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

URSODEOXYCHOLIC ACID
C24H40O4 Mr 392.6[128-13-2]
HOAKAKA
3α,7β-Dihydroxy-5β-cholan-24-oic acid.
ʻIke: 99.0 pākēneka a 101.0 pākēneka (mea maloʻo).
NA ANOAI
Nānā: keʻokeʻo a aneane keʻokeʻo pauka.
Hoʻoheheʻe: hiki ʻole ke hoʻoheheʻe ʻia i ka wai, hiki ke hoʻoheheʻe ʻia i ka ethanol (96 pākēneka), hiki ke hoʻoheheʻe ʻia i ka acetone, hiki ʻole ke hoʻoheheʻe ʻia i ka methylene chloride.
mp: ma kahi o 202 ℃.
IKE
ʻO ka ʻike mua: A.
ʻO ka ʻike lua: B, C.
A. Infrared absorption spectrophotometry (2.2.24).
Hoʻohālikelike: Ursodeoxycholic Acid CRS.
B. E nānā i nā chromatograms i loaʻa i ka hoʻāʻo no ka haumia C.
Nā hualoaʻa: ʻo ke kiko nui o ka chromatogram i loaʻa me ka hoʻonā hoʻāʻo (b) ua like ia i ke kūlana, ka waihoʻoluʻu a me ka nui me ke kiko nui o ka chromatogram i loaʻa me ka hoʻonā kuhikuhi (a).
C. E hoʻoheheʻe ma kahi o 10 mg i ka 1 mL o ka waikawa sulfuric R. E hoʻohui i 0.1 mL o ka wai formaldehyde R a e kū no 5 min.E hoʻohui i 5 mL o ka wai R. ʻO ka hoʻokuʻu i loaʻa he ʻōmaʻomaʻo-uliuli.
NA HOAO
ʻO ka hoʻololi ʻana o ka optical kikoʻī (2.2.7): + 58.0 a i + 62.0 (mea maloʻo).
E hoʻoheheʻe i 0.500 g i ka ethanol R a hoʻoheheʻe i 25.0 mL me ka mea hoʻokahi.
haumia C. Thin-layer chromatography (2.2.27).
Hui hoʻoheheʻe: wai R, acetone R (10:90 V/V).
Haʻina hoʻāʻo (a).E hoʻoheheʻe i 0.40 g o ka mea e nānā ʻia i loko o ka hui solvent a hoʻoheheʻe i ka 10 mL me ka hui solvent.
Haʻina hoʻāʻo (b).E hoʻoheheʻe i 1 mL o ka hoʻonā hoʻāʻo (a) i 10 mL me ka hui hoʻoheheʻe.
Haʻina kuhikuhi (a).E hoʻoheheʻe i 40 mg o ka ursodeoxycholic acid CRS i loko o ka hui hoʻoheheʻe a hoʻoheheʻe i 10 mL me ka hui hoʻoheheʻe.
Haʻina kuhikuhi (b).E hoʻoheheʻe i ka 20 mg o ka lithocholic acid CRS (ka haumia C) i loko o ka hui solvent a hoʻoheheʻe ʻia i 10.0 mL me ka hui solvent (pane A).E hoʻoheheʻe i 2.0 mL o kēia hoʻonā i 100.0 mL me ka hui hoʻoheheʻe.
Haʻina kuhikuhi (c).I ka 5 mL o ka solution A e hoʻohui i 10 mg o ka chenodeoxycholic acid CRS (ka haumia A) a e hoʻoheheʻe i 50 mL me ka hui ʻana.
Papa: TLC silica gel plate R.
Māhele kelepona: ʻakika acetic glacial R, acetone R, methylenechloride R (1:30:60 V/V/V).
Noi: 5μL.
Hoʻomohala: ma luna o 2/3 o ka pā.
Hoʻomaloʻo: ma 120 ℃ no 10 min.
ʻIke: e kāpī koke me ka 47.6 g/L solution o ka phosphomolybdic acid R i loko o ka hui ʻana o 1 volume o ka sulfuric acid R a me 20 mau puke o ka glacial acetic acid R a me ka wela ma 120 ℃ a hiki i ka ʻike ʻana o nā kiko polū ma kahi ʻoi aku ka māmā.
ʻO ke kūpono o ka ʻōnaehana: hoʻonā kuhikuhi (c):
- hōʻike ka chromatogram i 2 mau kiko nui i hoʻokaʻawale ʻia.
Palena: hoʻonā hoʻāʻo (a):
-ʻeleʻele C: ʻaʻole ʻoi aku ka ikaika o kekahi wahi ma muli o ka haumia C ma mua o ka wahi nui o ka chromatogram i loaʻa me ka hopena kuhikuhi (b) (0.1 pākēneka).
Nā mea pili.ʻO ka chromatography wai (2.2.29).
Ka hui ʻana o ka mea hoʻoheheʻe: methanol R, ka pae paʻa (10:90 V/V).
Hoʻoholo hoʻāʻo.E hoʻoheheʻe i 60 mg o ka mea e nānā ʻia i loko o ka hui solvent a hoʻoheheʻe i ka 20.0 mL me ka hui solvent.
Haʻina kuhikuhi (a).E hoʻoheheʻe i nā mea i loko o kahi hue o Ursodeoxycholic Acid no ka pono o ka ʻōnaehana CRS (loaʻa nā haumia A a me H) i loko o 1.0 mL o ka hui solvent.
