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Carbamazepine is a crucial medication used to treat nervous system disorders, and its low level of absorption in the human body suggests that a significant amount of it may be present in sewage water. Consequently, this pioneering research deals with the synthesis and application of a luminescent sensor based on rhodamine 6 G-modified bifunctional silica particles for the determination of carbamazepine. The sensing material was fabricated in one step by the sol–gel technique and the dye was adsorbed onto the surface from an alcohol solution. The composition, morphology and size of functionalized silica particles were determined by physico-chemical methods. The material’s features provide the possibility of its application as a sensing material for carbamazepine determination at a variety of concentrations. The sensor possesses a linear response towards carbamazepine in the concentration range of 0.8–200.0 μM with a limit of detection (LOD) of 17.9 μM and a limit of quantification (LOQ) of 59.7 μM and has demonstrated reliable quantification over a wide range of concentrations, from therapeutic to high fatal concentrations. Additionally, the sensing mechanism has been proposed, which involves the formation of hydrogen bonding between carbamazepine and Rhodamine 6G immobilized bifunctional silica particles.