Brinco, JoãoCarvalho, RaquelSilva, Marco Gomes daGuedes, PaulaRibeiro, Alexandra B．Mateus, Eduardo P．2025-02-252025-02-252024-100021-9673PURE: 104658489PURE UUID: dc68207d-7a96-4ec7-b652-992796eb1a53ORCID: /0000-0003-1761-7376/work/166794378WOS: 001308245700001PubMed: 39236359Scopus: 85203013949ORCID: /0000-0002-5606-3591/work/178935817http://hdl.handle.net/10362/179814LAQV/REQUIMTE (UID/QUI/50006/2020). UI/BD/150867/2021. CEECIND/01969/2020. © 2024 The Author(s). Published by Elsevier B.V.A new method was evaluated and developed for the analysis of pesticides in sandy-loam soil by direct-immersion solid phase microextraction (DI-SPME) followed by gas chromatography tandem-mass spectrometry (GC–MS/MS) determination. Ten pesticides were selected based on a literature survey of the compounds reported to be present in EU soils. The extraction was performed using SPME LC-Tips, a new SPME configuration with the coated fibers attached to a disposable and easy-to-handle micropipette tip, which was immersed into a soil slurry made by the addition of an aqueous solution to the soil sample. Ten experimental parameters were evaluated with a Plackett-Burman design, after which the extraction time and percentage of organic solvent in the aqueous extraction were optimized separately. The two fiber chemistries available (PDMS/DVB and C18) were evaluated in parallel for the entire work. In the final method, slurry samples were made by adding an aqueous solution (6 % methanol v/v) to 2 g of soil. The fiber was conditioned and then inserted, for extraction, into the samples, stirred by a magnetic bar. Afterwards, the analytes were desorbed onto 100 µL of methanol. After the addition of analyte protectants (ethylglycerol, gulonolactone, and sorbitol) the extract was injected into the GC–MS/MS system. Isotopically labelled penconazole was used as internal standard. A calibration was performed by extracting spiked soil with analyte concentrations of 0.1–50 µg/kg. Coefficients of determination of the linear calibration were between 0.94–0.98 for the PDMS/DVB and 0.92–0.99 for the C18. Limits of detection range between 0.01–10 µg/kg for the PDMS/DVB and 0.1–10 µg/kg for the C18. Overall, the C18 analytically outperformed the PDMS/DVB but required a longer extraction time (120 min vs 75 min for the PDMS/DVB). This method allows automation and generates low residual toxic waste, having the potential to be introduced as a greener and simpler alternative to currently used sample preparation methodologies.2072223engAnalysisDirect immersion SPMEPesticideSoilsoil pesticide extractionjournal article10.1016/j.chroma.2024.465295https://www.scopus.com/pages/publications/85203013949