Food Analytical Methods

, Volume 9, Issue 11, pp 3170–3178 | Cite as

Assessment of Dimethoate Residues in Olives at the Time of Harvest and After Brine Using QuEChERS Extraction

  • Paula Paíga
  • Carla Meneses
  • David H. Lopes
  • Manuela CorreiaEmail author
  • Cristina Delerue-Matos


Pesticides are among the most investigated priority pollutants in agricultural products due to their widespread use and toxicity. The olive fruit fly (Bactrocera oleae) is one of the main pests of the olive tree in Portugal, and for an effective protection against this plague, farmers rely mostly on the use of insecticides. Six olive samples were collected in four olive groves to evaluate the presence of residues of dimethoate used for the combat of olive fruit fly, in table olives at the time of harvest and after brine. QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) extraction was optimized, one factor at a time, applied to the olive samples, and the extracts were analysed using liquid chromatography–diode array detection. Positive results were obtained in two samples at the time of harvest (3.58 and 4.34 mg/kg fw). One olive grove was selected to test two concentrations of salt and assess their influence on the quantity of residues. After brine, dimethoate residues were not detected.


Dimethoate Table olives QuEChERS Liquid chromatography 


Compliance with Ethical Standards


This work received financial support from the European Union (FEDER funds through COMPETE) and National Funds (FCT, Fundação para a Ciência e Tecnologia) through project UID/QUI/50006/2013.

Conflict of Interest

Paula Paíga declares that she has no conflict of interest. Carla Meneses declares that she has no conflict of interest. David H. Lopes declares that he has no conflict of interest. Manuela Correia declares that she has no conflict of interest. Cristina Delerue-Matos declares that she has no conflict of interest.

Ethical Approval

This article does not contain any studies with human participants or animals performed by any of the authors.

