Skip to main content

Advertisement

Log in

Multiresidue Determination of Pesticides in Potato Tuber, Peel, and Pulp by QuEChERS and UHPLC-MS/MS

  • Published:
Food Analytical Methods Aims and scope Submit manuscript

Abstract

Pesticides have been widely used to control pests and weeds during food production or storage, but when used incorrectly, they can cause damage to human health and the environment. Thus, this study aimed to develop and validate a multiresidue method for the determination of pesticides in potatoes, as well as to evaluate the concentrations in the peel and pulp of the tuber. The method is based on the original QuEChERS procedure for sample preparation, with a clean-up step by dispersive solid phase extraction (d-SPE) using C18 as sorbent and determination by ultra-high performance liquid chromatography with tandem mass spectrometry (UHPLC-MS/MS). The method was validated for 82 pesticides at the spike levels 10, 25, and 50 µg kg−1 presenting adequate accuracy and precision results. The method is simple and effective, achieving a practical quantification limit of 10 µg kg−1 for most of the pesticides. In order to evaluate the proposed method, it was applied to commercial potato samples, and, subsequently, the distribution of pesticides in the peel and pulp part was evaluated indicating that some pesticides are concentrated in the peel and others in the pulp, depending on the physicochemical properties of the pesticides. The results showed the presence of several pesticides, including some prohibited for potato crops. The method was successfully applied in commercial samples and demonstrated to be effective for routine analysis.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Fig. 1

Similar content being viewed by others

Data Availability

All data generated or analyzed during this study are included in this published article.

References

  • Anastassiades M, Lehotay SJ, Štajnbaher 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 Intern 86:412–431

    Article  CAS  Google Scholar 

  • Anastassiades M, Scherbaum E, Tasdelen B, Stajnbaher D (2007) Crop protection, public health, environmental safety. Wiley-VCH, Weinheim, Germany, pp 439–458

    Book  Google Scholar 

  • Antunes-Kenyon and Kennedy, G. Tiametoxam: a new active ingredient review. Massachusetts: Massachusetts Pesticide Bureau, 2001, 37

  • ANVISA (Agencia Nacional de Vigilância Sanitária), Agrotóxicos e Toxicologia (2023) https://www.gov.br/anvisa/pt-br/assuntos/agrotoxicos/programa-de-analise-de-residuos-em-alimentos

  • Barchanska H, Danek M, Sajdak M, Turek M (2018) Review of sample preparation techniques for the analysis of selected classes of pesticides in plant matrices. Crit Rev Anal Chem 48:467–491

    Article  CAS  PubMed  Google Scholar 

  • Cabrera LC, Martins ML, Primel EG, Prestes OD, Adaime MB, Zanella R (2012) Dispersive solid phase extraction in the determination of residues and contaminants in food. Scientia Chromatographica 4:227–240

    Article  Google Scholar 

  • Cabrera LC, Caldas SS, Prestes OD, Primel EG, Zanella R (2016) Evaluation of alternative sorbents for dispersive solid-phase extraction clean-up in the QuEChERS method for the determination of pesticide residues in rice by liquid chromatography with tandem mass spectrometry. J Sep Sci 39:1945–1954

    Article  CAS  PubMed  Google Scholar 

  • Carbo L, Martins EL, Dores EF, Spadotto CA, Weber OL, De-Lamonia-Freire EM (2007) Acetamiprid, carbendazim, diuron and thiamethoxam sorption in two Brazilian tropical soils. J Environ Sci Health B 42:499–507

    Article  CAS  PubMed  Google Scholar 

  • Codex Alimentarius. Pesticides (2010) https://www.fao.org/fao-who-codexalimentarius/thematicareas/pesticides/en/

  • de Haan S and Rodriguez F (2016) “Potato origin and production.” Advances in Potato Chemistry and Technology, Academic Press 1–32

