Sunset Yellow FCF (SY FCF) is one of the widely used synthetic azo dyes in the food industry whose content has to be controlled for safety reasons. Electrochemical sensors are a promising tool for this type of task. A voltammetric sensor based on a combination of tin and cerium dioxide nanoparticles (SnO2–CeO2 NPs) with surfactants has been developed for SY FCF determination. The synergetic effect of both types of NPs has been confirmed. Surfactants of various natures (sodium lauryl sulfate (SLS), Brij® 35, and hexadecylpyridinium bromide (HDPB)) have been tested as dispersive media. The best effects, i.e., the highest oxidation currents of SY FCF, have been observed in the case of HDPB. The sensor demonstrates a 4.5-fold-higher electroactive surface area and a 38-fold-higher electron transfer rate compared to the bare glassy carbon electrode (GCE). The electrooxidation of SY FCF is an irreversible, two-electron, diffusion-driven process involving proton transfer. In differential pulse mode in Britton–Robinson buffer (BRB) pH 2.0, the sensor gives a linear response to SY FCF from 0.010 to 1.0 μM and from 1.0 to 100 μM with an 8.0 nM detection limit. The absence of an interferent effect from other typical food components and colorants has been shown. The sensor has been tested on soft drinks and validated with the standard chromatographic method.