Abstarct: In this study, an azo–azomethine ligand (L) was introduced as a novel chemical sensor for the selective and simultaneous detection of cyanide (CN⁻) and carbonate (CO₃²⁻) anions in acetonitrile medium. its sensing behavior was investigated through UV–Vis studies. Analytical parameters including the limit of detection (LOD), limit of quantification (LOQ), stoichiometric ratio, and binding constant between anion and ligand (Ka) were determined. The ligand exhibited a distinct color change from dark yellow to dark orange in the presence of CN⁻ and CO₃²⁻ ions, while other tested anions showed no significant response. The UV–Vis spectra displayed a bathochromic shift accompanied by an increase in absorbance intensity at 490 nm, which was attributed to intramolecular charge transfer (ICT). The limit of detection was found to be 6.00 × 10⁻⁶ M for cyanide and 8.78 × 10⁻⁶ M for carbonate. Job’s plot studies indicated a 1:1 binding stoichiometry for the ligand–cyanide complex and a 2:1 ratio for the ligand–carbonate complex. The binding constant was calculated to be 3.5 × 10⁴ M⁻¹ for CN⁻ and 1.59 × 10¹⁰ M⁻² for CO₃²⁻, indicating a stronger interaction with carbonate ions. The performance of the sensor was evaluated in real samples including bitter almonds, biscuits, and water samples. Matrix effects were examined using the spike recovery method, and the results demonstrated acceptable accuracy and precision of the proposed method. Furthermore, the development of a simple colorimetric kit enabled rapid, low-cost, and on-site measurements.