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Liquid chromatography time-of-flight mass spectrometry following sorptive microextraction for the determination of fungicide residues in wine

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Abstract

This work evaluates the suitability of sorptive microextraction, using disposable silicone sorbents, and liquid chromatography time-of-flight mass spectrometry (LC-TOF-MS) for the determination of 15 fungicides in wine. Under optimized conditions, wine samples (10 mL) were diluted with the same volume of ultrapure water and poured in a glass vessel containing a magnetic stirrer and 4 g of sodium chloride. Extractions were performed at room temperature for 4 h, using an inexpensive silicone disk (12 μL volume) exposed directly to the sample. Thereafter, analytes were recovered with 0.2 mL of acetonitrile. The electrospray ionization (ESI) source was operated in the fast polarity switching mode obtaining, in the same injection, selective LC-MS records (extracted with a mass window of 10 ppm) of compounds rendering [M + H]+ and [M-H] ions. The method provided limits of quantification (LOQs) between 0.1 and 2.2 ng mL−1, linear response ranges up to 500 ng mL−1, relative recoveries from 75% to 117% and an inter-day variability below 15% for all analytes in red and white wine samples. The feasibility of in situ sample enrichment followed by delayed desorption and analysis is also assessed.

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References

  1. Flamini R, Panighel A (2006) Mass Spectrom Reviews 25:741–774

    Article  CAS  Google Scholar 

  2. Cus F, Basa Cesnik H, Velikonja Bolta S, Gregorcic A (2010) Food Control 21:1512–1518

    Article  CAS  Google Scholar 

  3. González-Rodríguez RM, Cancho-Grande B, Simal-Gándara J (2009) J Sci Food Agric 89:2625–2635

    Article  Google Scholar 

  4. Payá P, Anastassiades M, Mack D, Sigalova I, Tasdelen B, Oliva J, Barba A (2007) Anal Bioanal Chem 389:1697–1714

    Article  Google Scholar 

  5. Economou A, Botitsi H, Antoniou S, Tsipi D (2009) J Chromatogr A 1216:5856–5867

    Article  CAS  Google Scholar 

  6. Gilbert-López B, García-Reyes JF, Ortega-Barrales P, Molina-Díaz A, Fernández-Alba AR (2007) Rapid Commun Mass Spectrom 21:2059–2071

    Article  Google Scholar 

  7. Ferrer I, Thurman EM (2007) J Chromatogr A 1175:24–37

    Article  CAS  Google Scholar 

  8. Oliva J, Navarro S, Barba A, Navarro G (1999) J Chromatogr A 833:43–51

    Article  CAS  Google Scholar 

  9. de Melo Abreu S, Caboni P, Cabras P, Garau VL, Alves A (2006) Anal Chim Acta 573:291–297

    Article  Google Scholar 

  10. González-Rodríguez RM, Cancho-Grande B, Simal-Gándara J (2009) J Chromatogr A 1216:6033–6042

    Article  Google Scholar 

  11. Carpinteiro I, Ramil M, Rodríguez I, Cela R (2010) J Chromatogr A 1217:7484–7492

    Article  CAS  Google Scholar 

  12. Nozal MJ, Bernal JL, Jiménez JJ, Martín MT, Bernal J (2005) J Chromatogr A 1076:90–96

    Article  CAS  Google Scholar 

  13. Rial Otero R, Yague Ruiz C, Cancho Grande B, Simal Gandara J (2002) J Chromatogr A 942:41–52

    Article  CAS  Google Scholar 

  14. Millán S, Sampedro MC, Unceta N, Goicolea MA, Rodriguez E, Barrio RJ (2003) J Chromatogr A 995:135–142

    Article  Google Scholar 

  15. Ravelo-Pérez LM, Hernández-Borges H, Borges-Miquel TM, Rodríguez-Delgado MA (2007) Electrophoresis 28:4072–4081

    Article  Google Scholar 

  16. Sandra P, Tienpont B, Vercammen J, Tredoux A, Sandra T, David F (2001) J Chromatogr A 928:117–126

    Article  CAS  Google Scholar 

  17. Vinas P, Aguinaga N, Campillo N, Hernández-Córdoba M (2008) J Chromatogr A 1194:178–183

    Article  CAS  Google Scholar 

  18. Montero L, Popp P, Paschke A, Pawliszyn P (2004) J Chromatogr A 1025:17–26

    Article  CAS  Google Scholar 

  19. Burger BV, Marx B, Le Roux M, Burger WJG (2006) J Chromatogr A 1121:259–267

    Article  CAS  Google Scholar 

  20. van Pinxteren M, Paschke A, Popp P (2010) J Chromatogr A 1217:2589–2598

    Article  Google Scholar 

  21. Montes R, Rodríguez I, Rubi E, Cela R (2007) J Chromatogr A 1143:41–47

    Article  CAS  Google Scholar 

  22. Popp P, Bauer C, Paschke A, Montero L (2004) Anal Chim Acta 504:307–312

    Article  CAS  Google Scholar 

  23. Carpinteiro I, Abuín B, Rodríguez I, Ramil M, Cela R (2010) J Chromatogr A 1217:7208–7214

    Article  CAS  Google Scholar 

  24. Montes R, Rodriguez I, Rubi E, Bollaín MH, Cela R (2007) Anal Chim Acta 599:84–91

    Article  CAS  Google Scholar 

  25. Fontana AR, Rodríguez I, Ramil M, Altamirano JC, Cela R (2011) J Chromatogr A 1218:2165–2175

    Article  CAS  Google Scholar 

  26. Urruty L, Montury M (1996) J Agric Food Chem 44:3871–3877

    Article  CAS  Google Scholar 

  27. Trösken ER, Bittner N, Völkel W (2005) J Chromatogr A 1083:113–119

    Article  Google Scholar 

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Acknowledgments

Financial support from the Spanish Government and E.U. FEDER funds (projects CTQ2009-08377 and DE2009-0020) is acknowledged. A.R.F. thanks a short term formation fellowship to Fundación Carolina, Spain. M. R. acknowledges her contract to the Isidro Parga Pondal program (Xunta de Galicia).

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Correspondence to I. Rodríguez.

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Fig. S1

LC-MS chromatograms corresponding to fungicides quantified in a non-spiked white wine sample (code W3, Table 4). (PDF 309 kb)

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Fontana, A.R., Rodríguez, I., Ramil, M. et al. Liquid chromatography time-of-flight mass spectrometry following sorptive microextraction for the determination of fungicide residues in wine. Anal Bioanal Chem 401, 767–775 (2011). https://doi.org/10.1007/s00216-011-5127-8

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