Aminoglycosides are broad-spectrum antibiotics; they exhibit specific ototoxicity and nephrotoxicity and can cause respiratory depression up to the development of muscular blockade. Therefore, therapeutic drug monitoring is required in the majority of cases [1].Practical demands for monitoring the main component concentration in pharmaceutical dosage forms and the necessity of determining aminoglycosides in biological fluids stimulate research into the development of rapid analytical methods. Microbiological [2], spectroscopic [3][4][5], and chromatographic [6,7] techniques have been used for determining aminoglycoside antibiotics, whereas electrochemical techniques have been rarely used [8].This work is devoted to a study of the electroanalytical properties of membranes sensitive to aminoglycoside antibiotics and the development of procedures for the rapid potentiometric determination of gentamycin and kanamycin in biological fluids and pharmaceuticals using ion-selective electrodes (ISEs). EXPERIMENTAL Gentamycin (Gen) sulfate (4% solution in ampoules) and kanamycin (Kan) sulfate (in vials) were used. Aqueous stock solutions (1.0 × 10 -2 M) were prepared using accurately weighed portions of the preparations. Solutions with 1.0 × 10 -2 -1.0 × 10 -5 M concentrations were prepared by successive dilution. Table 1 summarizes the names, formulas, and characteristics of the substances used in this study. Sodium tetraphenylborate (TPB) and the Acid Chrome Black Special (ABS) azo dye were used as precipitant anions for preparing the active components of membranes.The gentamycin-tetraphenylborate ionophore was prepared by mixing sodium tetraphenylborate and gentamycin sulfate solutions in equimolar amounts ( c Gen = c TPB = 1.0 × 10 -2 M; V Gen = V TPB = 20.0 mL) at room temperature. The Gen-ABS and Kan-ABS ion pairs were prepared by mixing solutions of the antibiotics ( c = 1.0 × 10 -2 ) with an alcoholic solution of ABS ( c = 2%) at the ratios Gen : ABS = 1 : 5 and Kan : ABS = 1 : 4. The precipitates were allowed to stand for a day, washed with distilled water by decantation, filtered off, and dried in a drying oven at 60-70 ° C.We studied liquid electrodes with homemade plasticized PVC membranes ( c ionophore = 0.01 mol/(kg dibutyl phthalate (DBP)); the PVC-DBP weight ratio was 1 : 3). The internal solution contained a 1 : 1 mixture of a 1.0 × 10 -3 M antibiotic solution and a 1.0 × 10 -3 M Na 2 SO 4 solution. The emf of the circuit Ag, AgCl | internal solution | membrane | test solution | KCl sat | AgCl, Ag was measured to within ± 0.001 V using an I-130 potentiometer; an EMV-1MZ silver-silver chloride electrode served as a reference electrode.The thermoanalytical study of the ionophores was performed on an OD-103 derivatograph, which allowed us to perform programmed heating from room temperature to 1000 ° C in air. Temperature was measured with a Pt/Pt-Rh thermocouple; calcined aluminum oxide served as a reference substance.Abstract -Ion-selective electrodes with plasticized membranes based on ion pairs of gentamyci...