Abstract
1-(2,5-Dihydroxyphenyl)-2-bromoethanone (2,5-DBE) has been used as an electroactive labelling reagent for high performance liquid chromatographic (HPLC) analysis of chenodeoxycholic acid impurity in pharmaceutical formulations of ursodeoxycholic acid.
The preparation of this reagent has been performed in a single step by bromination of 2,5-dihydroxyacetophenone (2,5-DAP), with remarkable improvement as regards the synthesis previously reported. Several experiments have been performed in order to give maximum conversion of the bile acids to their electroactive esters.
The determination of the derivatized compounds has been carried out on an Adsorbosphere column with a methanol-acetonitrile-acetate buffer eluent and detected by a porous graphite electrode set at an oxidation potential of + 0.6 V. The high sensitivity and specificity shown by this novel method allows the determination of low concentrations of the cited impurity in capsule and tablet formulations containing the above therapeutic agent.