{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,2,14]],"date-time":"2026-02-14T00:47:41Z","timestamp":1771030061788,"version":"3.50.1"},"reference-count":50,"publisher":"MDPI AG","issue":"9","license":[{"start":{"date-parts":[[2025,4,26]],"date-time":"2025-04-26T00:00:00Z","timestamp":1745625600000},"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>Green coffee is essential in many tropical economies. Its cultivation often necessitates using pesticides that can leave behind residues harmful to human health. To ensure consumer safety, the European Community has set strict maximum residue limits (ranging from 0.01 to 1.0 mg\/kg) for pesticides in green coffee sold within Europe. However, the lack of official testing methods for neonicotinoids (NEOs) is a problem, as laboratories must spend resources and time developing and validating suitable analytical methods. This study developed and validated a method for the simultaneous analysis of seven NEOs frequently used in coffee cultivation: acetamiprid, clothianidin, dinotefuran, imidacloprid, nitenpyram, thiacloprid, and thiamethoxam. The proposed methodology uses Strata\u00ae-X PRO cartridges (solid-phase extraction) to remove interfering compounds present in the food matrix and high-performance liquid chromatography (HPLC), equipped with a diode array detector (DAD), to determine NEOs. The accuracy profile strategy validated the method\u2019s suitability for the intended application. NEO recovery rates above 97%; negligible matrix effects (&gt;93%); the linearity of the quantification method (R2 values above 0.99); relative biases and standard deviations below 5% and 6%, respectively; and an expected error rate less than 8% allowed to consider the method reliable for the intended objectives. Because of its low ecological impact and simple execution, this method can be used in routine analyses.<\/jats:p>","DOI":"10.3390\/molecules30091930","type":"journal-article","created":{"date-parts":[[2025,4,28]],"date-time":"2025-04-28T06:23:32Z","timestamp":1745821412000},"page":"1930","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":2,"title":["SPE-HPLC-DAD Dosage of Seven Neonicotinoids in Green Coffee"],"prefix":"10.3390","volume":"30","author":[{"given":"Serenella","family":"Seccia","sequence":"first","affiliation":[{"name":"Department of Pharmacy, University of Naples Federico II, Via Domenico Montesano 49, 80131 Napoli, Italy"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-1711-1236","authenticated-orcid":false,"given":"Stefania","family":"Albrizio","sequence":"additional","affiliation":[{"name":"Department of Pharmacy, University of Naples Federico II, Via Domenico Montesano 49, 80131 Napoli, Italy"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-1418-1431","authenticated-orcid":false,"given":"Irene","family":"Dini","sequence":"additional","affiliation":[{"name":"Department of Pharmacy, University of Naples Federico II, Via Domenico Montesano 49, 80131 Napoli, Italy"}],"role":[{"role":"author","vocabulary":"crossref"}]}],"member":"1968","published-online":{"date-parts":[[2025,4,26]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","unstructured":"Samoggia, A., and Fantini, A. (2023). Revealing the Governance Dynamics of the Coffee Chain in Colombia: A State-of-the-Art Review. Sustainability, 15.","DOI":"10.3390\/su151813646"},{"key":"ref_2","doi-asserted-by":"crossref","first-page":"110825","DOI":"10.1016\/j.foodres.2021.110825","article-title":"Coffee berry and green bean chemistry\u2014Opportunities for improving cup quality and crop circularity","volume":"151","author":"Hall","year":"2022","journal-title":"Food Res. Int."},{"key":"ref_3","doi-asserted-by":"crossref","first-page":"153018","DOI":"10.1016\/j.phymed.2019.153018","article-title":"The effect of green-coffee extract supplementation on obesity: A systematic review and dose-response meta-analysis of randomized controlled trials","volume":"63","author":"Gorji","year":"2019","journal-title":"Phytomedicine"},{"key":"ref_4","first-page":"67","article-title":"Dietary supplements in therapy to support weight reduction in obese patients","volume":"21","author":"Wawrzyniak","year":"2022","journal-title":"Acta Sci. Pol. Technol. Aliment."