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

URSODEOXYCHOLIC ACID
C24H40O4 Ọgbẹni 392.6[128-13-2]
ITUMO
3α,7β-Dihydroxy-5β-cholan-24-oic acid.
Akoonu: 99.0 fun ogorun si 101.0 fun ogorun (nkan ti o gbẹ).
ÀWỌN ÀWỌN ÀWỌN ADÁJỌ́
Irisi: funfun tabi fere funfun lulú.
Solubility: Oba insoluble ninu omi, larọwọto tiotuka ni ethanol (96 fun ogorun), die-die tiotuka ni acetone, Oba insoluble ni methylene kiloraidi.
mp: nipa 202 ℃.
Ìdámọ̀
Idanimọ akọkọ: A.
Idanimọ keji: B, C.
A. spectrophotometry gbigba infurarẹẹdi (2.2.24).
Ifiwera: Ursodeoxycholic Acid CRS.
B. Ṣe ayẹwo awọn chromatograms ti o gba ninu idanwo fun aimọ C.
Awọn abajade: aaye akọkọ ninu chromatogram ti a gba pẹlu ojutu idanwo (b) jẹ iru ni ipo, awọ ati iwọn si aaye akọkọ ninu chromatogram ti o gba pẹlu ojutu itọkasi (a).
C. Tu nipa 10 mg ninu 1 milimita sulfuric acid R. Fi 0.1 milimita ti formaldehyde ojutu R ati gba laaye lati duro fun iṣẹju 5.Fi 5 milimita ti omi kun R. Idaduro ti o gba jẹ alawọ alawọ-bulu.
AWON idanwo
Yiyi opitika kan pato (2.2.7): + 58.0 si + 62.0 (nkan ti o gbẹ).
Tu 0.500 g ninu ethanol R anhydrous ati dilute si 25.0 milimita pẹlu epo kanna.
Iwa aimọ C. Kiromatografi tinrin (2.2.27).
Apapo olomi: omi R, acetone R (10:90 V/V).
Idanwo ojutu (a).Tu 0.40 g ti nkan ti o yẹ ki o ṣe ayẹwo ni adalu olomi ati dilute si 10 milimita pẹlu adalu epo.
Idanwo ojutu (b).Dilute 1 milimita ti ojutu idanwo (a) si 10 milimita pẹlu adalu olomi.
Ojutu itọkasi (a).Tu 40 miligiramu ti ursodeoxycholic acid CRS sinu adalu olomi ati dilute si 10 milimita pẹlu adalu epo.
Ojutu itọkasi (b).Tu 20 miligiramu ti lithocholic acid CRS (aimọ aimọ C) ninu adalu olomi ati dilute si 10.0 milimita pẹlu adalu epo (ojutu A).Dilute 2.0 milimita ti ojutu yii si 100.0 milimita pẹlu adalu olomi.
Ojutu itọkasi (c).Si 5 milimita ti ojutu A ṣafikun 10 miligiramu ti chenodeoxycholic acid CRS (aimọ A) ati dilute si 50 milimita pẹlu adalu olomi.
Awo: TLC silica gel plate R.
Ipele alagbeka: glacial acetic acid R, acetone R, methylenekiloraidi R (1:30:60 V/V/V).
Ohun elo: 5μL.
Idagbasoke: lori 2/3 ti awo.
Gbigbe: ni 120 ℃ fun iṣẹju 10.
Iwari: fun sokiri lẹsẹkẹsẹ pẹlu ojutu 47.6 g/L ti phosphomolybdic acid R ninu adalu 1 iwọn didun ti sulfuric acid R ati awọn iwọn 20 ti glacial acetic acid R ati ooru ni 120 ℃ titi awọn aaye buluu yoo han lori ẹhin fẹẹrẹfẹ.
Ibamu eto: ojutu itọkasi (c):
- chromatogram fihan awọn aaye akọkọ ti o ya sọtọ 2 kedere.
Opin: ojutu idanwo (a):
-aimọ C: aaye eyikeyi nitori aimọ C ko ni iwọn diẹ sii ju aaye akọkọ ninu chromatogram ti a gba pẹlu ojutu itọkasi (b) (0.1 fun ogorun).
Awọn nkan ti o jọmọ.Kiromatogirafi olomi (2.2.29).
Apapo olomi: kẹmika R, alakoso alagbeka (10:90 V/V).
Idanwo ojutu.Tu 60 miligiramu ti nkan na lati ṣe ayẹwo ni adalu epo ati dilute si 20.0 milimita pẹlu adalu epo.
