AbstractMethacrylic acid is a hydrolytic breakdown product of methylmethacrylate which is widely used in orthopaedic surgery, dentistry and in the chemical industry for fabrication of acrylic resins. Information on the toxicity of methacrylic acid and its metabolism is limited. To facilitate studies in this field we developed a liquid chromatographic procedure allowing determination of methacrylate in blood serum. The procedure was based on reversed‐phase HPLC using a gradient elution with UV detection at 210 or 240 nm. The method was linear up to 5 mMconcentration with a detection limit of 0.5 μM. The procedure was applied to determination of methacrylate in rat blood serum after administration of sodium methacrylate solution into the stomach. A peak of this compound was demonstrated in the chromatogram 10 min after administration which disappeared after 60 min, confirming suitability of the method for biological applicatio