A Validated Stability-Indicating UPLC Method for the Determination of Impurities in Maraviroc

Abstract

Maraviroc is an antiretroviral drug in the CCR5 receptor antagonist class, which is used in the treatment of HIV. Maraviroc has six impurities. A novel, stability-indicating reversed-phase ultra-performance liquid chromatography (RP-UPLC) method has been developed for the quantitative determination of maraviroc in active pharmaceutical ingredients, along with its six impurities. The method is applicable to the quantification of related compounds and the assay of maraviroc. Efficient chromatographic separation was achieved on a BEH Shield RP-18 column, 100 × 2.1 mm, 1.7 µm, in isocratic elution within 12 min. The mobile phase was 0.01 M ammonium acetate in water and acetonitrile in the ratio of 63:37 (v/v). The flow rate was 0.4 mL/min, column oven temperature was maintained at 40°C and detection was conducted at 210 nm. Stress degradation conditions were established for maraviroc by subjecting it to acid, base, oxidation, water, humidity, thermal and photolysis stress. The stress samples were assayed against a qualified reference standard and the mass balance was close to 98.0%. The developed UPLC method was validated according to the current International Conference on Harmonization guidelines for specificity, detection limit, quantitation limit, linearity, accuracy, precision, intermediate precision and robustness. The resolution between maraviroc and its six impurities was greater than 3.0. A regression analysis showed that the correlation coefficient value was greater than 0.999 for maraviroc and its six impurities.