A review of the application of matrix solid-phase dispersion (MSPD) in the extraction of biologically active compounds and impurities from plants and food samples with a particular emphasis on conventional and new types of sorbents has been provided. An overview of MSPD applications for the isolation of organic residues from biological samples, determined using chromatographic and spectroscopic techniques, has been presented. In this study, procedural solutions that may extend MSDP applicability for the extraction such as vortex-assisted, ultrasound-assisted, microwave-assisted, and extraction with a magnetic sorbent have been discussed. Special attention has been paid to MSPD sorbents including modified silica, diatomite, magnesium silicate, alumina, carbon materials (carbon nanotubes, graphene oxide, graphene, or graphite), molecularly imprinted polymers, and cyclodextrin. An important aspect of the MSPD procedure is the use of high-purity and environmentally friendly solvents for extraction (e.g., deep eutectic solvents), with such criteria being the most important for modern analytical chemistry. Many advantages of MSPD are presented, such as high recoveries, the requirement for a smaller volume of solvent, and shorter procedure times than classical methods.