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Application of Ion-Imprinted Polymer Nanoparticles for Selective Trace Determination of Palladium Ions in Food and Environmental Samples with the Aid of Experimental Design Methodology

机译:离子印迹聚合物纳米颗粒在实验设计方法辅助下选择性痕量测定食品和环境样品中钯离子的应用

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A solid phase extraction method using Pd2+ ion-imprinted polymer (Pd2+-IIP) nanoparticles combined with flame atomic absorption spectrophotometry (FAAS) was developed for the preconcentration and trace detection of palladium ions. The Pd2+-IIP nanoparticles were obtained by precipitation polymerization of 4-vinylpyridine (the functional monomer), ethylene glycol dimethacrylate (the cross-linker), 2,2'-azobisisobutyronitrile (the initiator), Eriochrome Cyanine R (the lead-binding ligand), and palladium ions (the template ion) in acetonitrile solution. The parameters affecting adsorption and desorption steps were optimized by a Box-Behnken design through response surface methodology. Three variables (pH value, extraction time, and amount of the synthesized IIP) were selected as the main factors affecting sorption step, while four variables (type of eluent, volume of the eluent, concentration of the eluent, and elution time) were selected for desorption step in the optimization study. The optimized values by this optimization method were 30 mg, 15 min, 6.0, HCl, 4.0 mL, 1.8 mol L-l HCl, and 14 min, for amount of polymer, retention time, pH of solution, type, volume, concentration of the eluent, and elution time, respectively. Under the optimized conditions, the detection limit for the proposed method was found to be 0.2 mu g L-1, while the relative standard deviation (RSD) for five replicate measurements was calculated to be 3 %. Finally, the introduced solid phase extraction technique was successfully applied for extraction and determination of Pd2+ ions in food and environmental samples.
机译:开发了一种使用Pd2 +离子印迹聚合物(Pd2 + -IIP)纳米颗粒与火焰原子吸收分光光度法(FAAS)结合的固相萃取方法,用于钯离子的预浓缩和痕量检测。通过4-乙烯基吡啶(功能单体),乙二醇二甲基丙烯酸酯(交联剂),2,2'-偶氮二异丁腈(引发剂),Eriochrome Cyanine R(铅结合配体)的沉淀聚合获得Pd2 + -IIP纳米颗粒。 )和乙腈溶液中的钯离子(模板离子)。通过响应表面方法,通过Box-Behnken设计优化了影响吸附和解吸步骤的参数。选择三个变量(pH值,提取时间和合成的IIP的量)作为影响吸附步骤的主要因素,同时选择四个变量(洗脱液的类型,洗脱液的体积,洗脱液的浓度和洗脱时间)优化研究中的解吸步骤。对于聚合物的量,保留时间,溶液的pH值,类型,体积,洗脱液浓度,通过此优化方法得出的优化值为30 mg,15分钟,6.0,HCl,4.0 mL,1.8 mol Ll HCl和14分钟。和洗脱时间。在最佳条件下,该方法的检出限为0.2μg L-1,而五次重复测量的相对标准偏差(RSD)计算为<3%。最终,引入的固相萃取技术成功地用于食品和环境样品中Pd2 +离子的萃取和测定。

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