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<p>The presence of phenols in wastewater poses significant environmental and health risks due to their toxicity and persistence. This study explores a targeted approach of amine and/or aniline functionalization of fibrous silica material for the membrane supported micro solid phase extraction of polar phenols. Therefore, four different sorbents were synthesized: unmodified fibrous silica (FS), FS functionalized with N1-(3-Trimethoxysilylpropyl) diethylenetriamine (FS-Amine), FS functionalized with N-[3-(Trimethoxysilyl)propyl] aniline (FS-Aniline), and FS copolymerized with both amine and aniline monomers (FS-Mix). The synthesized materials were characterized using XPS, XRD, FTIR, SEM, and TGA techniques to confirm their structural and functional properties. The µ-SPE method was optimized for key parameters, including sorbent dosage, extraction time, desorption conditions, and solvent composition. High-performance liquid chromatography with diode array detector (HPLC–DAD) analysis demonstrated that FS-Mix exhibited the highest extraction efficiency for five target phenols: 2,3-Dichlorophenol (2,3-DCP), 3,4-Dichlorophenol (3,4-DCP), 2,4,6-Trichlorophenol (2,4,6-TCP), 4-Bromophenol (4-BP), and 4-Nitrophenol (4-NP). Method validation showed good linearity (<i>R</i><sup>2</sup> &gt; 0.99), low limits of detection (LOD: 0.97–2.31&#xa0;ppb), and high relative recovery rates (90.60–113.60%). Real wastewater analysis confirmed the applicability of FS-Mix for phenol extraction, with detected concentrations of 1.601&#xa0;µg·mL<sup>−1</sup> for 4-NP and 0.055&#xa0;µg·mL<sup>−1</sup> for 4-BP. This study highlights the potential of functionalized fibrous silica as a highly effective and selective sorbent for µ-SPE, offering a promising approach for the environmental monitoring and removal of phenols from wastewater.</p>

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Amine-Aniline Terminated Copolymerization of Fibrous Silica for the Extraction of Polar Phenolic Pollutants from Wastewater Using Membrane Supported Micro-SPE and the Subsequent HPLC–DAD Analysis

  • 期刊论文

  • 发表日期：

    2026年7月26日

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  • Shaima’ Ibrahim Alsabbahen,
  • Shehzada Muhammad Sajid Jillani,
  • Saheed A. Ganiyu,
  • Abdulkadir Tanimu,
  • Khalid Alhooshani

摘要

The presence of phenols in wastewater poses significant environmental and health risks due to their toxicity and persistence. This study explores a targeted approach of amine and/or aniline functionalization of fibrous silica material for the membrane supported micro solid phase extraction of polar phenols. Therefore, four different sorbents were synthesized: unmodified fibrous silica (FS), FS functionalized with N1-(3-Trimethoxysilylpropyl) diethylenetriamine (FS-Amine), FS functionalized with N-[3-(Trimethoxysilyl)propyl] aniline (FS-Aniline), and FS copolymerized with both amine and aniline monomers (FS-Mix). The synthesized materials were characterized using XPS, XRD, FTIR, SEM, and TGA techniques to confirm their structural and functional properties. The µ-SPE method was optimized for key parameters, including sorbent dosage, extraction time, desorption conditions, and solvent composition. High-performance liquid chromatography with diode array detector (HPLC–DAD) analysis demonstrated that FS-Mix exhibited the highest extraction efficiency for five target phenols: 2,3-Dichlorophenol (2,3-DCP), 3,4-Dichlorophenol (3,4-DCP), 2,4,6-Trichlorophenol (2,4,6-TCP), 4-Bromophenol (4-BP), and 4-Nitrophenol (4-NP). Method validation showed good linearity (R2 > 0.99), low limits of detection (LOD: 0.97–2.31 ppb), and high relative recovery rates (90.60–113.60%). Real wastewater analysis confirmed the applicability of FS-Mix for phenol extraction, with detected concentrations of 1.601 µg·mL−1 for 4-NP and 0.055 µg·mL−1 for 4-BP. This study highlights the potential of functionalized fibrous silica as a highly effective and selective sorbent for µ-SPE, offering a promising approach for the environmental monitoring and removal of phenols from wastewater.