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Natural Thymol–tert‐Butylhydroquinone–Based Deep Eutectic Solvent/Vortex‐Assisted Dispersive Liquid–Liquid Microextraction for Organophosphorus Pesticide Extraction in Water Samples.

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Title: Natural Thymol–tert‐Butylhydroquinone–Based Deep Eutectic Solvent/Vortex‐Assisted Dispersive Liquid–Liquid Microextraction for Organophosphorus Pesticide Extraction in Water Samples.
Authors: Salehi, Elham1 (AUTHOR), Dehghan, Kamine2 (AUTHOR), Najarzadekan, Hamid3 (AUTHOR), Karami, Sajad4 (AUTHOR), Joolaei Ahranjani, Parham5 (AUTHOR) Parhamjoolaei@gmail.com
Source: Journal of Separation Science. Nov2025, Vol. 48 Issue 11, p1-18. 18p.
Subject Terms: *Organophosphorus pesticides, *Water sampling, *Thymol, *Environmental monitoring, *Gas chromatography, *Solvents, *Hydroquinone
Abstract: Monitoring trace levels of pesticide residues in water remains a major global analytical challenge. We synthesized a bio‐derived hydrophobic deep eutectic solvent (DES), [thymol:tert‐butylhydroquinone] (Thy:TBHQ), and coupled it with vortex‐assisted dispersive liquid–liquid microextraction (DLLME) prior to gas chromatography (GC) with micro electron capture detection (µECD) for pre‐concentration of organophosphorus pesticides (OPPs) (phosphamidon, diazinon, chlorpyrifos). DES formation and stability were confirmed by Fourier transform infrared spectroscopy (O–H red shift) and 1H‐NMR (deshielded phenolic signals). Univariate optimization identified acetonitrile (ACN) as a disperser and ACN/DES = 1:1 (v/v), 100 mL sample, 3 min extraction, and pH 2–6 as optimal. The method showed excellent linearity (coefficients of determination = 0.991–0.997), limits of detection (LODs) of 3.44–15.43 ng L−1 and limits of quantification (LOQs) of 10.32–51.38 ng L−1, all well below the EU 100 ng L−1 per‐pesticide limit, with enrichment factors of 13–27. Precision supported routine application (intra‐day relative standard deviation [RSD] 1.67%–3.79%; inter‐day 5.25%–9.66%). Spiked real samples across environmental waters: tap (≈90%–100% relative recovery), river (≈60%–82%), and seawater (≈54%–66%), each with RSD < 10% and no background residues detected. The DES retained >85% of its extraction performance over ≥9 adsorption–desorption cycles. Satisfactory extraction efficiency is probably due to the synergistic π–π, hydrogen bonding, van der Waals, and hydrophobic interactions between aromatic OPPs and the DES. Overall, the [Thy:TBHQ]‐based vortex‐assisted DLLME/GC with µECD platform delivers sensitive, precise, and reusable trace analysis with reduced solvent use, offering a green alternative for monitoring pesticides in diverse water matrices. [ABSTRACT FROM AUTHOR]
Database: Academic Search Index
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DbLabel: Academic Search Index
An: 189714721
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PubTypeId: academicJournal
PreciseRelevancyScore: 1393.09326171875
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  Label: Title
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  Data: Natural Thymol–tert‐Butylhydroquinone–Based Deep Eutectic Solvent/Vortex‐Assisted Dispersive Liquid–Liquid Microextraction for Organophosphorus Pesticide Extraction in Water Samples.
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  Data: &lt;searchLink fieldCode=&quot;AR&quot; term=&quot;%22Salehi%2C+Elham%22&quot;&gt;Salehi, Elham&lt;/searchLink&gt;&lt;relatesTo&gt;1&lt;/relatesTo&gt; (AUTHOR)&lt;br /&gt;&lt;searchLink fieldCode=&quot;AR&quot; term=&quot;%22Dehghan%2C+Kamine%22&quot;&gt;Dehghan, Kamine&lt;/searchLink&gt;&lt;relatesTo&gt;2&lt;/relatesTo&gt; (AUTHOR)&lt;br /&gt;&lt;searchLink fieldCode=&quot;AR&quot; term=&quot;%22Najarzadekan%2C+Hamid%22&quot;&gt;Najarzadekan, Hamid&lt;/searchLink&gt;&lt;relatesTo&gt;3&lt;/relatesTo&gt; (AUTHOR)&lt;br /&gt;&lt;searchLink fieldCode=&quot;AR&quot; term=&quot;%22Karami%2C+Sajad%22&quot;&gt;Karami, Sajad&lt;/searchLink&gt;&lt;relatesTo&gt;4&lt;/relatesTo&gt; (AUTHOR)&lt;br /&gt;&lt;searchLink fieldCode=&quot;AR&quot; term=&quot;%22Joolaei+Ahranjani%2C+Parham%22&quot;&gt;Joolaei Ahranjani, Parham&lt;/searchLink&gt;&lt;relatesTo&gt;5&lt;/relatesTo&gt; (AUTHOR)&lt;i&gt; Parhamjoolaei@gmail.com&lt;/i&gt;
– Name: TitleSource
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  Data: &lt;searchLink fieldCode=&quot;JN&quot; term=&quot;%22Journal+of+Separation+Science%22&quot;&gt;Journal of Separation Science&lt;/searchLink&gt;. Nov2025, Vol. 48 Issue 11, p1-18. 18p.
