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This investigation used Mass Spectrometry as the main technique for the elucidation of organic compounds structures with cationic properties synthesized in our research group. Our main objective was the optimization of the synthesis of two free amidine cationic compounds and two N-substituted and the synthesis of one phosphonium salt as possible antiparasitic compounds. For the synthesis of amidine compounds, different types of commercially available nitriles were used, which by coupling with nitrogen compounds, in our case ammonium chloride and p-methoxyaniline, resulted in the desired amidines. In the case of phosphonium salt, the reaction was performed by a nucleophilic attack to 2-bromoethanol resulting in the desired product. Structural elucidation of the synthetized compounds was performed using ionization by electrospray in positive mode. We used a gradient in the fragmentation energy from 15 V to 30 V, making a gradual increase of every 5V, resulting in the confirmation of the structures of the synthesized compounds.