{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,9,27]],"date-time":"2026-09-27T19:17:31Z","timestamp":1790536651861,"version":"4.1.0"},"reference-count":35,"publisher":"MDPI AG","issue":"9","license":[{"start":{"date-parts":[[2026,4,27]],"date-time":"2026-04-27T00:00:00Z","timestamp":1777248000000},"content-version":"vor","delay-in-days":0,"URL":"https:\/\/creativecommons.org\/licenses\/by\/4.0\/"}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":["Molecules"],"abstract":"<jats:p>This study presents a novel approach for optimizing GC-MS\/MS performance and ensuring the reproducibility of pesticide residue analysis across diverse food matrices. Analysis of thermally treated (100\u2013280 \u00b0C) extracts using GC-MS (scan mode) and FTIR revealed that strawberry and dry mint contain significantly higher concentrations of non-volatile co-extractives of varying chemical natures compared to fennel seeds. It was further elucidated that polar non-volatile co-extractives exhibit a more pronounced negative impact on analytical performance. Consequently, a synergistic approach was developed for strawberry analysis, combining end-column back-flushing with the application of fennel extract as a Natural Analyte Protectant (NAP). For dry mint, optimal results were achieved through a different approach: standard forward carrier gas cleaning combined with a fivefold sample dilution. The developed protocols enabled the efficient analysis of 195 pesticides in strawberries, all achieving LOQs of 0.01 mg\/kg. Results demonstrated high precision (RSD &lt; 3% for most analytes) and excellent recoveries (90\u2013110%) at 0.01 and 0.05 mg\/kg. Furthermore, 154 and 186 pesticides were successfully validated in dry mint with LOQs of 0.01 and 0.05 mg\/kg, respectively. This research demonstrates that efficient column cleaning can be achieved through either back-flushing or the same forward-flow of the carrier gas, depending on whether the non-volatile co-extractives are polar or non-polar. Finally, ethyl acetate (EtOAc) fennel extract is introduced as a highly effective NAP, which is especially advantageous for samples lacking endogenous volatile components while simultaneously containing high concentrations of polar co-extractives. Pesticide residue monitoring was applied for 20 commercial samples, demonstrating high sensitivity. While strawberry samples exhibited excellent regulatory compliance and a total absence of chlorpyrifos, herbal matrices showed a higher chemical burden characterized by multi-residue co-occurrence and MRL exceedances.<\/jats:p>","DOI":"10.3390\/molecules31091449","type":"journal-article","created":{"date-parts":[[2026,4,28]],"date-time":"2026-04-28T07:49:36Z","timestamp":1777362576000},"page":"1449","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":1,"title":["The Impact of Volatile and Non-Volatile Co-Extracted Matrix Components on the Reproducible Residue Analysis of Pesticides Using GC-MS\/MS"],"prefix":"10.3390","volume":"31","author":[{"given":"Abd-Alrahman H.","family":"Abo-Gida","sequence":"first","affiliation":[{"name":"Central Laboratory of Residue Analysis of Pesticides and Heavy Metals in Foods, Agricultural Research Center, Dokki, Giza P.O. Box 12311, Egypt"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Al-Thabiani","family":"Aziz","sequence":"additional","affiliation":[{"name":"Department of Biology, Faculty of Science, University of Tabuk, Tabuk 71491, Saudi Arabia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Muhammed","family":"Issa","sequence":"additional","affiliation":[{"name":"Central Laboratory of Residue Analysis of Pesticides and Heavy Metals in Foods, Agricultural Research Center, Dokki, Giza P.O. Box 12311, Egypt"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-7232-9911","authenticated-orcid":false,"given":"Sherif M.","family":"Taha","sequence":"additional","affiliation":[{"name":"Central Laboratory of Residue Analysis of Pesticides and Heavy Metals in Foods, Agricultural Research Center, Dokki, Giza P.O. Box 12311, Egypt"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Amadeo R.","family":"Fern\u00e1ndez-Alba","sequence":"additional","affiliation":[{"name":"European Union Reference Laboratory for Pesticide Residues in Fruit & Vegetables, Department of Chemistry and Physics, University of Almer\u00eda, 04120 Almer\u00eda, Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"1968","published-online":{"date-parts":[[2026,4,27]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","first-page":"72","DOI":"10.1016\/j.talanta.2017.05.068","article-title":"Matrix interference evaluation employing GC and LC coupled to triple quadrupole tandem mass spectrometry","volume":"174","author":"Lozano","year":"2017","journal-title":"Talanta"},{"key":"ref_2","doi-asserted-by":"crossref","first-page":"241","DOI":"10.1016\/j.chroma.2007.01.018","article-title":"Matrix-induced response enhancement in pesticide residue analysis by gas chromatography","volume":"1158","author":"Poole","year":"2007","journal-title":"J. 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