This review updates our knowledge on matrix solid-phase dispersion (MSPD), a sample treatment procedure that is increasingly used for extracting/purifying contaminants from a variety of solid, semi-solid, viscous, and liquid foodstuffs. MSPD is primarily used because of its flexibility, selectivity, and the possibility of performing extraction and cleanup in one step, this resulting in drastically shortening of the analysis time and low consumption of toxic and expensive solvents. Technical developments and parameters influencing the extraction yield and selectivity are examined and discussed. Experimental results for the analysis of pesticides, veterinary drugs, persistent environmental chemicals, naturally occurring toxicants, and surfactants in food are reviewed.