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We describe here a method using matrix solid-phase dispersion (MSPD) for the analysis of atrazine, metribuzin, cyanazine, and simazine in fish muscle tissue with a minimal amount of time and solvent consumed. A tissue sample is placed in a glass mortar containing a bonded-phase solid support material. The solid support and sample are manually blended together using a glass pestle. The blended material is packed into a column containing activated Florisil and eluted with acetonitrile:methanol (9:1). The eluate is concentrated and analyzed by high-performance liquid chromatography with ultraviolet detection. The linearity of response ranges from 0.35 to 8.0 ppm, and the average percentage recoveries are between 75 � 3 and 106 � 4%, for a spiking level of 0.35 ppm. The intraassay variability is <3%, and the interassay variability is <5%.