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High-Throughput Methodology for the Determination of Carbamates in Food Supplements by UHPLC–MS/MS

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Abstract

Food supplements are increasingly consumed products that claim to have several benefits for health. In many cases, these supplements contain herbal products and, as a consequence, can be contaminated with pesticides used in crops. This study aimed to use a QuEChERS-based method and ultra-high performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) to determine carbamate residues in different food supplements, all of them containing different herbal products, such as Garcinia cambogia, Cynaras colymus, Equisetum arvense, soy lecithin, Spirulina maxima, Fucus vesiculosus, olive leaf and garlic extract. After testing different sorbents, the combination of PSA/C18 (75/25) provided the best clean-up effect. The method was validated in terms of linearity, matrix effect, limit of quantification, precision (intra and interday) and trueness. Good linearity (r 2 > 0.99) and precision lower than 16% (expressed as relative standard deviation) were obtained in all cases. Moreover, the recovery in all studied samples was within the acceptable range (71–104%), and limit of quantification was 0.8 µg kg−1. The method was proved to be successful as a quantitative method for carbamate residue analysis in various food supplements, which are known to be complex matrices.

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References

  1. Biesalski KH (2001) In: Kramer K, Hoppe PP, Packer L (eds) Nutraceuticals in health and disease prevention, 1st edn. Marcel Dekker, New York

    Google Scholar 

  2. Das L, Bhaumik E, Raychaudhuri U, Chakraborty R (2012) Role of nutraceuticals in human health. J Food Sci Technol 49:2173–2183

    Google Scholar 

  3. Majaz Q, MolviKhurshid I, Nazim S, Asir Q, Shoeb Q (2012) Nutraceuticals: importance and advances in medicine and health. Int Res J Pharm 4:71–73

    Google Scholar 

  4. Rishi KR (2006) Nutraceutical: borderline between food and drug. Pharm Rev. http://www.kppub.com/articles/herbal-safety-pharma-review-004/nutraceuticals-borderline-between-food-and-drugs.html. Accessed 21 June 2016

  5. Pandey M, Verma RK, Saraf SA (2010) Nutraceuticals: new era of medicine and health. Asian J Pharm Clin Res 3:11–15

    Google Scholar 

  6. EPA (2015) Benefits of pesticide use. http://www.epa.gov/oecaagct/ag101/pestbenefits.html. Accessed 21 June 2015

  7. Martínez-Domínguez G, Plaza-Bolaños P, Romero-González R, Garrido Frenich A (2014) Multiresidue method for the fast determination of pesticides in nutraceutical products (Camellia sinensis) by GC coupled to triple quadrupole MS. J Sep Sci 37:665–674

    Article  Google Scholar 

  8. Nieto-García JA, Romero-González R, Garrido Frenich A (2014) Determination of multi-class pesticide residue in dietary supplements from grape seed extracts by ultra-high-performance liquid chromatography coupled to triple quadrupole mass spectrometry. Food Addit Contam Part A 31:1550–1561

    Article  Google Scholar 

  9. Martínez-Domínguez G, Nieto-García JA, Romero-González R, Garrido Frenich A (2015) Application of QuEChERS based method for the determination of pesticides in nutraceutical products (Camellia sinensis) by liquid chromatography coupled to triple quadrupole tandem mass spectrometry. Food Chem 177:182–190

    Article  Google Scholar 

  10. Páleníková A, Martínez-Domínguez G, Arrebola FJ, Romero-González R, Hrouzková S, Garrido Frenich A (2015) Multifamily determination of pesticide residues in soya-based nutraceutical products by GC/MS–MS. Food Chem 173:796–807

    Article  Google Scholar 

  11. Regulation EC No 1924/2006 of the European Parliament and of the Council of 20 December 2006 on nutrition and health claims made on foods OJ L 404, 30.12.2006, p. 9. http://eur-lex.europa.eu/legal-content/EN/TXT/PDF/?uri=CELEX:02006R1924-20121129&from=EN. Accessed 21 June 2016

  12. Pennings EJ (2012) The emerging European nutraceuticals innovation system. Master thesis Science and Innovation Management, Faculty of Geosciences Theses, Universiteit Utrecht, Netherlands. http://dspace.library.uu.nl/bitstream/handle/1874/256565/Thesis%20Nutraceuticals%20Jef%20Pennings.pdf?sequence=1. Accessed 21 June 2016

  13. Coppens P, Fernandes da Silva M, Pettman S (2006) European regulations on nutraceuticals, dietary supplements and functional foods: a framework based on safety. Toxicology 221:59–74

    Article  CAS  Google Scholar 

  14. Ahmad F, Ashraf AS, Ahmad FA, Ansari JA, Siddiquee RA (2011) Nutraceutical market and its regulation. Am J Food Tech 6:342–347

    Article  Google Scholar 

  15. WHO (1986) Carbamate pesticides: a general introduction International program on chemical safety, environmental health criteria 64. http://www.inchem.org/documents/ehc/ehc/ehc64.htm. Accessed 21 June 2016

  16. Blasco C, Fernández M, Pena A, Lino C, Silveira IM, Font G, Picó Y (2003) Assessment of pesticide residues in honey samples from Portugal and Spain. J Agric Food Chem 51:8132–8138

