{"title":"基于磁铁矿纳米颗粒、氧化石墨烯和离子液体的复合材料在基质固相分散法萃取底层沉积物中双酚 A 中的应用","authors":"A. S. Gubin, P. T. Sukhanov, A. A. Kushnir","doi":"10.1134/S1061934824700631","DOIUrl":null,"url":null,"abstract":"<p>A composite based on Fe<sub>3</sub>O<sub>4</sub> nanoparticles, graphene oxide, and a ionic liquid (1-butyl-3-methylimidazolium-2-carboxylate) is proposed as a sorbent for the extraction of bisphenol A (<b>BPA</b>) from bottom sediments by matrix solid-phase dispersion (<b>MSPD</b>). The saturation magnetization of the synthesized sorbent is 34 emu/g. Grinding of bottom sediments and subsequent grinding with a sorbent was carried out in a ball mill. Some stages of MSPD were partially automated, in particular, the procedures of magnetic separation, BPA desorption, and sorbent regeneration. The recovery of BPA under the experimentally selected conditions (sorbent mass 0.5 g, time required to grind the sorbent 5 min) was 94%. The sorbent can withstand four sorption-desorption cycles without a loss of sorption capacity. To purify the matrix from interferents, washing with <i>n</i>-heptane was proposed. Bisphenol A was determined by gas chromatography–mass spectrometry after derivatization with acetic anhydride. The analytical characteristics of the method were established using model samples of bottom sediments artificially contaminated with BPA. The limit of determination using the developed method is 0.1 μg/kg, the linearity range of the calibration curve is 0.3–12 μg/kg (<i>r</i><sup>2</sup> = 0.994). As real samples for analysis, we used bottom sediments selected near the discharge of wastewater treatment plants in the city of Voronezh (Voronezh River and Don River). The BPA concentration in bottom sediments is 3.83–6.52 μg/kg.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":null,"pages":null},"PeriodicalIF":1.0000,"publicationDate":"2024-09-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Application of a Composite Based on Magnetite Nanoparticles, Graphene Oxide, and an Ionic Liquid for the Extraction of Bisphenol A from Bottom Sediments by the Matrix Solid-Phase Dispersion Method\",\"authors\":\"A. S. Gubin, P. T. Sukhanov, A. A. Kushnir\",\"doi\":\"10.1134/S1061934824700631\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p>A composite based on Fe<sub>3</sub>O<sub>4</sub> nanoparticles, graphene oxide, and a ionic liquid (1-butyl-3-methylimidazolium-2-carboxylate) is proposed as a sorbent for the extraction of bisphenol A (<b>BPA</b>) from bottom sediments by matrix solid-phase dispersion (<b>MSPD</b>). The saturation magnetization of the synthesized sorbent is 34 emu/g. Grinding of bottom sediments and subsequent grinding with a sorbent was carried out in a ball mill. Some stages of MSPD were partially automated, in particular, the procedures of magnetic separation, BPA desorption, and sorbent regeneration. The recovery of BPA under the experimentally selected conditions (sorbent mass 0.5 g, time required to grind the sorbent 5 min) was 94%. The sorbent can withstand four sorption-desorption cycles without a loss of sorption capacity. To purify the matrix from interferents, washing with <i>n</i>-heptane was proposed. Bisphenol A was determined by gas chromatography–mass spectrometry after derivatization with acetic anhydride. The analytical characteristics of the method were established using model samples of bottom sediments artificially contaminated with BPA. The limit of determination using the developed method is 0.1 μg/kg, the linearity range of the calibration curve is 0.3–12 μg/kg (<i>r</i><sup>2</sup> = 0.994). As real samples for analysis, we used bottom sediments selected near the discharge of wastewater treatment plants in the city of Voronezh (Voronezh River and Don River). 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引用次数: 0
摘要
摘要 提出了一种基于Fe3O4纳米颗粒、氧化石墨烯和离子液体(1-丁基-3-甲基咪唑鎓-2-羧酸盐)的复合材料,作为基质固相分散(MSPD)从底层沉积物中萃取双酚A(BPA)的吸附剂。合成吸附剂的饱和磁化率为 34 emu/g。底层沉积物的研磨以及随后与吸附剂的研磨是在球磨机中进行的。MSPD 的某些阶段实现了部分自动化,特别是磁分离、双酚 A 解吸和吸附剂再生过程。在实验选定的条件下(吸附剂质量为 0.5 克,吸附剂研磨所需时间为 5 分钟),双酚 A 的回收率为 94%。该吸附剂可经受四次吸附-解吸循环而不损失吸附能力。为了从干扰物中净化基质,建议使用正庚烷进行洗涤。用醋酸酐衍生后,采用气相色谱-质谱法测定双酚 A。利用人工污染的底层沉积物模型样品确定了该方法的分析特性。该方法的测定限为 0.1 μg/kg,校正曲线的线性范围为 0.3-12 μg/kg(r2=0.994)。我们在沃罗涅日市(沃罗涅日河和顿河)污水处理厂排放口附近选择了底层沉积物作为实际分析样本。底层沉积物中的双酚 A 浓度为 3.83-6.52 μg/kg。
Application of a Composite Based on Magnetite Nanoparticles, Graphene Oxide, and an Ionic Liquid for the Extraction of Bisphenol A from Bottom Sediments by the Matrix Solid-Phase Dispersion Method
A composite based on Fe3O4 nanoparticles, graphene oxide, and a ionic liquid (1-butyl-3-methylimidazolium-2-carboxylate) is proposed as a sorbent for the extraction of bisphenol A (BPA) from bottom sediments by matrix solid-phase dispersion (MSPD). The saturation magnetization of the synthesized sorbent is 34 emu/g. Grinding of bottom sediments and subsequent grinding with a sorbent was carried out in a ball mill. Some stages of MSPD were partially automated, in particular, the procedures of magnetic separation, BPA desorption, and sorbent regeneration. The recovery of BPA under the experimentally selected conditions (sorbent mass 0.5 g, time required to grind the sorbent 5 min) was 94%. The sorbent can withstand four sorption-desorption cycles without a loss of sorption capacity. To purify the matrix from interferents, washing with n-heptane was proposed. Bisphenol A was determined by gas chromatography–mass spectrometry after derivatization with acetic anhydride. The analytical characteristics of the method were established using model samples of bottom sediments artificially contaminated with BPA. The limit of determination using the developed method is 0.1 μg/kg, the linearity range of the calibration curve is 0.3–12 μg/kg (r2 = 0.994). As real samples for analysis, we used bottom sediments selected near the discharge of wastewater treatment plants in the city of Voronezh (Voronezh River and Don River). The BPA concentration in bottom sediments is 3.83–6.52 μg/kg.
期刊介绍:
The Journal of Analytical Chemistry is an international peer reviewed journal that covers theoretical and applied aspects of analytical chemistry; it informs the reader about new achievements in analytical methods, instruments and reagents. Ample space is devoted to problems arising in the analysis of vital media such as water and air. Consideration is given to the detection and determination of metal ions, anions, and various organic substances. The journal welcomes manuscripts from all countries in the English or Russian language.