Selective Matrix Removal by TLC for Pesticide Residue Detection in Bee Pollen Using LC–MS/MS

Pesticide contamination in food products poses a significant risk to public health and ecosystems, necessitating rapid, reliable, and environmentally friendly analytical methods. In this study, a novel combination of thin‐layer chromatography (TLC) and liquid chromatography‐tandem mass spectrometry (LC–MS/MS) was developed for the selective prescreening and quantification of pesticide residues. The TLC method enabled effective initial separation of matrix components and target pesticides, including atrazine, carbaryl, and chlorpyrifos, while matrix interferences were effectively excluded by selective zone cutting prior to LC–MS/MS analysis. The LC–MS/MS system provided robust quantification with limits of detection (LOD) as low as 0.001 mg/kg for atrazine and acceptable precision. The method demonstrated linearity for chlorpyrifos and atrazine ( R 2 = 0.971 and 0.955). A green chemistry evaluation was also performed, benchmarking this TLC‐guided approach against the conventional QuEChERS method. Results showed significant reductions in solvent use, energy input, toxic reagent exposure, and sample preparation costs (approx. 0.10 USD/sample vs. 2.50 USD/sample, respectively), while still maintaining acceptable analytical performance. Overall, this TLC/LC–MS/MS method offers a simple and cost‐effective alternative for pesticide monitoring, especially in resource‐limited or field settings.