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Article · Journal of Separation Science · June 30, 2025

Eco‐Friendly Miniaturized Solid Phase Microextraction for Pesticide Analysis in Grapes

Mereke B. Alimzhanova, Yerkanat Syrgabek, Pedro Antonio García-Encina

Yerkanat Syrgabek
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Abstract

ABSTRACT A simple and environmentally friendly method based on miniaturized headspace solid‐phase microextraction (Mini‐HS‐SPME) coupled with gas chromatography–mass spectrometry (GC‐MS) was developed for the identification and quantification of ten pesticides (atrazine, simazine, prometryn, metribuzin, cyanazine, fluroxypyr‐meptyl, tebuconazole, epoxiconazole, quizalofop‐methyl, and boscalid) in grape samples. Key extraction parameters were optimized, including extraction temperature, extraction time, selection of the optimal fiber, incubation time, effect of salt, volume of sample, and pH. Final extraction conditions included the use of 200 µL of sample using PDMS 100 µm fiber in headspace mode at 90°C for 30 min. The Mini‐HS‐SPME coupled with the GC‐MS method has been successfully validated in terms of linearity, recovery, and accuracy. The studied linear range of pesticides was 5–1000 ng mL −1 . The limit of detection and limit of quantification ranged between 0.09–3.0 ng mL⁻¹ and 0.2–10.1 ng mL⁻¹, respectively. In conclusion, this research presents a method for detecting pesticides in terms of miniaturization, and evaluation of environmental friendliness and applicability using modern GAPI, AGREEprep, and BAGI tools.

Analytical chemistry methods developmentPesticide Residue Analysis and SafetyAnalytical Chemistry and Chromatographypesticide residuesgrapesgreen analytical chemistry

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