A simple, rapid and accurate method for separating and analysing components in the synthesis of special esters of methacrylic acid by gas chromatography is reported. An SE-54 wide-bore capillary column of 50 m x 0.53 mm i.d. x 0.6 microns was used. The esters include dimethylaminoethyl methacrylate(DMAM), n-butyl methacrylate(BMA) and ethylene glycol dimethacrylate(EGDMA). Crude materials such as methyl methacrylate(MMA) and N, N-dimethyl ethanol amine (DMEA) were also analysed. The recoveries were 99.71%-102.89%, and the RSDs of the main components were below 0.1%. The method can be used to control the production of the esters.