Herein, an analytical method using gas chromatography-tandem mass spectrometry (GC- MS/MS) was devised to detect the presence of the troublesome pesticide dimethipin in various animal-based food products, including chicken, pork, beef, eggs, and milk. The injection port was primed with a matrix derived from pepper leaves that acts as an analyte protectant (AP) to safeguard the target compound from thermal degradation during gas chromatography. The presence of AP resulted in a remarkable limit of quantification of 0.005 mg/kg for dimethipin in five matrices. Three different versions (original, EN, and AOAC) of the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method were compared for dimethipin extraction, with a double-layer solid-phase extraction (SPE) cartridge utilized for matrix purification. A seven-point external calibration curve was established for dimethipin in the five matrices, demonstrating excellent linearity with determination coefficients (R2) ≥ 0.998. The developed quantitative method was validated by fortifying each matrix with three different concentrations of standard dimethipin, and the average recovery fell within the acceptable range outlined in the CODEX guidelines (ranging from 88.8% to 110.0%), with a relative standard deviation (RSD) of ≤ 11.97%. This method effectively addresses the challenge of analyzing dimethipin and can therefore be used as a routine monitoring tool for dimethipin across various matrices.