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首页> 外文期刊>International journal of environmental analytical chemistry >Preparation of a novel stir bar coating based on montmorillonite doped polypyrroleylon-6 nanocomposite for sorptive extraction of organophosphorous pesticides in aqueous samples
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Preparation of a novel stir bar coating based on montmorillonite doped polypyrroleylon-6 nanocomposite for sorptive extraction of organophosphorous pesticides in aqueous samples

机译：基于蒙脱土掺杂的聚吡咯/尼龙-6纳米复合材料的新型搅拌棒涂料的制备，用于吸附萃取水性样品中的有机磷农药

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摘要

In the present work, a novel nanocomposite (NC) was prepared by reinforcing montmorillonite (MMT) into polypyrrole-nylon-6 (PPy-N6) hybrid through in situ oxidative polymerisation of PPy in the MMT-N6 mixture. The prepared novel NC was deposited as a thin layer coating on the stir bar substrate by solvent exchange method. Fourier transform infrared spectroscopy, scanning electron microscopy, X-ray diffraction and energy dispersive X-ray spectroscopy were applied to characterise the prepared NCs. The prepared stir bar based on MMT/PPy/N6 NC was applied for sorptive extraction of some organophosphorous pesticides (OPPs) in river water samples with detection by gas chromatography-mass spectrometry (GC-MS). The effect of MMT doping level in the NC and also the effect of PPy hybridation with N6 on the coating extraction capability were studied. Central composite design was used to optimise and study the effects of influencing factors on the stir bar sorptive extraction efficiency such as salt content, pH, extraction time, desorption time, desorption solvent and its volume. The method optimisation step was performed using gas chromatography-flame ionisation detector, while the method validation was conducted using GC-MS. Limits of detection of the developed method are in the range of 0.05-0.3g L-1 and the linear dynamic ranges are in the range of 0.3-1000 and 1-1000g L-1, respectively. The intra-day precision (RSD %) of developed method with four replicates varied between 5.4 and 8.2% for distilled water spiked at 100g L-1. The applicability of the developed method was examined by extraction and determination of OPP compounds in river water samples, indicating the relative recoveries in the range of 80.3-95.3%.
机译：在目前的工作中，通过将蒙脱石（MMT）通过在MMT-N6混合物中进行原位氧化聚合，将蒙脱土（MMT）增强为聚吡咯-尼龙6（PPy-N6）杂化物，制备了一种新型的纳米复合材料。通过溶剂交换法将制备的新型NC作为薄层涂层沉积在搅拌棒基材上。傅里叶变换红外光谱，扫描电子显微镜，X射线衍射和能量色散X射线光谱用于表征制备的NCs。将制备的基于MMT / PPy / N6 NC的搅拌棒用于吸附萃取河水中样品中的某些有机磷农药（OPP），并通过气相色谱-质谱（GC-MS）检测。研究了NC中MMT掺杂水平的影响以及PPy与N6杂化对涂层提取能力的影响。采用中央复合设计优化和研究了影响搅拌棒吸附萃取效率的因素，如盐含量，pH，萃取时间，脱附时间，脱附溶剂及其体积。使用气相色谱-火焰电离检测器执行方法优化步骤，同时使用GC-MS进行方法验证。所开发方法的检出限分别为0.05-0.3g L-1和线性动态范围为0.3-1000和1-1000g L-1。对于加标为100g L-1的蒸馏水，四次重复的开发方法的日内精度（RSD％）在5.4至8.2％之间变化。通过萃取和测定河水样品中的OPP化合物来检验所开发方法的适用性，表明相对回收率在80.3-95.3％的范围内。

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