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Method Validation Using Normal and Weighted Linear Regression Models for Quantification of Pesticides in Mango (Mangifera indica L.) Samples

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Abstract

A fast and efficient method was developed and validated for the determination of pesticides in mangos, which uses the QuEChERS citrate and gas chromatography–mass spectrometry (GC–MS) techniques. A detailed statistical analysis was performed to study the matrix effect. The calibration model using the method of weighted least squares is used in cases, where heteroscedasticity is observed. The matrix effect was observed for most studied compounds using analytical curves based on a spiked matrix. The limits of detection were 0.0025–0.01 mg kg−1, and the limits of quantification (LOQ) were 0.008–0.03 mg kg−1. The LOQ values were minor or equal to the established MRLs by major regulatory agencies in Brazil (ANVISA), the United States (US-EPA), and Europe (CE). The compounds showed acceptable recovery levels of 71–109% with a standard deviation less than 15%. The method was applied to determine pesticide residues in mango samples. For 12 samples, five compounds (chloroneb, propachlor, α-chlordane, chlorpyrifos, DCPA, chlorobenzilate, and trans-permethrin) were detected, with contents of 0.004–0.042 mg kg−1. For chloroneb, propachlor, and α-chlordane, the found concentrations were above the maximum permitted residue limit, according to data from the European Commission.

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References

  1. Saúco VG (2004) Acta Hortic 645:107–116

    Article  Google Scholar 

  2. ANVISA—Agência Nacional de Vigilância Sanitária (2016). Monografias de agrotóxicos. http://portal.anvisa.gov.br/. Accessed 20 June 2016

  3. MAPA—Ministério da Agricultura, Pecuária e Abastecimento (2016) Sistema de agrotóxicos fitossanitários (AGROFIT). http://agrofit.agricultura.gov.br/agrofit_cons/principal_agrofit_cons. Accessed 23 June 2016

  4. USFDA (2015). Pesticides residues in food. United States Food and Drug Administration. http://www.fda.gov/ICECI/ComplianceManuals/CompliancePolicyGuidanceManual/ucm123236.htm. Accessed 08 Oct 2015

  5. European Commission Health and Consumer Protection Directorate-General (2013) Guidance document on analytical quality control and validation procedures for pesticide residues analysis in food and feed. SANCO 12571/2013

  6. Prestes OD, Adaime MB, Zanela R (2011) Sci Chromatogr 3:51–64

    Google Scholar 

  7. Prestes OD, Friggi CA, Adaime MB, Zanella R (2009) Quím Nova 32:1620–1634

    Article  CAS  Google Scholar 

  8. Silva RO, Castro RC, Milhome MAL, Nascimento RF (2014) Food Sci Technol LEB 59:21–25

    Article  Google Scholar 

  9. Anastassiades M, Lehotay SJ, Tajnbaher D, Schenck FJ (2003) J AOAC Int 86:412–431

    CAS  Google Scholar 

  10. Lehotay SJ, Son KA, Kwon H, Koesukwiwat U, Fu W, Mastovska K, Hoh E, Leepipatpiboon N (2010) J Chromatogr A 1217:2548–2560