},{"key":"ref_5","doi-asserted-by":"crossref","first-page":"163","DOI":"10.1186\/s13643-023-02311-4","article-title":"Chlorogenic acid in green bean coffee on body weight: A systematic review and meta-analysis of randomized controlled trials","volume":"12","author":"Kanchanasurakit","year":"2023","journal-title":"Syst. Rev."},{"key":"ref_6","doi-asserted-by":"crossref","first-page":"18","DOI":"10.1016\/j.jconhyd.2018.08.008","article-title":"Environmental risk assessment for sustainable pesticide use in coffee production","volume":"219","author":"Azevedo","year":"2018","journal-title":"J. Contam. Hydrol."},{"key":"ref_7","doi-asserted-by":"crossref","first-page":"1041","DOI":"10.1007\/s41348-022-00628-1","article-title":"Pests and diseases regulation in coffee agroecosystems by management systems and resistance in changing climate conditions: A review","volume":"129","author":"Harelimana","year":"2022","journal-title":"J. Plant Dis. Prot."},{"key":"ref_8","doi-asserted-by":"crossref","unstructured":"Dantas, J., Motta, I.O., Vidal, L.A., Nascimento, E.F.M.B., Bilio, J., Pupe, J.M., Veiga, A., Carvalho, C., Lopes, R.B., and Rocha, T.L. (2021). A Comprehensive Review of the Coffee Leaf Miner Leucoptera coffeella (Lepidoptera: Lyonetiidae)\u2014A Major Pest for the Coffee Crop in Brazil and Others Neotropical Countries. Insects, 12.","DOI":"10.3390\/insects12121130"},{"key":"ref_9","doi-asserted-by":"crossref","first-page":"437","DOI":"10.1007\/s12020-022-03229-y","article-title":"Pesticides as endocrine disruptors: Programming for obesity and diabetes","volume":"79","author":"Miranda","year":"2023","journal-title":"Endocrine"},{"key":"ref_10","doi-asserted-by":"crossref","first-page":"325","DOI":"10.2174\/1573411013666170822161018","article-title":"Bisphenols and alkylphenols in food: From farm to table","volume":"14","author":"Seccia","year":"2018","journal-title":"Curr. Anal. Chem."},{"key":"ref_11","doi-asserted-by":"crossref","first-page":"59","DOI":"10.1016\/j.chemosphere.2017.10.149","article-title":"Human exposure to neonicotinoid insecticides and the evaluation of their potential toxicity: An overview","volume":"192","author":"Han","year":"2018","journal-title":"Chemosphere"},{"key":"ref_12","unstructured":"(2023, July 18). EU Pesticides Database. Available online: https:\/\/food.ec.europa.eu\/plants\/pesticides\/eu-pesticides-database_en."},{"key":"ref_13","doi-asserted-by":"crossref","first-page":"16","DOI":"10.1016\/j.chroma.2012.06.041","article-title":"A multi-residue method for pesticides analysis in green coffee beans using gas chromatography-negative chemical ionization mass spectrometry in selective ion monitoring mode","volume":"1251","author":"Pizzutti","year":"2012","journal-title":"J. Chromatogr. A"},{"key":"ref_14","doi-asserted-by":"crossref","first-page":"296","DOI":"10.5614\/j.math.fund.sci.2015.47.3.7","article-title":"QuEChERS method for the determination of pesticide residues in indonesian green coffee beans using liquid chromatography tandem mass spectrometry","volume":"47","author":"Harmoko","year":"2015","journal-title":"J. Math. Fund. Sci."},{"key":"ref_15","doi-asserted-by":"crossref","first-page":"167","DOI":"10.1016\/j.chroma.2014.12.016","article-title":"Analysis of organo-chlorine pesticides residue in raw coffee with a modified \u201cquick easy cheap effective rugged and safe\u201d extraction\/clean up procedure for reducing the impact of caffeine on the gas chromatography-mass spectrometry measurement","volume":"1376","author":"Bresin","year":"2015","journal-title":"J. Chromatogr. A"},{"key":"ref_16","doi-asserted-by":"crossref","first-page":"60","DOI":"10.1016\/j.foodchem.2015.05.035","article-title":"Flutriafol and Pyraclostrobin Residues in Brazilian Green Coffees","volume":"190","author":"Pacheco","year":"2016","journal-title":"Food Chem."