Dissolution testing of ursodeoxycholic acid suspension using SPE as sample preparation

BOSCOLO O.; FLOR S.; DOBRECKY C.; TRIPODI V.; LUCANGIOLI S.

RPS Pharmacy and Pharmacology Reports

Oxford

Lugar: Londres; Año: 2022

Objective: To develop and validate an analytical method by HPLC-UV for the quantification of ursodeoxycholic acid suspension in a dissolution test followed by a solid phase extraction to circumvent the interference of sodium lauryl sulfate present in the dissolution medium. Methods: USP apparatus 2. The dissolution medium was 900 mL of an aqueous solution of 0.05 M phosphate buffer (pH 8.4) with 2% sodium lauryl sulfate. The samples were filtered and cleaned by solid phase extraction with 500 mg/3mL C18 cartridges. The analytical method was validated for specificity, linearity, LOD, LOQ accuracy and precision. Chromatographic conditions, Symmetry-C18 column (150 mm x 4.6 mm, id; 5 µm particle size), 40 ˚C, 100 µL injection volume, and UV detection at 200 nm. The flow rate was 1 mL/min using acetonitrile-phosphoric acid (pH 3.0, 0.15 mM) (48:52). Key Findings: Solid phase extraction provided an efficient and selective extraction of ursodeoxycholic acid from the dissolution medium. On the other hand, the solid phase extraction washing step allowed the elimination of sodium lauryl sulfate. The ursodeoxycholic acid method optimization and validation were accomplished with no less than 80% in 30 minutes.Conclusion: The developed analytical method was simple and adequate for the analysis of ursodeoxycholic acid suspension samples which met the USP specifications for dissolution test.