– Name: Subject
  Label: Subject Terms
  Group: Su
  Data: *&lt;searchLink fieldCode=&quot;DE&quot; term=&quot;%22Organophosphorus+pesticides%22&quot;&gt;Organophosphorus pesticides&lt;/searchLink&gt;&lt;br /&gt;*&lt;searchLink fieldCode=&quot;DE&quot; term=&quot;%22Water+sampling%22&quot;&gt;Water sampling&lt;/searchLink&gt;&lt;br /&gt;*&lt;searchLink fieldCode=&quot;DE&quot; term=&quot;%22Thymol%22&quot;&gt;Thymol&lt;/searchLink&gt;&lt;br /&gt;*&lt;searchLink fieldCode=&quot;DE&quot; term=&quot;%22Environmental+monitoring%22&quot;&gt;Environmental monitoring&lt;/searchLink&gt;&lt;br /&gt;*&lt;searchLink fieldCode=&quot;DE&quot; term=&quot;%22Gas+chromatography%22&quot;&gt;Gas chromatography&lt;/searchLink&gt;&lt;br /&gt;*&lt;searchLink fieldCode=&quot;DE&quot; term=&quot;%22Solvents%22&quot;&gt;Solvents&lt;/searchLink&gt;&lt;br /&gt;*&lt;searchLink fieldCode=&quot;DE&quot; term=&quot;%22Hydroquinone%22&quot;&gt;Hydroquinone&lt;/searchLink&gt;
– Name: Abstract
  Label: Abstract
  Group: Ab
  Data: Monitoring trace levels of pesticide residues in water remains a major global analytical challenge. We synthesized a bio‐derived hydrophobic deep eutectic solvent (DES), [thymol:tert‐butylhydroquinone] (Thy:TBHQ), and coupled it with vortex‐assisted dispersive liquid–liquid microextraction (DLLME) prior to gas chromatography (GC) with micro electron capture detection (&#181;ECD) for pre‐concentration of organophosphorus pesticides (OPPs) (phosphamidon, diazinon, chlorpyrifos). DES formation and stability were confirmed by Fourier transform infrared spectroscopy (O–H red shift) and 1H‐NMR (deshielded phenolic signals). Univariate optimization identified acetonitrile (ACN) as a disperser and ACN/DES = 1:1 (v/v), 100 mL sample, 3 min extraction, and pH 2–6 as optimal. The method showed excellent linearity (coefficients of determination = 0.991–0.997), limits of detection (LODs) of 3.44–15.43 ng L−1 and limits of quantification (LOQs) of 10.32–51.38 ng L−1, all well below the EU 100 ng L−1 per‐pesticide limit, with enrichment factors of 13–27. Precision supported routine application (intra‐day relative standard deviation [RSD] 1.67%–3.79%; inter‐day 5.25%–9.66%). Spiked real samples across environmental waters: tap (≈90%–100% relative recovery), river (≈60%–82%), and seawater (≈54%–66%), each with RSD &lt; 10% and no background residues detected. The DES retained &gt;85% of its extraction performance over ≥9 adsorption–desorption cycles. Satisfactory extraction efficiency is probably due to the synergistic π–π, hydrogen bonding, van der Waals, and hydrophobic interactions between aromatic OPPs and the DES. Overall, the [Thy:TBHQ]‐based vortex‐assisted DLLME/GC with &#181;ECD platform delivers sensitive, precise, and reusable trace analysis with reduced solvent use, offering a green alternative for monitoring pesticides in diverse water matrices. [ABSTRACT FROM AUTHOR]
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RecordInfo BibRecord:
  BibEntity:
    Identifiers:
      – Type: doi
        Value: 10.1002/jssc.70315
    Languages:
      – Code: eng
        Text: English
    PhysicalDescription:
      Pagination:
        PageCount: 18
        StartPage: 1
    Subjects:
      – SubjectFull: Organophosphorus pesticides
        Type: general
      – SubjectFull: Water sampling
        Type: general
      – SubjectFull: Thymol
        Type: general
      – SubjectFull: Environmental monitoring
        Type: general
      – SubjectFull: Gas chromatography
        Type: general
      – SubjectFull: Solvents
        Type: general
      – SubjectFull: Hydroquinone
        Type: general
    Titles:
      – TitleFull: Natural Thymol–tert‐Butylhydroquinone–Based Deep Eutectic Solvent/Vortex‐Assisted Dispersive Liquid–Liquid Microextraction for Organophosphorus Pesticide Extraction in Water Samples.
        Type: main
  BibRelationships:
    HasContributorRelationships:
      – PersonEntity:
          Name:
            NameFull: Salehi, Elham
      – PersonEntity:
          Name:
            NameFull: Dehghan, Kamine
      – PersonEntity:
          Name:
            NameFull: Najarzadekan, Hamid
      – PersonEntity:
          Name:
            NameFull: Karami, Sajad
      – PersonEntity:
          Name:
            NameFull: Joolaei Ahranjani, Parham
    IsPartOfRelationships:
      – BibEntity:
          Dates:
            – D: 01
              M: 11
              Text: Nov2025
              Type: published
              Y: 2025
          Identifiers:
            – Type: issn-print
              Value: 16159306
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            – Type: volume
              Value: 48
            – Type: issue
              Value: 11
          Titles:
            – TitleFull: Journal of Separation Science
              Type: main
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