Boscolo Oriana
University of Buenos Aires, Argentina
Title: Development of HPLC-UV/MS-MS methods applied to the quality control of Ursodeoxycholic acid in oral liquid pediatric formulations and raw material
Biography
Biography: Boscolo Oriana
Abstract
Ursodeoxycholic acid (UDCA), is a bile acid used to dissolve gallstones and for the treatment of hepatobiliary diseases. It is the only drug approved by the FDA for the treatment of primary biliary cirrhosis.
In UDCA raw material other bile acid may be present as impurities. Some of them, like lithocholic acid (LCA) is highly toxic, and others are associated with several side effects such as chenodeoxicholic acid (CDCA). USP Pharmacopeia describes the determination of CDCA and LCA by TLC, where each impurity limit should be not more than 1.5% and 0.02% respectively.
The aim of this work was to developed, and validated an analytical method by HPLC-UV for the determination of UDCA in oral liquid pharmaceutical formulations for pediatrics administration. Also, determined the impurities present in the raw material by HPLC / MS-MS.
HPLC-UV system was applied a C18 Symmetry column (150 mm x 4,6 mm id, particle size 3,5 µm, Waters), mobile phase ACN: H2O pH 3 (48:52), column temperature 40° C, flow rate 1 mL/min, injection volume 100 µL and detection UV 200 nm.
In the determination of impurities the chromatography method was carried isocratically at 25° C, using a column C18 Symmetry, mobile phase methanol:acetonitrile:10mM ammonium acetate buffer (40:40:20), flow rate 0.4 mL/min. Negative polarity and SRM mode were set for MS detection. The parameters optimized were: voltage; sheat gas pressure and tubulence offset.
Both methods were validated in terms of specificity, LOD, LOQ, linearity, precision, accuracy and robustness.
The developed methods meet specifications and are suitable for quality control.