首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Solid phase microextraction using new sol-gel hybrid polydimethylsiloxane-2-hydroxymethyl-18-crown-6-coated fiber for determination of organophosphorous pesticides
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Solid phase microextraction using new sol-gel hybrid polydimethylsiloxane-2-hydroxymethyl-18-crown-6-coated fiber for determination of organophosphorous pesticides

机译:使用新型溶胶-凝胶杂化聚二甲基硅氧烷-2-羟甲基-18-皇冠-6涂层纤维进行固相微萃取测定有机磷农药

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摘要

A new sol-gel hybrid coating, polydimethylsiloxane-2-hydroxymethyl-18-crown-6 (PDMS-2OHMe18C6) was prepared in-house for use in solid phase microextraction (SPME). The three compositions produced were assessed for its extraction efficiency towards three selected organophosphorus pesticides (OPPs) based on peak area extracted obtained from gas chromatography with electron capture detection. All three compositions showed superior extraction efficiencies compared to commercial 100μm PDMS fiber. The composition showing best extraction performance was used to obtain optimized SPME conditions: 75°C extraction temperature, 10min extraction time, 120rpm stirring rate, desorption time 5min, desorption temperature 250°C and 1.5% (w/v) of NaCl salt addition. The method detection limits (S/N=3) of the OPPs with the new sol-gel hybrid material ranged from 4.5 to 4.8ngg~(-1), which is well below the maximum residue limit set by Codex Alimentarius Commission and European Commission. Percentage recovery of OPPs from strawberry, green apple and grape samples with the new hybrid sol-gel SPME material ranged from 65 to 125% with good precision of the method (%RSD) ranging from 0.3 to 7.4%.
机译:内部制备了一种新的溶胶-凝胶杂化涂料,即聚二甲基硅氧烷-2-羟甲基-18-皇冠-6(PDMS-2OHMe18C6),用于固相微萃取(SPME)。基于从具有电子俘获检测的气相色谱获得的峰面积,评估了所产生的三种组合物对三种选定的有机磷农药(OPP)的萃取效率。与市售的100μmPDMS纤维相比,这三种组合物均显示出优异的提取效率。使用表现出最佳萃取性能的组合物获得优化的SPME条件:75°C萃取温度,10min萃取时间,120rpm搅拌速率,解吸时间5min,解吸温度250°C和1.5%(w / v)的NaCl盐添加量。新型溶胶-凝胶杂化材料对OPP的方法检测限(S / N = 3)为4.5至4.8ngg〜(-1),远低于食品法典委员会和欧盟委员会设定的最大残留限量。使用新型混合溶胶凝胶SPME材料从草莓,青苹果和葡萄样品中回收OPP的百分比范围为65%至125%,该方法的精密度(%RSD)为0.3%至7.4%。

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