},{"key":"ref_17","doi-asserted-by":"crossref","first-page":"3928","DOI":"10.1002\/jssc.201700579","article-title":"Fast analysis of quaternary ammonium pesticides in food and beverages using cation-exchange chromatography coupled with isotope-dilution high-resolution mass spectrometry","volume":"40","author":"Nardin","year":"2017","journal-title":"J. Sep. Sci."},{"key":"ref_18","doi-asserted-by":"crossref","first-page":"40","DOI":"10.1016\/j.aca.2017.11.077","article-title":"Simultaneous determination of 117 pesticides and 30 mycotoxins in raw coffee, without cleanup, by LC-ESI-MS\/MS analysis","volume":"1004","author":"Reichert","year":"2018","journal-title":"Anal. Chim. Acta"},{"key":"ref_19","doi-asserted-by":"crossref","first-page":"2115","DOI":"10.1002\/jssc.201901135","article-title":"Magnetic amino-functionalized hollow silica-titania microsphere as an efficient sorbent for extraction of pesticides in green and roasted coffee beans","volume":"43","author":"Asadi","year":"2020","journal-title":"J. Sep. Sci."},{"key":"ref_20","doi-asserted-by":"crossref","first-page":"139223","DOI":"10.1016\/j.foodchem.2024.139223","article-title":"Optimization and Validation of High Throughput Methods for the Determination of 132 Organic Contaminants in Green and Roasted Coffee Using GC-QqQ-MS\/MS and LC-QqQ-MS\/MS","volume":"449","author":"Gamal","year":"2024","journal-title":"Food Chem."},{"key":"ref_21","doi-asserted-by":"crossref","first-page":"26098","DOI":"10.1021\/acs.jafc.4c06366","article-title":"Alternative Method for Glyphosate Determination in Unroasted Green Coffee Beans by Liquid Chromatography Tandem Mass Spectrometry (LC-MS\/MS)","volume":"72","author":"Paiva","year":"2024","journal-title":"J. Agric. Food Chem."},{"key":"ref_22","doi-asserted-by":"crossref","first-page":"106928","DOI":"10.1016\/j.jfca.2024.106928","article-title":"A modified QuEChERS method for the generic and rapid determination of pesticides and mycotoxins in raw coffee beans by liquid chromatography","volume":"137","author":"Wang","year":"2025","journal-title":"J. Food Compost. Anal."},{"key":"ref_23","doi-asserted-by":"crossref","first-page":"44","DOI":"10.1016\/j.foodchem.2018.02.135","article-title":"Gas chromatography\u2013mass spectrometry determination of polycyclic aromatic hydrocarbons in baby food using QuEChERS combined with low-density solvent dispersive liquid\u2013liquid microextraction","volume":"257","author":"Petrarca","year":"2018","journal-title":"Food Chem."},{"key":"ref_24","doi-asserted-by":"crossref","unstructured":"Kamal El-Deen, A., and Shimizu, K. (2021). Modified \u03bc-QuEChERS coupled to diethyl carbonate-based liquid microextraction for PAHs determination in coffee, tea, and water prior to GC\u2013MS analysis: An insight to reducing the impact of caffeine on the GC\u2013MS measurement. J. Chromatogr. B Anal. Technol. Biomed. Life Sci., 1171.","DOI":"10.1016\/j.jchromb.2021.122555"},{"key":"ref_25","doi-asserted-by":"crossref","first-page":"295","DOI":"10.1093\/jaocint\/qsz019","article-title":"Review of analytical methods to detect adulteration in coffee","volume":"103","author":"Wang","year":"2020","journal-title":"J. AOAC Int."},{"key":"ref_26","doi-asserted-by":"crossref","first-page":"106592","DOI":"10.1016\/j.jfca.2024.106592","article-title":"Detection of 13 pyrethroid pesticides in jasmine (Jasminum sp.) by modified QuEChERS method and gas chromatography-tandem mass spectrometry","volume":"135","author":"Dai","year":"2024","journal-title":"J. Food Comp. Anal."},{"key":"ref_27","doi-asserted-by":"crossref","first-page":"4093","DOI":"10.1039\/D4AY00243A","article-title":"Application of the QuEChERS method combined with UHPLC-QqQ-MS\/MS for the determination of isoprocarb and carbaryl pesticides in Indonesian coffee","volume":"16","author":"Harmoko","year":"2024","journal-title":"Anal. Methods"},{"key":"ref_28","doi-asserted-by":"crossref","first-page":"138498","DOI":"10.1016\/j.foodchem.2024.138498","article-title":"Monitoring of seven pesticide residues by LC-MS\/MS in extra virgin olive oil samples and risk assessment for consumers","volume":"442","author":"Schiano","year":"2024","journal-title":"Food Chem."