In order to develop new available matrixcompatible solid phase microextraction (SPME) coating and promote the development of in vivo SPME sampling technology in agriculture,the matrix compatibility of solgel polydimethylsiloxane coating was evaluated and a simple and sensitive DISPME/gas chromatography method was established for analysis of five organophosphorus pesticides in citrus pulp.When the citrus pulp was diluted by equal amount of water,adjusted to pH 1.84,and subjected to DISPME at 50℃ for 60 min with a stirring rate of 1 200 r/min,the good linear ranges were obtained with linear regression coefficients (R2) greater than 0.999 for all test compounds in citrus matrix as well as low limits of detection (ranging from 0.002 to 0.046 μg/kg),good repeatability (0.5%15.6%) and high recoveries (71.0%125.3%).The solgel fiber could be used more than 50 times for in vivo sampling in citrus pulp.