    Article  CAS  Google Scholar 

  17. Sungur S, Tunur C (2012) Investigation of pesticide residues in vegetables and fruits grown in various regions of Hatay, Turkey. Food Addit Contam Part B 5:265–277

    Article  CAS  Google Scholar 

  18. Mondello L (2013) Nutraceuticals and separations. Anal Bioanal Chem 405:4589–4590

    Article  CAS  Google Scholar 

  19. Arienzo M, Cataldo D, Ferrara L (2013) Pesticide residues in fresh-cut vegetables from integrated pest management by ultra performance liquid chromatography coupled to tandem mass spectrometry. Food Control 3:1108–1115

    Google Scholar 

  20. Moreno-González D, Huertas-Pérez JF, Gámiz-Gracia L, García-Campaña AM (2015) High-throughput methodology for the determination of 33 carbamates in herbal products by UHPLC–MS/MS. Food Anal Method 8:2059–2068

    Article  Google Scholar 

  21. Moreno-González D, Huertas-Pérez JF, García-Campaña AM, Gámiz-Gracia L (2014) Determination of carbamates in edible vegetable oils by ultra-high performance liquid chromatography–tandem mass spectrometry using a new clean-up based on zirconia for QuEChERS methodology. Talanta 128:299–304

    Article  Google Scholar 

  22. Beyer A, Biziuk M (2008) Applications of sample preparation techniques in the analysis of pesticides and PCBs in food. Food Chem 108:669–680

    Article  CAS  Google Scholar 

  23. Martínez-Domínguez G, Plaza-Bolaños P, Romero-González R, Garrido-Frenich A (2014) Analytical approaches for the determination of pesticide residues in nutraceutical products and related matrices by chromatographic techniques coupled to mass spectrometry. Talanta 118:277–291

    Article  Google Scholar 

  24. González-Curbelo MA, Socas-Rodríguez B, Herrera-Herrera AV, González-Sálamo J, Hernández-Borges J, Rodríguez-Delgado MA (2015) Evolution and applications of the QuEChERS method. Trac Trend Anal Chem 71:169–185

    Article  Google Scholar 

  25. Anastassiades M, Lehotay JS, Stajnbaher D, Schenck JF (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 86:412–431

    CAS  Google Scholar 

  26. Niell S, Cesio V, Hepperle J, Doerk D, Kirsch L, Kolberg D, Scherbaum E, Anastassiades M, Heinzen H (2014) QuEChERS-based method for the multiresidue analysis of pesticides in beeswax by LC-MS/MS and GC × GC-TOF. J Agric Food Chem 62:3675–3683

    Article  CAS  Google Scholar 

  27. Kinsella B, O’Mahony J, Malone E, Moloney M, Cantwella H, Furey A, Danaher M (2009) Current trends in sample preparation for growth promoter and veterinary drug residue analysis. J Chromatogr A 1216:7977–8015

    Article  CAS  Google Scholar 

  28. Nguyen DT, Lee HM, Lee HG (2010) Rapid determination of 95 pesticides in soybean oil using liquid–liquid extraction followed by centrifugation, freezing and dispersive solid phase extraction as cleanup steps and gas chromatography with mass spectrometric detection. Microchem J 95:113–119

    Article  CAS  Google Scholar 

  29. Wilkowska A, Biziuk M (2011) Determination of pesticide residues in food matrices using the QuEChERS methodology, review. Food Chem 125:803–812

    Article  CAS  Google Scholar 

  30. European Commission (2015) Guidance document on analytical quality control and method validation procedures for pesticides residues analysis in food and feed, SANTE/11945/2015

  31. Kruve A, Künnapas A, Herodes K, Leito I (2008) Matrix effects in pesticide multi-residue analysis by liquid chromatography–mass spectrometry. J Chromatogr A 1187:58–66

    Article  CAS  Google Scholar 

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Acknowledgements

Thanks to Project Ref. AGL2015-70708-R (MINECO/FEDER, UE). DMG acknowledges MINECO for a Juan de la Cierva postdoctoral research contract (Ref. JCI-2014-19573).

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    Authors and Affiliations

    1. Department of Biochemistry, Faculty of Science, University of Bamenda, PO Box 39, Bambili, Cameroon

      Edouard Akono Nantia

    2. Department of Analytical Chemistry, Faculty of Sciences, University of Granada, Av. Fuentenueva s/n, 18071, Granada, Spain

      David Moreno-González, Ana M. García-Campaña & Laura Gámiz-Gracia

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    1. Edouard Akono Nantia
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    2. David Moreno-González
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    3. Ana M. García-Campaña
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    4. Laura Gámiz-Gracia
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    Correspondence to Laura Gámiz-Gracia.

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    The authors report no conflicts of interest with this study.

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    E. A. Nantia and D. Moreno-González contributed equally to this work.

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    Nantia, E.A., Moreno-González, D., García-Campaña, A.M. et al. High-Throughput Methodology for the Determination of Carbamates in Food Supplements by UHPLC–MS/MS. Chromatographia 80, 63–70 (2017). https://doi.org/10.1007/s10337-016-3211-0

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    • DOI: https://doi.org/10.1007/s10337-016-3211-0

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