Review of the article „Development and validation of novel UPLC-MS/MS method for the analysis of macitenan in pharmaceutical formulations“

Abstract

Macitentan is an endothelin receptor antagonist drug used in the treatment of pulmonary arterial hypertension. A new, sensitive, simple, accurate and rapid UPLC-MS/MS method is developed and validated for determination of macitentan in pharmaceutical formulations. Macitentan and bosentan which is used as internal standard (IS) were detected using APCI in positive ion, multiple reaction monitoring mode by monitoring the mass transitions (precursor to product) m/z 589.1→203.3 and 552.6→311.5, respectively. Chromatographic separation was carried out on reverse phase C18 column (5 μm, 4.6 * 150 mm). It was used water containing 0,2 % acetic acid: acetonitrile (90:10, V/V) in isocratic elution as mobile phase. The system was optimized as injection volume of 10 μl, column temperature of 35 °C and flow rate of 1 mL/min. Retention times were 1.97 min. for macitentan and 1.72 min. for IS. The calibration curve with high correlation coefficient (0.9997) was linear range 0.5-500 ng mL-1. The LLOQ and average recovery values were determined as 0.5 ng mL-1 and 99.7 %, respectively. The developed novel method has been successfully applied for determination of macitentan in pure form and pharmaceutical formulations.