Development and Validation of RP-HPLC Method for Determination of Thermal Degradation Impurity in Macrolide Immunosuppressant Substance and Drug Product

Abstract

Abstract

The present study describes a simple and stability-indicating reverse phase high-performance liquid chromatography (RP-HPLC) method for the quantification of the thermal degradation impurities of Tacrolimus (FK506) namely Ally ester rearrangement impurity (Impurity R) in Tacrolimus capsules and drug substances. Successful separation of impurity R from Tacrolimus, its other related substances and its tautomers were achieved on a Zorbax XDB C8 (150×4.6 mm, 5 μm) and detector of UV at 210 nm, 2.0 ml/min as a flow rate, and 20 μl as an injection volume. For the RP- HPLC method, 0.1% Trifluroacetic acid in water and Acetonitrile was used as a binary linear gradient and the column temperature was 55° C. Percentage recovery obtained in the range of 96.8%–101.2% and the method is linear for impurity R for specified concentration range with coefficient of variation (r) not less than 0.99. acid, base, oxidation, thermal and photolytic degradation have been carried in drug substance and drug product. The proposed RP-HPLC method was found to be specific, linear, precise, accurate and robust.

Keywords: Tacrolimus, FK506, Thermal degradation impurity, Allyl ester rearrangement impurity, RP-HPLC

Cite this Article

J. Balaji, C. Nisha Shri. Development and Validation of RP-HPLC Method for Determination of Thermal Degradation Impurity in Tacrolimus Drug Substance and Drug Product. Research & Reviews: A Journal of Drug Formulation, Development and Production. 2016; 3(1): 14–19p.