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

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 R 2 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.