Informed Consent

Not applicable


  1. Albi T, Vioque A, Albi MA (1970) Permanencia de residuos de los insecticidas dimetoato, endotion en aceitunas. Grasas y Aceites 21:147–53Google Scholar
  2. Amvrazi EG, Abanis TA (2008) Multiclass pesticide determination in olives and their processing factors in olive oil: comparison of different olive oil extraction systems. J Agric Food Chem 56:5700–9CrossRefGoogle Scholar
  3. Anastassiades M, Lehotay SJ, Stajnbaher D, Schenck FJ (2003) Fast and easy multiresidue method employing acetonitrile extraction/partitioning and dispersive solid-phase extraction for the determination of pesticide residues in produce. J AOAC Int 86:412–31Google Scholar
  4. Arroyo-López FN, Querol A, Bautista-Gallego J, Garrido-Fernández A (2008) Role of yeasts in table olive production. Int J Food Microbiol 128:189–96CrossRefGoogle Scholar
  5. Asehraou A, Peres C, Brito D, Faid M, Serhrouchni M (2000) Characterization of yeast strains isolated from bloaters of fermented green table olives during storage. Grasas y Aceites 51:225–9Google Scholar
  6. Asehraou A, Peres C, Faid M, Brito D (2002) Reducing the bloater spoilage incidence in fermented green olives during storage. Grasas y Aceites 53:330–4CrossRefGoogle Scholar
  7. Bakas I et al (2013) Computational and experimental investigation of molecular imprinted polymers for selective extraction of dimethoate and its metabolite omethoate from olive oil. J Chromatogr A 1274:13–8CrossRefGoogle Scholar
  8. Cabras P, Angioni A, Garau VL, Melis M, Pirisi FM, Karim M, Minelli EV (1997) Persistence of insecticide residues in olives and olive oil. J Agric Food Chem 45:2244–7CrossRefGoogle Scholar
  9. Campaniello D, Bevilacqua A, D’Amato D, Corbo MR, Altieri C, Sinigaglia M (2005) Microbial characterization of table olives processed according to Spanish and natural styles. Food Technol Biotechnol 43:289–94Google Scholar
  10. Cunha SC, Lehotay SJ, Mastovska K, Fernandes JO, Oliveira MBPP (2007) Evaluation of the QuEChERS sample preparation approach for the analysis of pesticide residues in olives. J Sep Sci 30:620–32CrossRefGoogle Scholar
  11. EN 15662 (2008) Foods of Plant Origin - Determination of Pesticide Residues Using GC-MS and/or LC-MS/MS Following Acetonitrile Extraction/Partitioning and Clean-up by Dispersive SPE. Retrieved on 2015-05-01.
  12. European Commission (2009) COMMISSION REGULATION (EC) No 1097/2009 of 16 November 2009. amending Annex II to Regulation (EC) No 396/2005 of the European Parliament and of the Council as regards maximum residue levels for dimethoate, ethephon, fenamiphos, fenarimol, methamidophos, methomyl, omethoate, oxydemeton-methyl, procymidone, thiodicarb and vinclozolin in or on certain products. Official Journal of the European Union. 17.11.2009, L 301/6 Retrieved on 2015-02-20
  13. FAO. Retrieved on 2015-03-08.
  14. Ferreira JR, Taínha AM (1983) Organophosphorus insecticide residues in olives and olive oil. Journal of Pest Science 14:167–72CrossRefGoogle Scholar
  15. Ferrer C, Gómez MJ, García-Reyes JF, Imma F, Thurman EM, Fernández-Alba AR (2005) Determination of pesticide residues in olives and olive oil by matrix solid-phase dispersion followed by gas chromatography/mass spectrometry and liquid chromatography/tandem mass spectrometry. J Chromatogr A 1069:183–94CrossRefGoogle Scholar
  16. Galeano-Diaz T, Guiberteau A, López Soto MD, Ortiz JM (2006) Determination of dimethoate in olive oil by adsorptive stripping square voltammetry. Electroanalysis 18:695–702CrossRefGoogle Scholar
  17. Gómez AHS, García PG, Navarro LR (2006) Elaboration of table olives. Grasas y Aceites 57:86–94Google Scholar
  18. Kanavouras A, Gazouli M, Leonidas LT, Petrakis C (2005) Evaluation of black table olives in different brines. Grasas y Aceites 56:106–15CrossRefGoogle Scholar
  19. Kowalski J, Lupo S, Cochran J (2014) Mitigating Matrix Effects: Examination of Dilution, QuEChERS, and Calibration Strategies for LC-MS/MS Analysis of Pesticide Residues in Diverse Food Types.
  20. Lehotay SJ (2011) QuEChERS sample preparation approach for mass spectrometric analysis of pesticide residues in foods. Methods in molecular biology (Clifton, NJ) 747:65–91CrossRefGoogle Scholar
  21. Lentza-Rizos C (1999) Pesticide residues in olives and in olive oil from a European perspective. Proceedings of International Symposium “Pesticides in Food in Mediterranean Countries”, Chia, Laguna, Cagliari, Italy 125-147Li Q, Wang X, Yuan D (2009) Solid-phase extraction of polar organophosphorous pesticides from aqueous samples with oxidized carbon nanotubes. J Environ Monit 11:439–44Google Scholar
  22. Maldonado MB, Zuritz CA, Miras N (2008) Influence of brine concentration on sugar and sodium chloride diffusion during the processing of the green olive variety Arauco. Grasas y Aceites 59:267–73Google Scholar
  23. Martins N, Carreiro EP, Simões M, Cabrita MJ, Burke AJ, Garcia R (2015) An emerging approach for the targeting analysis of dimethoate in olive oil: the role of molecularly imprinted polymers based on photo-iniferter induced “living” radical polymerization. Reactive and Functional Polymers 86:37–46CrossRefGoogle Scholar
  24. Matuszewski BK, Constanzer ML, Chavez-Eng CM (2003) Strategies for the assessment of matrix effect in quantitative bioanalytical methods based on HPLC-MS/MS. Anal Chem 75:3019–30CrossRefGoogle Scholar
  25. Method AOAC (2007) Official Methods of Analysis 2007.01, Pesticide Residues in Foods by Acetonitrile Extraction and Partitioning with Magnesium Sulfate. Retrieved on 2015-03-02.
  26. Miller JN, Miller JC (2000) Statistics for analytical chemistry. Pearson Education Limited, HarlowGoogle Scholar
  27. Oujji NB, Bakas I, Istamboulié G, Ait-Ichou I, Ait-Addi E, Rouillon R, Noguer T (2014) A simple colorimetric enzymatic-assay, based on immobilization of acetylcholinesterase by adsorption, for sensitive detection of organophosphorus insecticides in olive oil. Food Control 46:75–80CrossRefGoogle Scholar
  28. Olive Diseases and Pests (2010). Retrieved on 2015-04-29.
  29. Randazzo CL, Fava G, Tomaselli F, Romeo FV, Pennino G, Vitello E, Caggia C (2011) Effect of kaolin and copper based products and of starter cultures on green table olive fermentation. Food Microbiol 28:910–9CrossRefGoogle Scholar
  30. Rodrigues SA, Caldas SS, Furlong EB, Primel EG, Zanella R (2011) Optimization and validation of a method using modified quechers and LC-ESI-MS/MS for the determination of pesticides in onion. Quim Nov. 34:780–U762Google Scholar
  31. Sibbett GS, Fergunson L (2005) Olive production manual, 2nd edn. Division of Agriculture and Natural Resources, University of California, pp 1–10Google Scholar
  32. Tsatsakis AM, Tsakiris IN, Tzatzarakis MN, Agourakis ZB, Tutudaki M, Alegaki AK (2003) Three-year study of fenthion and dimethoate pesticides in olive oil from organic and conventional cultivation. Food Addit Contam 20:553–9CrossRefGoogle Scholar
  33. Tsoutsi C, Konstantinou I, Hela D, Albanis T (2006) Screening method for organophosphorus insecticides and their metabolites in olive oil samples based on headspace solid-phase microextraction coupled with gas chromatography. Anal Chim Acta 573–574:216–22CrossRefGoogle Scholar
  34. Yada S, Harris LO (2007) Safe Methods for Home Pickling. University of California, Division of Agricultural and Natural Resources. University of California, Division of Agricultural and Natural Resources. Publication 8267. Retrieved on 2015-11-01.
  35. Zhang ZL, Hong HS, Zhou JL, Yu G (2002) Occurrence and behaviour of organophosphorus insecticides in the River Wuchuan, southeast China. J Environ Monit 4:498–504CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media New York 2016

Authors and Affiliations

  • Paula Paíga
    • 1
  • Carla Meneses
    • 2
  • David H. Lopes
    • 2
  • Manuela Correia
    • 1
    Email author
  • Cristina Delerue-Matos
    • 1
  1. 1.REQUIMTE/LAQV, Instituto Superior de Engenharia do Porto, Instituto Politécnico do PortoPortoPortugal
  2. 2.Departamento de Ciências AgráriasAzorean Biodiversity Group (GBA, CITA-A) and Platform for Enhancing Ecological Research and Sustainability (PEERS), Universidade dos AçoresAngra do HeroísmoPortugal

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