A new analytical method for the determination of gallamine triethiodide (Flaxedil ; 1) and pancuronium bromide (Pavulon ; 2), two muscle relaxants used in surgical operations and in pain relief, has been developed. Our approach relies on rapid, precise, and sensitive potentiometric sensors based on modified-carbon-paste ionselective electrodes (CP-ISEs). Linear calibration graphs in the working ranges of ca. 4.5 ± 892 and 7.3 ± 733 mg/ ml (in H 2 O, pH 7.0, T 258) were established for 1 and 2, respectively; and Nernst slopes corresponding to threeor two-electrons transfers, respectively, were obtained. The method works best in a pH range of 7 ± 9. Average relative errors of 2.12 and 2.14%, with average standard deviations of 1.98 ± 2.47 and 2.64 ± 3.45, respectively, were obtained for urine samples of 1 and 2. The corresponding relative errors for the pharmaceutical samples were 1.59 and 1.64%, with standard deviations of 0.54 ± 1.34 and 0.52 ± 1.67, respectively. Statistical Student and F tests were applied to the data, and satisfactory results were obtained.1. Introduction. ± The two drugs gallamine triethiodide (Flaxedil ; 1) and pancuronium bromide (Pavulon ; 2) 2 ) are muscle relaxants used in surgical operations and for relief pain. These compounds possess only weak chromophores, which limits their detection by classical HPLC analysis based on UV and refractive-index measurements [1] [2]. Reported HPLC methods based on mass-spectrometric and fluorescence detection with pre-or post-column derivatizations are costly and complicated. Therefore, reliable, accurate, and economical analytical methods are still needed for analysis. The aim of this investigation was to develop new, rapid, sensitive, and reliable carbon-paste ion-selective electrodes (CP-ISEs) for the determination of 1 and 2 in pharmaceutical and urine samples.Gallamine triethiodide (1) and pancuronium bromide (2) are colorless, hygroscopic, crystalline powders freely soluble in H 2 O and EtOH, and are typically 98 ± 100% pure. They have to be freshly prepared and stored in air-tight containers protected from light. Almost 100% of intravenously administered gallamine (40 ± 120 mg) is excreted unchanged in urine within 24 ± 30 h [3]. In contrast, only ca. 25% of pancuronium bromide (40 ± 100 mg/kg body weight) is excreted unchanged in urine, together with 15% of 3-hydroxy metabolites; and 10% are excreted in the bile [4].