Ojutu itọkasi (a).Tu awọn akoonu inu vial kan ti Ursodeoxycholic Acid fun ibamu eto CRS (ti o ni awọn aimọ A ati H ninu) ni 1.0 milimita ti adalu olomi.
Ojutu itọkasi (b).Dilute 1.0 milimita ti ojutu idanwo si 100.0 milimita pẹlu adalu olomi.Dilute 1.0 milimita ti ojutu yii si 10.0 milimita pẹlu adalu olomi.
Àwọ̀n:
-iwọn: l = 0.25 m, Ø = 4.6 mm;
-Stationary alakoso: opin-capped octadecylsilyl silica jeli funchromatography R (5 μm);
- otutu: 40℃ ± 1℃.
Ipele alagbeka: dapọ awọn iwọn 30 ti acetonitrile R, awọn iwọn 37 ti ojutu 0.78 g/L ti iṣuu soda dihydrogen fosifeti R ni atunṣe si pH 3 pẹlu phosphoric acid R, ati awọn iwọn 40 ti methanol R.
Oṣuwọn sisan: 0.8 milimita / min.
Iwari: refractometer ni 35 ± 1 ℃.
Abẹrẹ: 150 μL.
Akoko ṣiṣe: awọn akoko 4 akoko idaduro Ursodeoxycholic Acid.
Idanimọ ti awọn aimọ: lo chromatogram ti a pese pẹlu ursodeoxycholic acid fun ibaramu eto CRS ati chromatogram ti a gba pẹlu ojutu itọkasi (a) lati ṣe idanimọ awọn giga julọ nitori awọn aimọ A ati H.
Idaduro ibatan pẹlu itọkasi si ursodeoxycholic acid (akoko idaduro = nipa 14 min): aimọ H = nipa 0.9;aimọ A = nipa 2,8.
Ibamu eto: ojutu itọkasi (a):
-ipinnu: o kere ju 1.5 laarin awọn oke giga nitori aimọ H ati ursodeoxycholic acid.
Awọn ifilelẹ:
- aimọ A: ko ju awọn akoko 10 lọ agbegbe ti tente oke akọkọ ni chromatogram ti a gba pẹlu ojutu itọkasi (b) (1.0 ogorun);
-awọn aiṣedeede ti ko ni pato: fun aimọ kọọkan, kii ṣe diẹ sii ju agbegbe ti o ga julọ ni chromatogram ti a gba pẹlu ojutu itọkasi (b) (0.10 fun ogorun);
- lapapọ: kii ṣe diẹ sii ju awọn akoko 15 agbegbe ti oke akọkọ ni chromatogram ti a gba pẹlu ojutu itọkasi (b) (1.5 ogorun);
-aibikita opin: awọn akoko 0.5 agbegbe ti tente akọkọ ninu chromatogram ti a gba pẹlu ojutu itọkasi (b) (0.05 ogorun).
Awọn irin ti o wuwo (2.4.8): o pọju 20 ppm.
1.0 g ni ibamu pẹlu idanwo C. Mura ojutu itọkasi nipa lilo 2 milimita ti ojutu boṣewa asiwaju (10 ppm Pb) R.
Pipadanu lori gbigbe (2.2.32): o pọju 1.0 fun ogorun, pinnu lori 1.000 g nipasẹ gbigbe ni adiro ni 105 ℃.
Sulfated eeru (2.4.14): o pọju 0.1 fun ogorun, pinnu lori 1.0 g.
ASAY
Tu 0.350 g ni 50 milimita ti ethanol (96 fun ogorun) R, ni iṣaaju didoju si 0.2 mL ti ojutu phenolphthalein R. Fi 50 milimita ti omi R ati titrate pẹlu 0.1 M sodium hydroxide titi ti awọ Pink yoo fi gba.
1 milimita ti 0.1 M sodium hydroxide jẹ deede si 39.26 mg ti C24H40O4.
ALÁÌṢẸ́
Awọn aimọ ti o ni pato: A, C.
Awọn idoti ti o ṣawari miiran (awọn nkan wọnyi yoo, ti o ba wa ni ipele ti o to, jẹ wiwa nipasẹ ọkan tabi miiran ti awọn idanwo ni monograph. Wọn ni opin nipasẹ ami iyasọtọ gbigba gbogbogbo fun awọn aimọ miiran / awọn aiṣedeede ati / tabi nipasẹ Awọn nkan monograph gbogbogbo Fun lilo oogun (2034) Nitori naa ko ṣe pataki lati ṣe idanimọ awọn aimọ wọnyi fun iṣafihan ibamu.Wo tun 5.10.
Iṣakoso ti awọn aimọ ni awọn nkan fun lilo oogun): 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.