  • de Morais CR, Travençolo BAN, Carvalho SM, Beletti ME, Vieira SVS, Campus CF, de Campus JEO, Pererira BB, Carvalho NMP, de Rezende AAA, Spanó MA (2018) Ecotoxicological effects of the insecticide fipronil in Brazilian native stingless bees Melipona scutellaris (Apidae: Meliponini). Chemosphere 206:632–642

    Article  PubMed  Google Scholar 

  • EMBRAPA (2023) available in: www.embrapa.br/hortalicas/batata/colheita-e-poscolheita?fbclid=IwAR3UNHzwZ8GKoFIBZcfQBHH_TpZADV2nPUr423o4ZV0ToPRlX-9mHcO91to

  • FAO - Food and Agriculture Organization of the United Nations (2023) Crops and livestock products. Accessed via https://www.fao.org/faostat/en/#data/QCL/visualize on 8th February 2023.

  • Gao J, Wang J, Zuo M, Ma L, Cui Y, Yang T, Ding M (2015) A highly sensitive method for simultaneous determination of the quaternary ammonium pesticides chlormequat and mepiquat in pears and potatoes by modified QuEChERS-high performance liquid chromatography-tandem mass spectrometry. RSC Adv 5:5895–5903

    Article  CAS  Google Scholar 

  • Garcia EL, Carmo EL, Pádua JG, Leonel M (2015) Industrial processing potential of potato cultivars. Fitotecnia 45:1742–1747

    Google Scholar 

  • Hajslová J, Holadová K, Kocourek V, Poustka J, Godula M, Cuhra P, Kempný M (1998) Matrix-induced effects: a critical point in the gas chromatographic analysis of pesticide residues. J Chromatogr A 800:283–295

    Article  Google Scholar 

  • Ierna A, Parisini B (2014) Crop growth and tuber yield of “early” potato crop under organic and conventional farming. Sci Hortic 165:260–265

    Article  Google Scholar 

  • Lehotay SJ, Mastovská K, Lightfield A (2005) Use of buffering and other means to improve results of problematic pesticides in a fast and easy method for residue analysis of fruits and vegetables. J AOAC Intern 88:615–630

    Article  CAS  Google Scholar 

  • Lehotay SJ, Son KA, Kwon H, Koesukwiwat U, Fu W, Mastovska K, Hoh E, Leepipatpiboon N (2010) Comparison of QuEChERS sample preparation methods for the analysis of pesticide residues in fruits and vegetables. J Chromatogr A 1217:2548–2560

    Article  CAS  PubMed  Google Scholar 

  • Machado I, Gérez N, Pistón M, Heinzen H, Cesio MV (2017) Determination of pesticide residues in globe artichoke leaves and fruits by GC-MS and LC-MS/MS using the same QuEChERS procedure. Food Chem 227:227–236

    Article  CAS  PubMed  Google Scholar 

  • Martins ML, Kemmerich M, Prestes OD, Maldaner L, Jardim ICSF, Zanella R (2017) Evaluation of an alternative fluorinated sorbent for dispersive solid-phase extraction clean-up of the quick, easy, cheap, effective, rugged, and safe method for pesticide residues analysis. J Chromatogr A 1514:36–43

    Article  CAS  PubMed  Google Scholar 

  • Matsadiqa G, Hu H, Ren H, Zhou Y, Liu L, Cheng J (2010) Quantification of multi-residue levels in peach juices, pulps and peels using dispersive liquid–liquid microextraction based on floating organic droplet coupled with gas chromatography-electron capture detection. J Chromatogr B 819:2113–2118

    Google Scholar 

  • Nieto-García AJ, Romero-González R, Frenich AG (2015) Multi-pesticide residue analysis in nutraceuticals from grape seed extracts by gas chromatography coupled to triple quadrupole mass spectrometry. Food Control 47:369–380

