Ministry of Education Key Laboratory for the Synthesis and Application of Organic Functional Molecules, Hubei Collaborative Innovation Center for Advanced Organic Chemical Materials, College of Chemistry and Chemical Engineering, Hubei University, Wuhan, China.
J Sep Sci. 2014 Mar;37(5):587-94. doi: 10.1002/jssc.201301227. Epub 2014 Jan 25.
An IPC-imprinted (IPC is isoprocarb) poly(methacrylic acid)/SiO2 hybrid monolithic column was prepared and applied for the recognition of the template. The hybrid monolithic column was synthesized in a micropipette tip using methyltrimethoxysilane as the inorganic precursor, 3-(methacryloxy)propyltrimethoxysilane as the coupling agent, and ethylene glycol dimethacrylate as the cross-linker. The synthesis conditions, including the porogenic solvent, coupling agent, volume ratio of the inorganic alcoholysate and organic part, were optimized. The prepared monolithic column was characterized by SEM and FTIR spectroscopy. A simple, rapid, and sensitive method for the determination of IPC in rice using the imprinted monolithic column microextraction combined with HPLC was developed. Several parameters affecting the sample pretreatment were investigated, including the eluent, washing solution, and loading sample volume. The linearity of the calibration curve was observed in the range of 9.0-1000 μg/kg for IPC in rice with the correlation coefficient (r2) of 0.9983. The LOD was 3.0 μg/kg (S/N = 3). The assay gave recovery values ranging from 91 to 107%. The proposed method has been successfully applied for the selective extraction and sensitive determination of IPC in rice and a satisfactory result was obtained.
采用静态吸附法制备了对模板分子异丙威（IPC）具有识别性能的印迹整体柱。以甲基三甲氧基硅烷为硅源、3-（甲基丙烯酰氧）丙基三甲氧基硅烷为偶联剂、乙二醇二甲基丙烯酸酯为交联剂，在微流控芯片中制备了聚（甲基丙烯酸）/SiO2 整体柱。考察了致孔剂、偶联剂、硅醇与有机相体积比等因素对整体柱制备的影响，利用 SEM 和 FTIR 对整体柱进行了形貌和结构表征。建立了基于印迹整体柱微萃取-高效液相色谱法测定大米中异丙威残留的分析方法。考察了萃取条件对萃取效率的影响，确定了最佳萃取条件。在 9.0-1000 μg/kg 浓度范围内，异丙威的峰面积与质量浓度呈良好的线性关系，相关系数（r2）为 0.9983，检出限为 3.0 μg/kg（S/N = 3）。在加标水平为 100、200、500 μg/kg 时，平均回收率为 91%-107%，相对标准偏差为 3.6%-5.5%（n = 5）。该方法已成功用于大米中异丙威的测定，结果令人满意。