},{"key":"ref_29","doi-asserted-by":"crossref","first-page":"174","DOI":"10.1016\/j.chroma.2007.02.021","article-title":"Validation of analytical methods based on accuracy profiles","volume":"1158","author":"Feinberg","year":"2007","journal-title":"J. Chromatogr. A"},{"key":"ref_30","doi-asserted-by":"crossref","unstructured":"Hubert, P., Nguyen-Huu, J.J., Boulanger, B., Chapuzet, E., Cohen, N., Compagnon, P.A., Dew\u00e9, W., Feinberg, M., Laurentie, M., and Mercier, N. (2008). Harmonization of strategies for the validation of quantitative analytical procedures: A SFSTP proposal: Part IV. Examples of application. J. Pharm. Biomed. Anal., 48.","DOI":"10.1016\/j.jpba.2008.07.018"},{"key":"ref_31","doi-asserted-by":"crossref","unstructured":"Feinberg, M., Boulanger, B., Dew\u2019e, W., and Hubert, P. (2004). New advances in method validation and measurement uncertainty aimed at improving the quality of chemical data. Anal. Bioanal. Chem., 380.","DOI":"10.1007\/s00216-004-2791-y"},{"key":"ref_32","first-page":"1112","article-title":"Validation of a high-performance thin-layer chromatography\/densitometry method for the quantitative determination of glucosamine in a herbal dietary supplement","volume":"156","author":"Esters","year":"2006","journal-title":"J. Chromatogr. A"},{"key":"ref_33","doi-asserted-by":"crossref","first-page":"31","DOI":"10.1016\/j.chroma.2018.03.036","article-title":"Validation and application of analytical method for glyphosate and glufosinate in foods by liquid chromatography-tandem mass spectrometry","volume":"1549","author":"Liao","year":"2018","journal-title":"J. Chromatogr. A"},{"key":"ref_34","doi-asserted-by":"crossref","first-page":"12746","DOI":"10.1021\/acsomega.1c01056","article-title":"Chemometric Approach Based on Accuracy Profile and Data Chronological Distribution as a Tool to Detect Performance Degradation and Improve the Analytical Quality Control for Aflatoxins\u2019 Analysis in Almonds Using UPLC\u2013MS\/MS","volume":"6","author":"Ouakhssase","year":"2021","journal-title":"ACS Omega"},{"key":"ref_35","doi-asserted-by":"crossref","first-page":"114614","DOI":"10.1016\/j.foodres.2024.114614","article-title":"Targeted quantification and untargeted exploration of furan and derivatives in infant food by headspace extraction-gas chromatography-Q Exactive Orbitrap mass spectrometry","volume":"191","author":"Sayon","year":"2024","journal-title":"Food Res. Inter."},{"key":"ref_36","doi-asserted-by":"crossref","unstructured":"Seccia, S., Albrizio, S., Morelli, E., and Dini, I. (2024). Development and Validation of a High-Performance Liquid Chromatography Diode Array Detector Method to Measure Seven Neonicotinoids in Wheat. Foods, 13.","DOI":"10.3390\/foods13142235"},{"key":"ref_37","unstructured":"ISO (2020, November 06). ISO\/IEC 17025\u2014Testing and Calibration Laboratories. Available online: https:\/\/www.iso.org\/ISO-IEC-17025-testing-and-calibration-laboratories.html."},{"key":"ref_38","doi-asserted-by":"crossref","first-page":"239342","DOI":"10.1155\/2013\/239342","article-title":"A simple HPLC-DAD method for the analysis of melamine in protein supplements: Validation using the accuracy profiles","volume":"2013","author":"Montesano","year":"2013","journal-title":"J. Chem."},{"key":"ref_39","unstructured":"(2022, December 01). United States Pharmacopeia (USP). Stage 4 Harmonization General chapter Chromatography. Available online: https:\/\/www.usp.org\/sites\/default\/files\/usp\/document\/harmonization\/gen-chapter\/harmonization-november-2021-m99380.pdf."