Ursodeoxycholic Acid Capsules
Action and use
Bile acid; treatment of gallstones.
Definition
Ursodeoxycholic Acid Capsules contain Ursodeoxycholic Acid.
Content of ursodeoxycholic acid, C24H40O4
95.0 to 105.0% of the stated amount.
Identification
Tests
Dissolution
Comply with the requirements for Monographs of the British Pharmacopoeia in the dissolution test for tablets and capsules, Appendix XII B1.
Carry out the method for liquid chromatography, Appendix III D, using the following solutions.
The chromatographic conditions described under Assay may be used with an injection volume of 250 µL.
Calculate the total content of ursodeoxycholic acid, C24H40O4, in the medium from the chromatograms obtained and using the declared content of C24H40O4 in ursodeoxycholic acid BPCRS.
Related substances
Carry out the method for liquid chromatography, Appendix III D, using the following solutions in Solvent A.
25 volumes of acetonitrile, 34 volumes of methanol and 47 volumes of a solution prepared by dissolving 0.8 g of sodium dihydrogen orthophosphate dihydrate in 1000 mL of water and adjusting the pH to 3.0 with orthophosphoric acid.
When the chromatograms are recorded under the prescribed conditions the retention time relative to ursodeoxycholic acid (retention time, about 5 minutes) are: 7-ketolithocholic acid (impurity F), about 1.3 and chenodeoxycholic acid, about 2.8.
The test is not valid unless, in the chromatogram obtained with solution (3), the resolution between the peaks due to ursodeoxycholic acid and 7-ketolithocholic acid is at least 2.0.
In the chromatogram obtained with solution (1):
the area of any peaks corresponding to chenodeoxycholic acid is not greater than 3 times the area of the principal peak in the chromatogram obtained with solution (2) (1.5%);
the area of any other secondary peak is not greater than the area of the principal peak in the chromatogram obtained with solution (2) (0.5%);
the sum of the areas of any secondary peak is not greater than 4.2 times the area of the principal peak in the chromatogram obtained with solution (2) (2.1%).
Disregard any peak with an area less than the area of the principal peak in the chromatogram obtained with solution (4) (0.05%).
Assay
Weigh a quantity of the mixed contents of 20 capsules. Carry out the method for liquid chromatography, Appendix III D, using the following solutions.
To 40 volumes of acetonitrile R1 add 60 volumes of 0.001m potassium dihydrogen orthophosphate, allow to equilibrate to room temperature, adjust to pH 2.0 with orthophosphoric acid (85%) and filter.
Calculate the content of C24H40O4 using the declared content of C24H40O4 in ursodeoxycholic acid BPCRS.
Impurities
The impurities limited by the requirements of this monograph include A, D, E and F listed under Ursodeoxycholic Acid and the following: