Dispersive microextraction based on magnetic polypyrrole nanowires for the fast determination of pesticide residues in beverage and environmental water samples
Dispersive microextraction based on magnetic polypyrrole nanowires for the fast determination of pesticide residues in beverage and environmental water samples
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DOI：
10.1007/s00216-013-6866-5
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发表时间：
2013-03
影响因子：
4.3
通讯作者：
Qin Zhao;Q. Lu;Yuqi Feng
中科院分区：
文献类型：
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作者：
Qin Zhao;Q. Lu;Yuqi Feng
在这项研究中，磁性聚吡咯纳米线（mPPYs）是通过一种基于“聚集-包裹”机制的简单共混方法制备的。以十六烷基三甲基溴化铵为“软模板”，采用原位化学氧化聚合法制备了聚吡咯（PPy）纳米线，并采用溶剂热法制备了磁性纳米粒子（MNPs）。通常，当这两种纳米材料在溶剂中涡旋混合时，MNPs被包裹在聚合过程中形成的PPy纳米线网络中，从而形成mPPYs，可以通过磁铁快速方便地从溶剂中分离出来。由于所得材料具有较好的渗透性、良好的吸附能力和磁性可分离性，利用磁性固相萃取（MSPE）对有机磷、有机氯、拟除虫菊酯等11种农药进行富集，以验证其在样品制备中的可行性。考察了影响提取效率的几个参数，在优化条件下，建立了一种简便有效的气相色谱/质谱联用分析方法。整个预处理过程快速，可在15 min内完成。该方法的线性范围为0.2 ~ 10 μg/L，相关系数(R)为0.995 ~ 0.999；目标化合物的定量限在0.09 ~ 0.29 μg/L范围内。此外，在相对标准偏差分别小于14%和16%的情况下，通过评估日内和日内精密度，获得了可接受的再现性。最后，建立的MSPE-GC/MS方法成功应用于饮料茶、果汁和环境水样中农药残留的检测。图1基于“聚合-包裹”的mPPYs的简易制备
In this study, magnetic polypyrrole nanowires (mPPYs) were fabricated via a simple co-mixing method based on an “aggregation-wrap” mechanism. The polypyrrole (PPy) nanowires were synthesized by in situ chemical oxidative polymerization using cetyltrimethylammonium bromide as the “soft template” and the magnetic nanoparticles (MNPs) prepared using solvothermal methods. Typically, when these two nanomaterials were vortically mixed in a solvent, the MNPs were wrapped into the PPy nanowire networks that formed during the aggregation process, leading to the formation of mPPYs which can be separated from the solvent rapidly and conveniently by a magnet. Due to the better permeability, good adsorption ability, and magnetic separability of the resultant material, mPPYs were applied for the enrichment of 11 pesticides including organophosphorus, organochlorine, and pyrethroid using magnetic solid phase extraction (MSPE) to test their feasibility in sample preparation. Several parameters affecting the extraction efficiency were investigated, and under the optimized conditions, a simple and effective method for the determination of pesticide residues was established by coupling with gas chromatography/mass spectrometry (GC/MS) analysis. The whole pretreatment process was rapid and can be accomplished within 15 min. The linearity range of the proposed method was 0.2–10 μg/L, with correlation coefficients (R) of 0.995–0.999; the limits of quantification for the target compounds were in the range of 0.09–0.29 μg/L. In addition, an acceptable reproducibility was achieved by evaluating the intra- and inter-day precisions with relative standard deviations of less than 14 and 16 %, respectively. Finally, the established MSPE-GC/MS method was successfully applied for the determination of pesticide residues in beverage teas, juices, and environmental water samples.FigureFacile preparation of mPPYs based on “aggregation-wrap”