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<p>Pyrimethanil is a widely used fungicide and its residues in carbohydrate rich foods require vigilant monitoring for consumer protection and regulatory compliance. In this study, a metal sieve-linked double-syringe sugaring-out liquid–liquid microextraction (MSLDS-SULLME) method coupled to GC-MS is presented for pesticide-residue determination in sugar-rich matrices exemplified by grape molasses. Endogenous sugars induce phase separation, while syringe-driven passage through a perforated metal sieve sustains interfacial renewal in a closed configuration, minimizing operator-dependent variability and avoiding disperser additives. In grape-molasses extracts, linear working range of 9.39–481.6&#xa0;µg kg<sup>−1</sup> was obtained with R<sup>2</sup> as 0.9989. The limit of detection (LOD) and limit of quantification (LOQ) values were determined as 4.31 and 14.37&#xa0;µg kg<sup>−1</sup>, respectively. Under identical GC-MS conditions, 79.66-fold sensitivity enhancement was observed relative to direct instrumental analysis. Using matrix-matching calibration strategy, recoveries of 83.00–129.16% were achieved with low within-set variability, thus confirming applicability in the authentic sugar-rich matrix. Overall, the developed approach offers a practical route for improving pesticide-residue analysis in viscous, sugar-rich matrices where conventional sample preparation may be limited by matrix effects and phase-handling difficulties. Therefore, it can be useful for analytical chemists, food-control laboratories and authorities involved in residue monitoring.</p>

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A metal sieve-linked double-syringe sugaring-out liquid–liquid microextraction as a new analytical system for the accurate and sensitive determination of pyrimethanil in GC-MS

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  • 发表日期：

    2026年7月3日

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  • Ayça Girgin,
  • Esra Sultan Doru,
  • Olcaytu Çetiner,
  • Tuğçe Unutkan Gösterişli,
  • Sezgin Bakırdere

摘要

Pyrimethanil is a widely used fungicide and its residues in carbohydrate rich foods require vigilant monitoring for consumer protection and regulatory compliance. In this study, a metal sieve-linked double-syringe sugaring-out liquid–liquid microextraction (MSLDS-SULLME) method coupled to GC-MS is presented for pesticide-residue determination in sugar-rich matrices exemplified by grape molasses. Endogenous sugars induce phase separation, while syringe-driven passage through a perforated metal sieve sustains interfacial renewal in a closed configuration, minimizing operator-dependent variability and avoiding disperser additives. In grape-molasses extracts, linear working range of 9.39–481.6 µg kg−1 was obtained with R2 as 0.9989. The limit of detection (LOD) and limit of quantification (LOQ) values were determined as 4.31 and 14.37 µg kg−1, respectively. Under identical GC-MS conditions, 79.66-fold sensitivity enhancement was observed relative to direct instrumental analysis. Using matrix-matching calibration strategy, recoveries of 83.00–129.16% were achieved with low within-set variability, thus confirming applicability in the authentic sugar-rich matrix. Overall, the developed approach offers a practical route for improving pesticide-residue analysis in viscous, sugar-rich matrices where conventional sample preparation may be limited by matrix effects and phase-handling difficulties. Therefore, it can be useful for analytical chemists, food-control laboratories and authorities involved in residue monitoring.