I-Chenodeoxycholic Acid (CDCA) CAS 474-25-9 Assay ≥98% (Dry Basic)

I-Chenodeoxycholic Acid
C24H40O4: 392.57
3a,7a-Dihydroxy-5b-cholan-24-oic acid [474-25-9]
I-Chenodeoxycholic Acid, xa yomisiwe, iqulethe ngaphantsi kwe-98.0z kwaye ingabi ngaphezu kwe-101.0% ye-C24H40O4.
Inkcazo I-Chenodeoxycholic Acid yenzeka njengomhlophe, iikristale, umgubo wekristale okanye umgubo.
Inyibilika ngokukhululekileyo kwi-methanol nakwi-ethanol (99.5), inyibilika kwi-acetone, kwaye ayinyibiliki ngokuthe ngqo emanzini.
Ukuchonga Ukumisela i-infrared absorption spectrum ye-Chenodeoxycholic Acid, eyomisiwe ngaphambili, njengoko iqondiswe kwindlela ye-potassium bromide disk phantsi kwe-Infrared Spectrophotometry <2.25>, kwaye uthelekise i-spectrum kunye ne-Reference Spectrum: zombini i-spectra ibonisa ubunzima obufanayo bokufunxa kwiinombolo zamaza afanayo.
Ukujikeleza kwe-Optical <2.49> [a] 20D : +11.0 °~ +13.0 ° (emva kokumisa, 0.4 g, ethanol (99.5), 20 mL, 100 mm).
Indawo yokunyibilika <2.60> 164~169℃
Ukucoceka (1) I-Chloride <1.03>-Dissolve 0.36 g ye-Chenodeoxycholic Acid kwi-30 mL ye-methanol, yongeza i-10 mL ye-dilute nitric acid kunye namanzi ukwenza i-50 mL, kwaye wenze uvavanyo ngesi sisombululo.Lungiselela isisombululo solawulo ngolu hlobo lulandelayo: Kwi-1.0 mL ye-0.01 mol / L i-hydrochloric acid VS yongeza i-30 mL ye-methanol, i-10 mL ye-dilute nitric acid kunye namanzi ukwenza i-50 mL (kungekho ngaphezu kwe-0.1%).
(2) Izinyithi ezinzima <1.07>-Qhubeka kunye ne-1.0 g ye-Chenodeoxycholic Acid ngokweNdlela ye-4, kwaye wenze uvavanyo.Lungiselela isisombululo solawulo kunye ne-2.0 mL yeSisombululo esiPhambili seNkokheli (kungekho ngaphezu kwe-20 ppm).
(3) I-Barium-Ukuya kwi-2.0 g ye-Chenodeoxycholic Acid yongeza i-100 mL yamanzi, kwaye ubilise imizuzu emi-2.Kwesi sisombululo yongeza i-2 mL ye-hydrochloric acid, ubilise imizuzu emi-2, ukucoca emva kokupholisa, kwaye uhlambe isihluzo ngamanzi de ufumane i-100 mL ye-filtrate.Kwi-10 mL yefiltrate yongeza i-1 mL ye-sulfuric acid exutywe: akukho ntlupheko ibonakala.
