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基于三维石墨烯气凝胶固相萃取结合气相色谱/质谱法测定水样中的六种有机磷农药

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

作者信息

Sun P, Gao Y L, Xu C, Lian Y F

机构信息

Key Laboratory of Functional Inorganic Material Chemistry, Ministry of Education, School of Chemistry and Materials Science, Heilongjiang University Harbin 150080 China

Analytical Centre, Heilongjiang Bayi Agricultural University Daqing163319 China.

出版信息

RSC Adv. 2018 Mar 13;8(19):10277-10283. doi: 10.1039/c7ra13316b.

DOI:10.1039/c7ra13316b
PMID:35540481
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC9078834/
Abstract

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) ( 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 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 and 0.41-1.96 μg L, 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.

摘要

在本研究中,通过简单的水浴法用乙二胺热还原氧化石墨烯(GOs)水溶液,随后进行冷冻干燥处理,合成了三维石墨烯气凝胶(3D - GA),用于从水样中固相萃取(SPE)六种有机磷农药(OPPs)(敌百虫、乐果、灭线磷、对硫磷、杀螟硫磷和倍硫磷)。使用填充的SPE小柱萃取目标分析物,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吹干。在丙酮中重新溶解后,残留物用气相色谱/质谱联用仪(GC/MS)进行分析。所提出的方法在0.5至500μg/L之间表现出良好的线性,相关系数为0.9990 - 0.9998。六种OPPs农药的检测限(LODs)(S/N = 3)和定量限(LOQs)(S/N = 10)分别在0.12 - 0.58μg/L和0.41 - 1.96μg/L范围内。通过测量加标样品的回收率来评估本方法的准确性,回收率范围为93.8%至104.2%,相对标准偏差(RSDs)为1.1 - 5.6%。所建立的方法成功应用于测定包括自来水、河水、饮用水和湖水在内的环境水样中的目标分析物,证明了其在测定水中OPPs方面的巨大潜力。

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