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

Chenodeoxycholic Acid
C24H40O4: 392.57
3a,7a-Dihydroxy-5b-cholan-24-oic acid [474-25-9]
Chenodeoxycholic Acid, when dried, contains not less than 98.0z and not more than 101.0% of C24H40O4.
Description Chenodeoxycholic Acid occurs as white, crystals, crystalline powder or powder.
It is freely soluble in methanol and in ethanol (99.5), soluble in acetone, and practically insoluble in water.
Identification Determine the infrared absorption spectrum of Chenodeoxycholic Acid, previously dried, as directed in the potassium bromide disk method under Infrared Spectrophotometry <2.25>, and compare the spectrum with the Reference Spectrum: both spectra exhibit similar intensities of absorption at the same wave numbers.
Optical rotation <2.49> [a]20D : +11.0 °~ +13.0° (after drying, 0.4 g, ethanol (99.5), 20 mL, 100 mm).
Melting point <2.60> 164~169℃
Purity (1) Chloride <1.03>-Dissolve 0.36 g of Chenodeoxycholic Acid in 30 mL of methanol, add 10 mL of dilute nitric acid and water to make 50 mL, and perform the test with this solution. Prepare the control solution as follows: To 1.0 mL of 0.01 mol/L hydrochloric acid VS add 30 mL of methanol, 10 mL of dilute nitric acid and water to make 50 mL (not more than 0.1%).
(2) Heavy metals <1.07>-Proceed with 1.0 g of Chenodeoxycholic Acid according to Method 4, and perform the test. Prepare the control solution with 2.0 mL of Standard Lead Solution (not more than 20 ppm).
(3) Barium-To 2.0 g of Chenodeoxycholic Acid add 100 mL of water, and boil for 2 minutes. To this solution add 2 mL of hydrochloric acid, boil for 2 minutes, filter after cooling, and wash the filter with water until to get 100 mL of the filtrate. To 10 mL of the filtrate add 1 mL of dilute sulfuric acid: no turbidity is appeared.
(4) Related substances-Dissolve 0.20 g of Chenodeoxycholic Acid in a mixture of acetone and water (9:1) to make exactly 10 mL, and use this solution as the sample solution. Separately, dissolve 10 mg of lithocholic acid for thin-layer chromatography in the mixture of acetone and water (9:1) to make exactly 10 mL. Pipet 2 mL of this solution, add the mixture of acetone and water (9:1) to make exactly 100 mL, and use this solution as the standard solution (1). Separately, dissolve 10 mg of ursodeoxycholic acid in the mixture of acetone and water (9:1) to make exactly 100 mL, and use this solution as the standard solution (2). Separately, dissolve 10 mg of cholic acid for thin-layer chromatography in the mixture of acetone and water (9:1) to make exactly 100 mL, and use this solution as the standard solution (3). Pipet 1 mL of the sample solution, and add the mixture of acetone and water (9:1) to make exactly 20 mL. Pipet 0.5 mL, 1 mL, 2 mL, 3 mL and 5 mL of this solution, add the mixture of acetone and water (1) to each of them to make exactly 50 mL, and designate these solutions as standard solution A, standard solution B, standard solution C, standard solution D and standard solution E, respectively. Perform the test with these solutions as directed under Thin-layer Chromatography <2.03>. Spot 5 mL each of the sample solution, standard solutions (1), (2), (3) and standard solutions A, B, C, D and E on a plate of silica gel for thin-layer chromatography. Develop the plate with a mixture of 4-methyl-2-pentanone, toluene and formic acid (16:6:1) to a distance of about 15 cm, airdry the plate, and further dry at 1209C for 30 minutes. Immediately, spray evenly a solution of phosphomolybdic acid n-hydrate in ethanol (95) (1 in 5) on the plate, and heat at 120℃ for 2 to 3 minutes: the spot corresponding to the spot with the standard solution (1) is not more intense than the spot with the standard solution (1), the spot corresponding to the spot with the standard solution (2) is not more intense than the spot with the standard solution (2), and the spot corresponding to the spot with the standard solution (3) is not more intense than the spot with the standard solution
(3). As compared to the spots with the standard solutions A, B, C, D and E, the spots other than the principal spot and other than the spots mentioned above are not more intense than the spot with the standard solution E, and the total amount of them is not more than 1.5%.
Loss on drying <2.41> Not more than 1.5%(1 g, 105℃,3 hours).
Residue on ignition <2.44> Not more than 0.1% (1 g).
Assay Weigh accurately about 0.5 g of Chenodeoxycholic Acid, previously dried, dissolve in 40 mL of ethanol (95) and 20 mL of water, and titrate <2.50> with 0.1 mol/L sodium hydroxide VS (potentiometric titration). Perform a blank determination in the same manner, and make any necessary correction.
Each mL of 0.1 mol/L sodium hydroxide VS ＝ 39.26 mg of C24H40O4
Containers and storage Containers-Tight containers.