(4) Izinto ezihambelanayo-Dibanisa i-0.20 g ye-Chenodeoxycholic Acid kumxube we-acetone kunye namanzi (9: 1) ukwenza ngokuthe ngqo i-10 mL, kwaye usebenzise esi sisombululo njengesisombululo sesampuli.Ngokwahlukileyo, nyibilikisa i-10 mg ye-lithocholic acid kwi-chromatography ebhityileyo kumxube we-acetone namanzi (9: 1) ukwenza i-10 mL ngqo.Umbhobho we-2 mL yesi sisombululo, yongeza umxube we-acetone namanzi (9: 1) ukwenza i-100 mL ngqo, kwaye usebenzise esi sisombululo njengesisombululo esiqhelekileyo (1).Ngokwahlukileyo, chitha i-10 mg ye-ursodeoxycholic acid kumxube we-acetone kunye namanzi (9: 1) ukwenza i-100 mL ngqo, kwaye usebenzise esi sisombululo njengesisombululo esiqhelekileyo (2).Ngokwahlukileyo, nyibilikisa i-10 mg ye-cholic acid ye-chromatography ebhityileyo kumxube we-acetone namanzi (9: 1) ukwenza i-100 mL ngqo, kwaye usebenzise esi sisombululo njengesisombululo esiqhelekileyo (3).Umbhobho we-1 mL yesisombululo sesampuli, kwaye wongeze umxube we-acetone namanzi (9: 1) ukwenza i-20 mL ngqo.Umbhobho 0.5 mL, 1 mL, 2 mL, 3 mL kunye 5 mL yale isisombululo, yongeza umxube acetone namanzi (1) ukuze ngamnye kubo wenze ngokuchanekileyo 50 mL, kwaye ukhethe ezi zisombululo njengesisombululo A, isisombululo eqhelekileyo. B, isisombululo esiqhelekileyo C, isisombululo esisemgangathweni D kunye nesisombululo esiqhelekileyo E, ngokulandelanayo.Yenza uvavanyo ngezi zisombululo njengoko uyalela phantsi kweThin-layer Chromatography<2.03>.I-Spot 5 mL nganye yesisombululo sesampuli, izisombululo eziqhelekileyo (1), (2), (3) kunye nezisombululo eziqhelekileyo A, B, C, D kunye no-E kwi-plate ye-silica gel ye-chromatography encinci.Phuhlisa ipleyiti kunye nomxube we-4-methyl-2-pentanone, i-toluene kunye ne-asidi ye-formic (16: 6: 1) ukuya kumgama omalunga ne-15 cm, i-airdry plate, kwaye yome ngakumbi kwi-1209C imizuzu engama-30.Kwangoko, fafaza ngokulinganayo isisombululo se-phosphomolybdic acid n-hydrate kwi-ethanol (95) (1 ku-5) epleyitini, kunye nobushushu kwi-120 ℃ imizuzu emi-2 ukuya kwemi-3: indawo ehambelana nendawo enesisombululo esisemgangathweni (1) aliqini kakhulu kunebala elinesisombululo esisemgangathweni (1), indawo ehambelana nebala elinesisombululo esisemgangathweni (2) alibi kakhulu kunebala elinesisombululo esisemgangathweni (2), kunye nebala elihambelana nebala. kunye nesisombululo esisemgangathweni (3) asinamandla ngaphezu kwendawo enesisombululo esisemgangathweni
(3).Xa kuthelekiswa namabala anezisombululo ezisemgangathweni A, B, C, D kunye no-E, amabala angaphandle kwebala eliphambili kwaye ngaphandle kwamabala akhankanywe apha ngasentla awabi kakhulu kunendawo enesisombululo esiqhelekileyo E, kunye nesixa esipheleleyo. kubo akukho ngaphezu kwe-1.5%.
Ilahleko ekomisweni <2.41> Akukho ngaphezu kwe-1.5% (1 g, 105℃,3 iiyure).
Intsalela ekutshisweni <2.44> Akukho ngaphezu kwe-0.1% (1 g).
I-Assay Ukulinganisa ngokuchanekileyo malunga ne-0.5 g ye-Chenodeoxycholic Acid, eyomisiwe ngaphambili, inyibilika kwi-40 mL ye-ethanol (95) kunye ne-20 mL yamanzi, kunye ne-titrate <2.50> kunye ne-0.1 mol / L i-sodium hydroxide VS (i-potentiometric titration).Yenza ukuzimisela okungenanto ngendlela efanayo, kwaye wenze naluphi na ulungiso oluyimfuneko.
I-mL nganye ye-0.1 mol / L i-sodium hydroxide VS ＝ 39.26 mg ye-C24H40O4
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