Haʻina kuhikuhi (b).E hoʻoheheʻe i 1.0 mL o ka hopena hoʻāʻo i 100.0 mL me ka hui ʻana o ka solvent.E hoʻoheheʻe i 1.0 mL o kēia hoʻonā i 10.0 mL me ka hui solvent.
kolamu:
-nui: l = 0.25 m, Ø = 4.6 mm;
-paʻa kūʻokoʻa: hoʻopaʻa hope octadecylsilyl silica gel nochromatography R (5 μm);
- wela: 40 ℃ ± 1 ℃.
ʻĀpana paʻa: hoʻohui i 30 mau puke o ka acetonitrile R, 37 mau puke o kahi solution 0.78 g/L o ka sodium dihydrogen phosphate R i hoʻoponopono ʻia i ka pH 3 me ka waikawa phosphoric R, a me 40 mau puke o ka methanol R.
Kahe kahe: 0.8 mL / min.
ʻIke: refractometer ma 35 ± 1 ℃.
Hoʻopili: 150 μL.
Ka manawa holo: 4 manawa ka manawa paʻa o ka Ursodeoxycholic Acid.
Ka ʻike ʻana i nā haumia: e hoʻohana i ka chromatogram i hāʻawi ʻia me ka ursodeoxycholic acid no ka pono o ka ʻōnaehana CRS a me ka chromatogram i loaʻa me ka hoʻonā kuhikuhi (a) e ʻike i nā piko ma muli o nā haumia A a me H.
ʻO ka paʻa ʻana me ka pili ʻana i ka ursodeoxycholic acid (manawa paʻa = ma kahi o 14 min): haumia H = ma kahi o 0.9;haumia A = ma kahi o 2.8.
ʻO ke kūpono o ka ʻōnaehana: ʻōlelo hoʻonā (a):
-ka hoʻonā: 1.5 liʻiliʻi ma waena o nā piko ma muli o ka haumia H a me ka waikawa ursodeoxycholic.
Nā palena:
- haumia A: ʻaʻole ʻoi aku ma mua o 10 mau manawa o ka ʻāpana o ka piko nui o ka chromatogram i loaʻa me ka hoʻonā kuhikuhi (b) (1.0 pakeneka);
-ʻaʻole i hoʻopaʻa ʻia: no kēlā me kēia haumia, ʻaʻole i ʻoi aku ma mua o ka ʻāpana o ka piko nui o ka chromatogram i loaʻa me ka hopena kuhikuhi (b) (0.10 pākēneka);
- ka huina: ʻaʻole ʻoi aku ma mua o 15 mau manawa o ka ʻāpana o ka piko nui o ka chromatogram i loaʻa me ka hoʻonā kuhikuhi (b) (1.5 pakeneka);
-Ka palena palena ʻole: 0.5 manawa ka ʻāpana o ka piko nui o ka chromatogram i loaʻa me ka hoʻonā kuhikuhi (b) (0.05 pakeneka).
Nā metala kaumaha (2.4.8): 20 ppm kiʻekiʻe.
1.0 g e like me ka ho'āʻo C. E hoʻomākaukau i ka haʻina kuhikuhi me ka hoʻohana ʻana i 2 mL o ka solution maʻamau kepau (10 ppm Pb) R.
Nalo ma ka maloʻo ʻana (2.2.32): 1.0 pākēneka kiʻekiʻe, i hoʻoholo ʻia ma 1.000 g ma ka hoʻomaloʻo ʻana i ka umu ma 105 ℃.
ʻO ka lehu Sulfated (2.4.14): ʻoi aku ka nui o 0.1 pākēneka, i hoʻoholo ʻia ma 1.0 g.
HANA
E hoʻoheheʻe i 0.350 g i 50 mL o ka ethanol (96 pākēneka) R, i hoʻokaʻawale mua ʻia i 0.2 mL o ka solution phenolphthalein R. E hoʻohui i 50 mL wai R a e hoʻoemi me 0.1 M sodium hydroxide a loaʻa kahi waihoʻoluʻu poni.
1 mL o 0.1 M sodium hydroxide ua like ia me 39.26 mg o C24H40O4.
NA mea haumia
ʻO nā haumia i kuhikuhi ʻia: A, C.
ʻO nā mea haumia ʻē aʻe i ʻike ʻia (e ʻike ʻia nā mea ma lalo nei, inā aia ma kahi pae kūpono, e hoʻokahi a i ʻole nā ​​​​mea ʻē aʻe o nā hoʻokolohua ma ka monograph. no ka hoʻohana lāʻau (2034). No laila ʻaʻole pono e ʻike i kēia mau haumia no ka hōʻike ʻana i ka hoʻokō.
Ka mālama ʻana i nā haumia i loko o nā mea no ka hoʻohana lāʻau lapaʻau): B, D, E, F, G, H, I.
A. 3α,7α-dihydroxy-5β-cholan-24-oic acid (chenodeoxycholic acid),
ʻO ka B. 3α,7α,12α-trihydroxy-5β-cholan-24-oic acid (kolic acid),
C. 3α-hydroxy-5β-cholan-24-oic acid (lichocholic acid),
D. 3α,7β,12α-trihydroxy-5β-cholan-24-oic acid (ursocholic acid),
E. 3α,12α-dihydroxy-5β-cholan-24-oic acid (ʻakika deoxycholic),
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.