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, uma yomisiwe, iqukethe okungaphansi kuka-98.0z futhi hhayi ngaphezu kuka-101.0% we-C24H40O4.
I-Chenodeoxycholic Acid yenzeka imhlophe, ikristalu, i-crystalline powder noma impushana.
Incibilika ngokukhululeka ku-methanol naku-ethanol (99.5), inyibilika ku-acetone, futhi ayincibiliki emanzini.
Ukuhlonza Thola i-spectrum yokumuncwa kwe-infrared ye-Chenodeoxycholic Acid, omiswe ngaphambilini, njengoba kuqondiswe endleleni yediski ye-potassium bromide ngaphansi kwe-Infrared Spectrophotometry <2.25>, futhi uqhathanise i-spectrum ne-Reference Spectrum: yomibili i-spectra ibonisa amandla afanayo okumunca ezinombolweni zamagagasi afanayo.
Ukuzungezisa okubonakalayo <2.49> [a]20D : +11.0 °~ +13.0° (ngemuva kokumiswa, 0.4 g, i-ethanol (99.5), 20 mL, 100 mm).
Iphoyinti lokuncibilika <2.60> 164~169℃
Ukuhlanzeka (1) I-Chloride <1.03>-Chaza u-0.36 g we-Chenodeoxycholic Acid ku-30 ​​mL we-methanol, engeza u-10 mL we-nitric acid ehlanjululwe kanye namanzi ukuze wenze u-50 mL, futhi wenze ukuhlolwa ngalesi sixazululo.Lungiselela ikhambi lokulawula ngale ndlela elandelayo: Ku-1.0 mL ka-0.01 mol/L hydrochloric acid VS engeza u-30 mL we-methanol, u-10 mL we-nitric acid ehlanjululwe namanzi ukuze wenze u-50 mL (hhayi ngaphezu kuka-0.1%).
(2) Izinsimbi ezisindayo <1.07>-Qhubeka no-1.0 g we-Chenodeoxycholic Acid ngokweNdlela 4, futhi wenze ukuhlolwa.Lungiselela isixazululo sokulawula ngo-2.0 mL Wesixazululo Esijwayelekile Sokuhola (hhayi ngaphezu kuka-20 ppm).
(3) I-Barium-Kuya ku-2.0 g we-Chenodeoxycholic Acid engeza u-100 mL wamanzi, bese ubilisa imizuzu emi-2.Kulesi sixazululo faka u-2 mL we-hydrochloric acid, ubilise imizuzu emi-2, hlunga emva kokupholisa, futhi ugeze isisefo ngamanzi kuze kube yilapho uthola u-100 mL we-filtrate.Ku-10 ml we-filtrate engeza i-1 mL ye-sulfuric acid ehlanjululwe: akukho ukuxubha okubonakalayo.
(4) Izinto ezihlobene-Chaza u-0.20 g we-Chenodeoxycholic Acid enhlanganisweni ye-acetone namanzi (9:1) ukuze wenze u-10 mL ngqo, futhi usebenzise lesi sixazululo njengesampula yesixazululo.Ngokwehlukana, ncibilikisa u-10 mg we-lithocholic acid we-chromatography yongqimba oluncane engxube ye-acetone namanzi (9:1) ukwenza u-10 mL ngqo.Pipetha u-2 mL walesi sixazululo, engeza ingxube ye-acetone namanzi (9:1) ukuze wenze u-100 mL ngqo, bese usebenzisa lesi sixazululo njengesixazululo esijwayelekile (1).Ngokwehlukana, ncibilikisa u-10 mg we-ursodeoxycholic acid enhlanganisweni ye-acetone namanzi (9:1) ukuze wenze u-100 mL ngqo, bese usebenzisa lesi sixazululo njengesixazululo esijwayelekile (2).Ngokwehlukana, ncibilikisa u-10 mg we-cholic acid we-chromatography yongqimba oluncane engxube ye-acetone namanzi (9:1) ukwenza u-100 mL ngqo, bese usebenzisa lesi sixazululo njengesixazululo esijwayelekile (3).Ipayipi elingu-1 mL lesixazululo sesampula, bese wengeza ingxube ye-acetone namanzi (9:1) ukwenza u-20 mL ngqo.Ipayipi elingu-0.5 mL, 1 mL, 2 mL, 3 mL no-5 mL walesi sixazululo, engeza ingxube ye-acetone namanzi (1) kumuntu ngamunye ukwenza u-50 mL ncamashi, bese ubeka lezi zixazululo njengesixazululo esijwayelekile A, isixazululo esijwayelekile. B, isixazululo esijwayelekile C, isixazululo esijwayelekile D kanye nesixazululo esijwayelekile esingu-E, ngokulandelana.Yenza ukuhlolwa ngalezi zixazululo njengoba kuqondiswe ngaphansi kwe-Thin-layer Chromatography<2.03>.Faka i-5 ml ngayinye yesixazululo sesampula, izixazululo ezijwayelekile (1), (2), (3) nezixazululo ezijwayelekile A, B, C, D kanye no-E epuletini lejeli yesilika yechromatography yongqimba oluncane.Yakha ipuleti ngengxube ye-4-methyl-2-pentanone, i-toluene ne-formic acid (16:6:1) ukuya ebangeni elingaba ngu-15 cm, yomisa ipuleti emoyeni, bese uqhubeka wome ku-1209C imizuzu engu-30.Ngokushesha, fafaza ngokulinganayo isixazululo se-phosphomolybdic acid n-hydrate ku-ethanol (95) (1 ku-5) epuletini, bese ushisa ku-120℃ imizuzu emi-2 kuya kwemi-3: indawo ehambisana nendawo enesixazululo esijwayelekile (1) alishubi kakhulu kunendawo enesixazululo esijwayelekile (1), indawo ehambisana nendawo enesixazululo esijwayelekile (2) ayishubi kakhulu kunendawo enesixazululo esijwayelekile (2), kanye nebala elihambisana nendawo. ngesisombululo esijwayelekile (3) alishubi ngaphezu kwendawo enesixazululo esijwayelekile
(3).Uma kuqhathaniswa namachashaza anezixazululo ezijwayelekile A, B, C, D kanye no-E, amachashaza ngaphandle kwendawo eyinhloko namanye ngaphandle kwamachashazi ashiwo ngenhla awashubi kakhulu kunendawo enesixazululo esijwayelekile esingu-E, kanye nenani eliphelele. kubo akukho ngaphezu kwe-1.5%.
Ukulahlekelwa ekumisweni <2.41> Hhayi ngaphezulu kuka-1.5%(1 g, 105℃,3 amahora).
Insalela ekuthungeleni <2.44> Ayidluli ku-0.1% (1 g).
I-Assay Kala ngokunembile cishe u-0.5 g we-Chenodeoxycholic Acid, omisiwe ngaphambilini, ncibilika ku-40 mL we-ethanol (95) kanye no-20 mL wamanzi, kanye ne-titrate <2.50> nge-0.1 mol/L sodium hydroxide VS (potentiometric titration).Yenza isinqumo esingenalutho ngendlela efanayo, futhi wenze noma yikuphi ukulungisa okudingekayo.
I-mL ngayinye ka-0.1 mol/L i-sodium hydroxide VS ＝ 39.26 mg ye-C24H40O4
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