},{"key":"ref_40","doi-asserted-by":"crossref","unstructured":"Schiano, M.E., Sodano, F., Cassiano, C., Fiorino, F., Seccia, S., Rimoli, M.G., and Albrizio, S. (2022). Quantitative Determination of Bisphenol A and Its Congeners in Plant-Based Beverages by Liquid Chromatography Coupled to Tandem Mass Spectrometry. Foods, 11.","DOI":"10.3390\/foods11233853"},{"key":"ref_41","doi-asserted-by":"crossref","unstructured":"Seccia, S., and Dini, I. (2025). Development and Validation of an HPLC-DAD Method to Determine Alkylphenols in Milk. Beverages, 11.","DOI":"10.3390\/beverages11030059"},{"key":"ref_42","doi-asserted-by":"crossref","unstructured":"Mancusi, A., Seccia, S., Izzi, A., Coppola, D., Tessieri, M., Santini, A., and Dini, I. (2025). Chemometric Validation of a High-Performance Liquid Chromatography Method to Detect Ochratoxin A in Green Coffee. Beverages, 11.","DOI":"10.3390\/beverages11020032"},{"key":"ref_43","doi-asserted-by":"crossref","first-page":"135642","DOI":"10.1016\/j.foodchem.2023.135642","article-title":"Quantitative Determination of BPA, BPB, BPF and BPS Levels in Canned Legumes from Italian Market","volume":"416","author":"Schiano","year":"2023","journal-title":"Food Chem."},{"key":"ref_44","doi-asserted-by":"crossref","first-page":"125851","DOI":"10.1016\/j.foodchem.2019.125851","article-title":"Aptamer assisted ultrafiltration cleanup with high performance liquid chromatography-fluorescence detector for the determination of OTA in green coffee","volume":"310","author":"Moez","year":"2020","journal-title":"Food Chem."},{"key":"ref_45","doi-asserted-by":"crossref","first-page":"33","DOI":"10.5740\/jaoacint.18-0294","article-title":"Multiresidue Determination of Carbamate, Organophosphate, Neonicotinoid, and Triazole Pesticides in Roasted Coffee Using Ultrasonic Solvent Extraction and Liquid Chromatography-Tandem Mass Spectrometry","volume":"102","author":"Navickiene","year":"2019","journal-title":"J. AOAC Int."},{"key":"ref_46","doi-asserted-by":"crossref","first-page":"227","DOI":"10.1016\/j.trac.2007.01.009","article-title":"A Practical guide to analytical method validation, including measurement uncertainty and accuracy profiles","volume":"26","author":"Herrador","year":"2007","journal-title":"Trends Anal. Chem."},{"key":"ref_47","unstructured":"International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (2022). ICH Harmonised Tripartite Guideline. Validation of Analytical Procedures Q2(R2), International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use."},{"key":"ref_48","unstructured":"The European Commission (2023). Commission Regulation (EU) 2023\/915 of 25 April 2023 on Maximum Levels for Certain Contaminants in Food and Repealing Regulation (EC) No 1881\/2006. Off. J. Eur. Union, 19, 103\u2013157."},{"key":"ref_49","doi-asserted-by":"crossref","first-page":"106552","DOI":"10.1016\/j.jfca.2024.106552","article-title":"Development and validation of a HPLC-UV method for the quantification of major phospholipids in milk","volume":"134","author":"Ramani","year":"2024","journal-title":"J. Food Composit. Anal."},{"key":"ref_50","doi-asserted-by":"crossref","unstructured":"Kucharski, D., Drzewicz, P., Na\u0142\u0119cz-Jawecki, G., Mianowicz, K., Skowronek, A., and Giebu\u0142towicz, J. (2020). Development and Application of a Novel QuEChERS Method for Monitoring of Tributyltin and Triphenyltin in Bottom Sediments of the Odra River Estuary, North Westernmost Part of Poland. Molecules, 25.","DOI":"10.3390\/molecules25030591"}],"container-title":["Molecules"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/www.mdpi.com\/1420-3049\/30\/9\/1930\/pdf","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2025,10,9]],"date-time":"2025-10-09T17:22:05Z","timestamp":1760030525000},"score":1,"resource":{"primary":{"URL":"https:\/\/www.mdpi.com\/1420-3049\/30\/9\/1930"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2025,4,26]]},"references-count":50,"journal-issue":{"issue":"9","published-online":{"date-parts":[[2025,5]]}},"alternative-id":["molecules30091930"],"URL":"https:\/\/doi.org\/10.3390\/molecules30091930","relation":{},"ISSN":["1420-3049"],"issn-type":[{"value":"1420-3049","type":"electronic"}],"subject":[],"published":{"date-parts":[[2025,4,26]]}}}