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<p>This study developed, validated, and applied an integrated analytical method for the simultaneous determination of five high-production-volume branched alkylphenols (bAPs) in sediments. The target analytes—4-dodecylphenol (4-DDP), 4-tert-amylphenol (4-t-AP), 4-tert-butylphenol (4-t-BP), 2,4-di-tert-butylphenol (2,4-d-t-BP), and butylated hydroxytoluene (BHT)—are hazardous compounds of concern due to their persistence, bioaccumulation potential, toxicity, and endocrine-disrupting properties. BHT is currently included in the EU Watch List, while 4-DDP, 4-t-AP, and 4-t-BP have been proposed as candidates for future EU Watch List revisions and enhanced environmental monitoring. To the best of our knowledge, this is the first method enabling simultaneous determination of this complete suite of bAPs in sediments. The sample preparation is conducted on a miniaturized scale, integrating focused ultrasound solid–liquid extraction (FUSLE) with dispersive solid-phase extraction (dSPE) in a single step, followed by analysis using liquid chromatography with fluorescence detection (LC–FLD). This streamlined, cost-effective approach offers a greener alternative to conventional multi-step protocols. The method demonstrated strong performance, with good linearity, reliable accuracy (intra-day precision of 7.3–9.5% and recoveries of 81–115% with relative standard deviations of 2.0–17%), high selectivity, and low limits of detection (11–14&#xa0;ng&#xa0;g<sup>−1</sup>) and quantification (36–48&#xa0;ng&#xa0;g<sup>−1</sup>), enabling the determination of bAPs at environmentally relevant concentrations ranging from tens to thousands of ng g⁻<sup>1</sup> sediment. Its greenness and practicality were confirmed using assessment tools. Application to river sediments collected downstream of anthropogenic sources revealed frequent detection of BHT and 4-DDP at concentrations exceeding their predicted no-effect concentration (PNEC), indicating potential ecological risks. These findings provide critical monitoring data for substances currently included in, or proposed for inclusion in, EU monitoring programmes, thereby supporting environmental risk assessment and regulatory decision-making.</p>

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Determination of branched alkylphenols, including tert-alkyl derivatives, in sediments using an integrated ultrasound-assisted extraction and liquid chromatography with fluorescence detection method

  • 期刊论文

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  • 发表日期：

    2026年8月4日

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  • Peter Tölgyessy,
  • Marcel Brenkus,
  • Veronika Koperová Návojová,
  • Michal Kirchner,
  • Svetlana Hrouzková

摘要

This study developed, validated, and applied an integrated analytical method for the simultaneous determination of five high-production-volume branched alkylphenols (bAPs) in sediments. The target analytes—4-dodecylphenol (4-DDP), 4-tert-amylphenol (4-t-AP), 4-tert-butylphenol (4-t-BP), 2,4-di-tert-butylphenol (2,4-d-t-BP), and butylated hydroxytoluene (BHT)—are hazardous compounds of concern due to their persistence, bioaccumulation potential, toxicity, and endocrine-disrupting properties. BHT is currently included in the EU Watch List, while 4-DDP, 4-t-AP, and 4-t-BP have been proposed as candidates for future EU Watch List revisions and enhanced environmental monitoring. To the best of our knowledge, this is the first method enabling simultaneous determination of this complete suite of bAPs in sediments. The sample preparation is conducted on a miniaturized scale, integrating focused ultrasound solid–liquid extraction (FUSLE) with dispersive solid-phase extraction (dSPE) in a single step, followed by analysis using liquid chromatography with fluorescence detection (LC–FLD). This streamlined, cost-effective approach offers a greener alternative to conventional multi-step protocols. The method demonstrated strong performance, with good linearity, reliable accuracy (intra-day precision of 7.3–9.5% and recoveries of 81–115% with relative standard deviations of 2.0–17%), high selectivity, and low limits of detection (11–14 ng g−1) and quantification (36–48 ng g−1), enabling the determination of bAPs at environmentally relevant concentrations ranging from tens to thousands of ng g⁻1 sediment. Its greenness and practicality were confirmed using assessment tools. Application to river sediments collected downstream of anthropogenic sources revealed frequent detection of BHT and 4-DDP at concentrations exceeding their predicted no-effect concentration (PNEC), indicating potential ecological risks. These findings provide critical monitoring data for substances currently included in, or proposed for inclusion in, EU monitoring programmes, thereby supporting environmental risk assessment and regulatory decision-making.