An experimental design was applied for the optimization of the extraction process of two preservatives, benzoic and sorbic acids (BA, SA), from food drinks. A simple, rapid, and reliable solid-phase extraction (SPE) method for the simultaneous extraction of these two preservatives and their determination by liquid chromatography with a diode array detector was considered. Box–Behnken design (BBD) was applied to both steps of the SPE process: (i) the sample percolation to ensure the retention of the totality of the acids by the silica-based C18 sorbent; (ii) the elution step to ensure desorption of the totality of the acids from the cartridge. Thus, the volume, pH, and flow rate of the sample, and the percentage of MeOH, volume, and flow rate of the elution solvent, were optimized. Sample volume and pH have a significant influence (p < 0.0001 and p = 0.0115) on the percolation yield. However, no effect was recorded for the flow rate (p > 0.05). Flow rate also has no significant effect on the elution efficiency. The proposed new solid-phase extraction method, which can be easily applied to routine monitoring of preservatives BA and SA in juice and soft drink samples, included 0.5 g of C18 sorbent, 1 mL of food drink adjusted to pH 1 and percolated at 4.5 mL min−1, and 1 mL of a solvent mixture composed of methanol/acidified water (pH = 2.6) (90:10, v/v) used in the elution step at a flow rate of 4.5 mL min−1. Validation of the SPE method and the technique of analysis were evaluated, namely, the accuracy, precision, detection, and quantification limits and linearity. Recovery percentages of benzoic and sorbic acids were above 95% with relative standard deviations lower than 1.78%. Detection and quantification limits were 0.177 and 0.592 µg mL−1, and 0.502 and 0.873 µg mL−1 for benzoic acid and sorbic acid respectively. Optimal conditions were applied to commercial fruit juices and soft drinks and a minimal matrix effect was observed. This method was compared with other SPE methods using oxidized activated carbon and multiwalled carbon nanotubes as adsorbents. The yields determined with these last two were low compared to those determined with our method.