    Article  CAS  Google Scholar 

  11. Wilkowska A, Biziuk M (2011) Food Chem 125:803–812

    Article  CAS  Google Scholar 

  12. Guedes JAC, Silva RO, Lima CG, Milhome MAL, Nascimento RF (2016) Food Chem 199:380–386

    Article  CAS  Google Scholar 

  13. Stöckelhuber M, Müller C, Vetter F, Mingo V, Lötters S, Wagner N, Bracher F (2017) Chromatographia 80:825–829

    Article  Google Scholar 

  14. Li Y, Chen Z, Zhang R, Luo P, Zhou Y, Wen S, Ma M (2016) Chromatographia 79:1165–1175

    Article  CAS  Google Scholar 

  15. Miller JN (1991) Analyst 116(1991):3–14

    Article  CAS  Google Scholar 

  16. Karnes HT, Shiu G, Shah VP (1991) Pharm Res 8:421–426

    Article  CAS  Google Scholar 

  17. Caulcutt R, Boddy R (1994) Statistics for analytical chemists. Chapman and Hall, London

    Google Scholar 

  18. Feinberg M (2007) J Chromatogr A 1158:174–183

    Article  CAS  Google Scholar 

  19. Dong J, Pan Y-X, Lv J-X, Sun J, Gong X-M, Li K (2011) Chromatographia 74:109–119

    Article  CAS  Google Scholar 

  20. Lee SW, Choi JH, Cho SK (2011) J Chromatogr A 1218:4366–4377

    Article  CAS  Google Scholar 

  21. Sousa JS, Castro RC, Andrade GA, Lima CG, Nascimento RF (2013) Food Chem 141:2675–2681

    Article  CAS  Google Scholar 

  22. Milhome MAL, Sousa JS, Andrade GA, Castro RC, Lima LK, Lima CG, Nascimento RF (2015) J Phys Conf Ser 575:012032

    Article  Google Scholar 

  23. Almeida AM, Castel-Branco MM, Falcão AC (2002) J Chromatogr B 774:215–222

    Article  CAS  Google Scholar 

  24. Miller JN, Miller JC (2010) Statistics and chemometrics for analytical chemistry. Pearson, Harlow

    Google Scholar 

  25. Cacoullos T (2001) Stat Probab Lett 54:1–3

    Article  Google Scholar 

  26. Mansilha C, Melo A, Rebelo H, Ferreira IMPLVO, Pinho O, Domingues VC, Pinho C, Gameiro P (2010) J Chromatogr A 1217:6681–6691

    Article  CAS  Google Scholar 

  27. Barbosa PGA, Martins FICC, Lima LK, Milhome MAL, Cavalcante RM, Nascimento RF (2017) Food Anal Methods (in press)

  28. Lehotay SJ, Mastovska K (2004) J Chromatogr A 1040:259–272

    Article  Google Scholar 

  29. Egoburo DE, Diaz Peña R, Kolender A, Pettinari MJ (2017) Chromatographia 80:1121–1127

    Article  CAS  Google Scholar 

  30. Pang N, Wang T, Hu J (2016) Food Chem 190:793–800

    Article  CAS  Google Scholar 

  31. Pinho GP, Neves AA, Queiroz MELR, Silvério FO (2009) Quím Nova 32:985–987

    Google Scholar 

  32. Zainudin BH, Salleh S, Mohamed R, Yap KC, Muhamad H (2015) Food Chem 172:585–595

    Article  CAS  Google Scholar 

  33. Páleníková A, Martínez-Domínguez G, Arrebola FJ, Romero-González R, Hrouzková S, Frenich AG (2015) Food Chem 173:796–807

    Article  Google Scholar 

  34. Masibo M, He Q (2008) Compr Rev Food Sci Food Saf 7:309–319

    Article  Google Scholar 

  35. Palmeira SMV, Gois LM, Souza LD (2012) Lat Am Appl Res 42:77–81

    Google Scholar 

  36. WEBBOOK NIST. Disponível em. http://webbook.nist.gov/chemistry/cas-ser.html. Accessed 24 Feb 2015

  37. Choi S, Kim S, Shin JY, Kim M, Kim J (2015) Food Chem 173:1236–1242

    Article  CAS  Google Scholar 

  38. European Union (EU) (2012) Pesticides residues MRLs. European Commission. http://ec.europa.eu/food/plant/pesticides/eu-pesticides-database/public/?event=pesticide.residue.selection&language=EN. Accessed 07 Oct 2015

  39. Savant RH, Banerjee K, Uttre SC, Patil SH, Dasgupta S, Ghaste MS, Adsule PG (2010) J Agric Food Chem 58:1447–1454

    Article  CAS  Google Scholar 

Download references

Acknowledgements

The authors gratefully the Conselho Nacional de Desenvolvimento Científico e Tecnológico—CNPq (Grant Number 405167/2015-6 and 304888/2014-1) and Fundação Cearense de Apoio ao Desenvolvimento Científico e Tecnológico—FUNCAP for financial support of this research and the UFC for providing the laboratory infrastructure for the chromatographic analysis.

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Authors and Affiliations

  1. Department of Analytical Chemistry and Physical Chemistry, Federal University of Ceara, R. Humberto Monte S/N, Pici, Fortaleza, Ceara, CEP: 60455-760, Brazil

    Fátima Itana Chaves Custódio Martins & Ronaldo Ferreira do Nascimento

  2. Federal Institute of Education, Science and Technology of Ceará, Av. Doutor Guarani, 317, Derby Clube, Sobral, Ceara, CEP: 62042-030, Brazil

    Pablo Gordiano Alexandre Barbosa

  3. Embrapa Agroindústria Tropical, Rua Doutora Sara Mesquita 2270, Campus do Pici, Fortaleza, Ceara, CEP: 60511-110, Brazil

    Guilherme Julião Zocolo

Authors
  1. Fátima Itana Chaves Custódio Martins
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  2. Pablo Gordiano Alexandre Barbosa
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  3. Guilherme Julião Zocolo
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  4. Ronaldo Ferreira do Nascimento
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Correspondence to Ronaldo Ferreira do Nascimento.

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Martins, F.I.C.C., Barbosa, P.G.A., Zocolo, G.J. et al. Method Validation Using Normal and Weighted Linear Regression Models for Quantification of Pesticides in Mango (Mangifera indica L.) Samples. Chromatographia 81, 677–688 (2018). https://doi.org/10.1007/s10337-018-3483-7

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  • DOI: https://doi.org/10.1007/s10337-018-3483-7

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