首页> 外文期刊>Journal of separation science. >A molecularly imprinted organic-inorganic hybrid monolithic column for the selective extraction and HPLC determination of isoprocarb residues in rice
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A molecularly imprinted organic-inorganic hybrid monolithic column for the selective extraction and HPLC determination of isoprocarb residues in rice

机译:分子印迹有机-无机杂化整体柱用于选择性提取和HPLC测定大米中异丙威的残留量

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摘要

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 usingmethyltrimethoxysilane 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 (r~2) 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.
机译:制备了IPC印迹(IPC为异丙威)聚(甲基丙烯酸)/ SiO2混合整体柱,并将其用于模板识别。使用甲基三甲氧基硅烷作为无机前体,3-(甲基丙烯酰氧基)丙基三甲氧基硅烷作为偶联剂,乙二醇二甲基丙烯酸酯作为交联剂,在微量移液器吸头中合成杂化整体柱。对合成条件进行了优化,包括成孔剂,偶联剂,无机醇化物和有机部分的体积比。制备的整体柱通过SEM和FTIR光谱表征。建立了一种使用压印的整体柱微萃取与HPLC结合的简单,快速,灵敏的大米中IPC测定方法。研究了影响样品预处理的几个参数,包括洗脱液,洗涤液和上样量。水稻中IPC的校正曲线线性在9.0-1000μg/ kg范围内,相关系数(r〜2)为0.9983。 LOD为3.0μg/ kg(S / N = 3)。该测定给出的回收值为91%至107%。该方法已成功应用于水稻中IPC的选择性提取和灵敏测定,获得了满意的结果。

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