基质相容性溶胶凝胶固相微萃取涂层直接萃取柑橘中农药残留
Matrix compatible sol gel coating for direct immersion solid phase microextraction of pesticides residues in citrus

为了开发新的可利用的基质相容性固相微萃取（solid phase microextraction，SPME）涂层，促进活体SPME采样技术的发展。本研究评价了溶胶 凝胶聚二甲基硅氧烷萃取头在柑橘基质中的基质相容性，建立了直接SPME 气相色谱法检测柑橘果浆中有机磷农药的方法。结果表明：在柑橘果肉匀浆并添加同样质量的水，调节pH至1.84、50℃萃取60 min、搅拌速度为1 200 r/min条件下，5种有机磷农药在线性范围内具有良好的线性关系，R2≥0.999，检测限为0.002~0.046 μg/kg，加标回收率为71.0%~125.3%，相对标准偏差为0.5%~15.6%。该萃取头在柑橘活体基质中可以连续使用50次以上。
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