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Magnetic solid-phase extraction using a mixture of two types of nanoparticles followed by gas chromatography-mass spectrometry for the determination of six phthalic acid esters in various water samples

机译:磁性固相萃取,使用两种纳米颗粒的混合物,然后进行气相色谱-质谱法测定各种水样中的六种邻苯二甲酸酯

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Two types of magnetic microspheres (Fe _(3) O _(4) @MIL-100 and Fe _(3) O _(4) @SiO _(2) @polythiophene) were prepared and characterized as mixed sorbents for magnetic solid-phase extraction (MSPE) of six phthalic acid esters (PAEs), including dimethyl phthalate (DMP), diethyl phthalate (DEP), di- n -butyl phthalate (DBP), benzyl butyl phthalate (BBP), di-2-ethylhexyl phthalate (DEHP), and di- n -octyl phthalate (DnOP) from water samples prior to gas chromatography-mass spectrometry (GC-MS) analysis. The synthetic magnetic nanocomposites exhibited good repeatability and chemical stability, and improved extraction efficiency for the tested PAEs. The mixture of the two types of nanoparticles substantially improved the extraction efficiency of both DMP and DEP. The key parameters affecting the extraction efficiency, such as the type and the amount of sorbent, eluent (desorption solvent), adsorption and desorption time, pH of sample solution, and sample volume, were investigated and optimized, respectively. Under optimized conditions, the developed method showed satisfactory linearity in the range of 5–5000 μg L ~(?1) with coefficients of determination ( R ~(2) ) > 0.9935. The method detection limits (MDLs) and limits of quantitation (LOQs) were between 0.35–0.91 μg L ~(?1) and 1.1–2.9 μg L ~(?1) , respectively. At three fortification levels (1.0, 10.0, and 50.0 μg L ~(?1) ), the mean recoveries ranged from 76.9–109.1% with favorable relative standard deviations (RSDs) < 9%. The feasibility of the method was evaluated by analysis of water samples from various sources (tap, drinking, and mineral water). The results show that the developed method is suitable for determination of trace level PAEs in water samples.
机译:制备了两种类型的磁性微球(Fe _(3)O _(4)@ MIL-100和Fe _(3)O _(4)@SiO _(2)@聚噻吩)并表征为磁性固体的混合吸附剂相萃取(MSPE)的六种邻苯二甲酸酯(PAE),包括邻苯二甲酸二甲酯(DMP),邻苯二甲酸二乙酯(DEP),邻苯二甲酸二正丁酯(DBP),邻苯二甲酸苄基丁酯(BBP),二-2-乙基己基气相色谱-质谱(GC-MS)分析之前,从水样中提取邻苯二甲酸盐(DEHP)和邻苯二甲酸二正辛酯(DnOP)。合成的磁性纳米复合材料表现出良好的重复性和化学稳定性,并提高了被测PAE的提取效率。两种类型的纳米颗粒的混合物大大提高了DMP和DEP的提取效率。研究和优化了影响萃取效率的关键参数,例如吸附剂的类型和数量,洗脱液(解吸溶剂),吸附和解吸时间,样品溶液的pH值以及样品量。在最佳条件下,所开发的方法在5–5000μgL〜(?1)范围内表现出令人满意的线性,测定系数为(R〜(2))> 0.9935。方法的检测限(MDL)和定量限(LOQ)分别在0.35–0.91μgL〜(?1)和1.1–2.9μgL〜(?1)之间。在三个设防水平(1.0、10.0和50.0μgL〜(?1))下,平均回收率范围为76.9–109.1%,相对标准偏差(RSD)小于9%。通过分析各种来源(自来水,饮用水和矿泉水)中的水样,评估了该方法的可行性。结果表明,该方法适用于水样中痕量PAE的测定。

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