    Article  Google Scholar 

  • Prestes OD, Friggi CA, Adaime MB, Zanella R (2009) QuEChERS - a modern sample preparation method for pesticide multiresidue determination in food by chromatographic methods coupled to mass spectrometry. Quim Nova 32:1620–1634

    Article  CAS  Google Scholar 

  • Prestes OD, Adaime MB, Zanella R (2011) QuEChERS: possibilities and trends in sample preparation for multiresidue determination of pesticides in food. Scientia Chromatographica 3:51–64

    Article  Google Scholar 

  • Rasche C, Fournes B, Dirks U, Speer K (2015) Multi-residue pesticide analysis (gas chromatography–tandem mass spectrometry detection) - improvement of the quick, easy, cheap, effective, rugged, and safe method for dried fruits and fat-rich cereals - benefit and limit of a standardized apple purée calibration (screening). J Chromatogr A 1403:21–31

    Article  CAS  PubMed  Google Scholar 

  • SANTE (EUROPEAN COMMISSION) Guidance document on analytical quality control and method validation procedures for pesticides residues analysis in food and feed. Document SANTE/11312/2021

  • Shimshoni JA, Bommuraj V, Chena Y, Sperling R, Barel S, Kaye Y, Fallik E (2019) Residual distribution kinetics of pesticides in cherry tomato peel, pulp, and fruit as a function of irrigation water salinity, household rinsing, and storage regimen. Agronomy 9:800

    Article  CAS  Google Scholar 

  • Tomer V, Sangha JK (2013) Vegetable processing at household level: effective tool against pesticide residue exposure. IOSR J Environ Sci Toxicol Food Technol 6:43–53

    Article  CAS  Google Scholar 

  • Wang J, Gong Z, Zhang T, Feng S, Wang J, Zhang Y (2017) Simultaneous determination of 106 pesticides in nuts by LC–MS/MS using freeze-out combined with dispersive solid-phase extraction purification. J Sep Sci 40:2398–2405

    Article  CAS  PubMed  Google Scholar 

Download references

Acknowledgements

The authors gratefully acknowledge the financial support and fellowships granted by the Brazilian agencies CNPq and CAPES.

Funding

This study was financed in part by the Coordenação de Aperfeiçoamento de Pessoal de Nível Superior—Brazil (CAPES)—Finance Code 001.

Author information

Authors and Affiliations

Authors

Contributions

Leonardo Rabello Amaral, Cleusa Fátima Zanchin and Luana Flores did the practical work and wrote the main manuscript. Karina Ues participated in the execution of the experimental work. Osmar D. Prestes and Renato Zanella coordinated the work. All authors reviewed the manuscript.

Corresponding author

Correspondence to Renato Zanella.

Ethics declarations

Competing interests

The authors declare no competing interests.

Ethical Approval

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

Informed Consent

Informed consent was obtained from all individual participants included in the study.

Conflict of Interest

Leonardo Rabello Amaral declares that he has no conflict of interest. Cleusa Fátima Zanchin declares that she has no conflict of interest. Luana Flores declares that she has no conflict of interest. Karina Ues declares that she has no conflict of interest. Osmar D. Prestes declares that he has no conflict of interest. Renato Zanella declares that he has no conflict of interest.

Additional information

Publisher's Note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Supplementary Information

Below is the link to the electronic supplementary material.

Supplementary file1 (DOCX 59 KB)

Rights and permissions

Springer Nature or its licensor (e.g. a society or other partner) holds exclusive rights to this article under a publishing agreement with the author(s) or other rightsholder(s); author self-archiving of the accepted manuscript version of this article is solely governed by the terms of such publishing agreement and applicable law.

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Amaral, L.R., Zanchin, C.F., Floriano, L. et al. Multiresidue Determination of Pesticides in Potato Tuber, Peel, and Pulp by QuEChERS and UHPLC-MS/MS. Food Anal. Methods 16, 771–780 (2023). https://doi.org/10.1007/s12161-023-02471-y

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s12161-023-02471-y

Keywords

Navigation