dareeraha.
Tiirka:
-xajmiga: l = 0.25 m, Ø = 4.6 mm;
Marxaladda taagan: octadecylsilyl silica gel-ka-dhammaadka leh ee loogu talagalaychromatography R (5 μm);
- heerkulka: 40℃ ± 1℃.
Wajiga mobilada: isku dar 30 mug oo acetonitrile R, 37 mug oo ah 0.78 g/L xal sodium dihydrogen phosphate R oo lagu hagaajiyay pH 3 oo leh fosfooric acid R, iyo 40 mugga methanol R.
Heerka socodka: 0.8 mL/daqiiqo.
Ogaanshaha: refractometer at 35 ± 1 ℃.
Cirbad: 150 μL.
Wakhtiga orodka: 4 jeer wakhtiga haynta ursodeoxycholic acid.
Aqoonsiga wasakhda: isticmaal chromatogram-ka ay ku jirto ursodeoxycholic acid ee ku habboonaanta nidaamka CRS iyo chromatogram-ka lagu helay xalka tixraaca (a) si loo aqoonsado meelaha ugu sarreeya ee wasakhda A iyo H.
Haysashada qaraabada ah iyada oo la tixraacayo ursodeoxycholic acid (waqtiga haynta = qiyaastii 14 min): wasakh H = qiyaastii 0.9;wasakh A = qiyaastii 2.8.
Habboonaanta nidaamka: xal tixraac (a):
-xallin: ugu yaraan 1.5 inta u dhaxaysa meelaha ugu sarreeya sababtoo ah wasakhda H iyo ursodeoxycholic acid.
Xaddid:
- wasakh A: aan ka badnayn 10 jeer aagga ugu sarreeya ee chromatogram-ka ee lagu helay xal tixraaceed (b) (1.0 boqolkiiba);
Nijaasta aan la cayimin: wasakh kasta, oo aan ka badnayn aagga ugu sarreeya ee chromatogram-ka ee la helay xalka tixraaca (b) (0.10 boqolkiiba);
- wadarta: aan ka badnayn 15 jeer aagga ugu sarreeya ee chromatogram-ka ee lagu helay xal tixraaceed (b) (1.5 boqolkiiba);
Xadid la'aanta: 0.5 jeer bedka ugu sarreeya ee chromatogram-ka ee lagu helay xal tixraaceed (b) (0.05 boqolkiiba).
Biraha culus (2.4.8): ugu badnaan 20 ppm.
1.0 g ayaa u hoggaansamaya tijaabada C. Diyaari xalka tixraaca adigoo isticmaalaya 2 ml oo ah xalka caadiga ah ee rasaasta (10ppm Pb) R.
Luminta qalajinta (2.2.32): ugu badnaan 1.0 boqolkiiba, waxaa lagu go'aamiyay 1.000 g iyadoo lagu qallajinayo foornada 105 ℃.
Dambaska sulfated (2.4.14): ugu badnaan 0.1 boqolkiiba, oo lagu go'aamiyay 1.0 g.
ASSAY
Ku milmi 0.350 g 50 mL ee ethanol (96 boqolkiiba) R, oo hore looga dhexlay 0.2 mL of phenolphthalein xal R. Ku dar 50 mL oo biyo ah R iyo titrate leh 0.1 M sodium hydroxide ilaa midab casaan ah laga helayo.
1 ml oo ah 0.1 M sodium hydroxide waxay u dhigantaa 39.26 mg ee C24H40O4.
XANUUNKA
Wasakhda cayiman: A, C.
Wasakhyada kale ee la ogaan karo (walxaha soo socdaa, haddii ay jiraan heer ku filan, waxaa lagu ogaan karaa hal ama mid kale oo ka mid ah tijaabooyinka monograph. Waxay xaddidan yihiin shuruudaha aqbalaadda guud ee wasakhooyinka kale/aan la cayimin iyo/ama hal-abuurka guud Walxaha Isticmaalka dawooyinka (2034) Sidaa darteed muhiim maaha in la garto waxyaalahan wasakhaysan si loo muujiyo u hoggaansanaanta, sidoo kale eeg 5.10.
Xakamaynta wasakhda walxaha loogu talagalay isticmaalka dawooyinka): 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. 3α,12α-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.