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Determination of six organophosphorus pesticides in water samples by three-dimensional graphene aerogel-based solid-phase extraction combined with gas chromatography/mass spectrometry

机译:三维石墨烯气凝胶固相萃取-气相色谱/质谱法测定水样中的六种有机磷农药

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In the present study, a three-dimensional graphene aerogel (3D-GA), synthesised by chemical reduction of an aqueous solution of graphene oxides (GOs) with ethylenediaminethermal by a simple water bath method followed by freeze-drying treatment, was used for the solid-phase extraction (SPE) of six organophosphorus pesticides (OPPs) ( i.e. trichlorfon, dimethoate, ethoprophos, parathion, fenitrothion and fenthion) from water samples. The target analytes were extracted using packed SPE cartridges and then eluted with tetrahydrofuran. The eluate was collected and dried with high-purity nitrogen gas at room temperature. After redissolving in acetone, the residue was analysed using gas chromatography/mass spectrometry (GC/MS). The proposed method demonstrated a good linearity between 0.5 and 500 μg L ~(?1) with the correlation coefficient of 0.9990–0.9998. The limits of detection (LODs) (S/N = 3) and the limits of quantification (LOQs) (S/N = 10) for the six OPPs pesticides were in the range of 0.12–0.58 μg L ~(?1) and 0.41–1.96 μg L ~(?1) , respectively. The accuracy of the present method was evaluated by measuring the recovery of the spiked samples, which ranged from 93.8% to 104.2% with relative standard deviations (RSDs) of 1.1–5.6%. The established method was successfully applied to the determination of the target analytes in environmental water samples including tap water, river water, drinking water and lake water, demonstrating its great potential for the determination of OPPs in water.
机译:在本研究中,三维石墨烯气凝胶(3D-GA)是通过乙二胺热通过简单的水浴方法化学还原氧化石墨烯(GOs)的水溶液,然后进行冷冻干燥处理而合成的。从水样中固相萃取六种有机磷农药(OPP)(即敌百虫,乐果,乙草胺,对硫磷,杀nitro硫磷和倍硫磷)。使用填充的SPE柱提取目标分析物,然后用四氢呋喃洗脱。收集洗脱液,并在室温下用高纯度氮气干燥。在丙酮中重新溶解后,使用气相色谱/质谱法(GC / MS)分析残余物。所提出的方法在0.5和500μgL〜(?1)之间表现出良好的线性,相关系数为0.9990-0.9998。六种OPP农药的检出限(LOD)(S / N = 3)和定量限(LOQs)(S / N = 10)在0.12-0.58μgL〜(?1)和分别为0.41–1.96μgL〜(?1)。通过测量加标样品的回收率来评估本方法的准确性,加标样品的回收率在93.8%至104.2%之间,相对标准偏差(RSD)为1.1-5.6%。所建立的方法已成功应用于环境水样中自来水,河水,饮用水和湖水中目标分析物的测定,证明了其在水中OPPs测定中的巨大潜力。

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