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基于石墨烯的疏水性固相微萃取纤维的溶胶-凝胶制备及性能评价及其在水样中多种农药残留分析中的应用。

Sol-gel fabrication and performance evaluation of graphene-based hydrophobic solid-phase microextraction fibers for multi-residue analysis of pesticides in water samples.

机构信息

Research Center of Analytical Instrumentation, Northwest University, 1 Xuefu Ave., Xi'an, Shaanxi 710069, China.

出版信息

Anal Methods. 2020 Aug 21;12(31):3954-3963. doi: 10.1039/d0ay01153c. Epub 2020 Aug 3.

DOI:10.1039/d0ay01153c
PMID:32744282
Abstract

Widespread use of organophosphorus pesticides poses serious environmental threats, and hence calls for effective analysis methods for these classes of compounds. In this study, a lab-made graphene-based solid-phase microextraction (SPME) fiber was fabricated by the sol-gel method and combined with a gas chromatography-flame photometry detector (GC-FPD) to realize the detection of trace OPPs in water samples. Compared to the commercial fiber coatings, the new sol-gel graphene fiber coatings showed advantages of good durability and solvent resistance, which were attributed to the hydrophobic and antibacterial properties of the functionalized graphene and 3-(trimethoxysilyl)propyldimethyloctadecylammonium chloride (QAS). A headspace SPME method in combination with a GC-FPD was established to evaluate the performance of the novel fibers. The proposed method showed a good linear relationship for the eight OPPs (R≥ 0.9957) in the concentration range of 1 to 1000 μg L, with limits of quantification of 0.11-3.37 μg L and limits of detection of 0.03-1.01 μg L. Furthermore, the developed method also exhibited good recoveries for the analysis of OPPs both in rainwater and lake water, which demonstrates that this method is an alternative choice for multi-residue analysis of OPPs, and it has the potential for broader applications in the future.

摘要

广泛使用有机磷农药对环境造成严重威胁,因此需要有效的分析方法来检测这些化合物。在本研究中,通过溶胶-凝胶法制备了一种实验室制造的基于石墨烯的固相微萃取(SPME)纤维,并与气相色谱-火焰光度检测器(GC-FPD)结合,实现了水样中痕量有机磷农药的检测。与商业纤维涂层相比,新的溶胶-凝胶石墨烯纤维涂层具有良好的耐久性和耐溶剂性优势,这归因于功能化石墨烯和 3-(三甲氧基硅基)丙基二甲基十八烷基氯化铵(QAS)的疏水性和抗菌性能。建立了顶空 SPME 法与 GC-FPD 相结合的方法来评估新型纤维的性能。该方法对 8 种有机磷农药(R≥0.9957)在 1 至 1000 μg/L 的浓度范围内表现出良好的线性关系,定量限为 0.11-3.37 μg/L,检测限为 0.03-1.01 μg/L。此外,该方法还对雨水和湖水样品中的有机磷农药分析表现出良好的回收率,这表明该方法是有机磷农药多残留分析的一种替代选择,并且将来有更广泛的应用潜力。

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