In the present paper, the microwave synthesis of MOF-199 and its application as an electrode modifier for the simultaneous voltammetric determination of paracetamol (PAR) and caffeine (CAF) were demonstrated. The obtained materials were characterised by X-ray diffraction, a scanning electron microscope (SEM), nitrogen adsorption/desorption isotherms and thermal gravity. The microwave (MW) synthesis of MOF-199 has been compared to its conventional hydrothermal synthesis. It is found that by using the MW synthesis, MOF-199 can be obtained in a much shorter synthesis time with improved yield and textural properties. The electrode modified by MOF-199 was used in order to develop an electroanalytical method that can be used to simultaneously quantify PAR and CAF. The kinetic parameters of the electrode reaction process were also investigated. This proposed method was successfully employed for the simultaneous detection of PAR and CAF in pharmaceutical formulations using the standard addition method and the obtained results compared with the results determined by means of HPLC were found to be statistically similar.