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Micro-solid phase extraction of ochratoxin A, and its determination in urine using capillary electrophoresis

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Abstract

We describe a simple, environmentally friendly and selective technique for the determination of ochratoxin A (OTA) in urine. It involves (a) the use of a molecularly imprinted polymer as a sorbent in micro-solid-phase extraction in which the sorbent is contained in a propylene membrane envelope, and (b) separation and detection by capillary electrophoresis (CE). Under optimized conditions, response is linear in the range between 50 and 300 ng mL−1 (with a correlation coefficient of 0.9989), relative standard deviations range from 4 to 8 %, the detection limit for OTA in urine is 11.2 ng mL−1 (with a quantification limits of 32.5 ng mL−1) which is lower than those of previously reported methods for solid-phase extraction combined with CE. The recoveries of OTA from urine spiked at levels of 50, 150 and 300 ng mL−1 ranged from 93 to 97 %.

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References

  1. Commission Regulation (EC) (2010) 105/2010 of 5 February 2010 amending Regulation (EC) No 1881/2006 setting maximum levels for certain contaminants in foodstuffs as regards ochratoxin A. Off. J. Eur. Communities, L 35/7

  2. Mally A, Dekant W (2009) Mycotoxins and the kidney: modes of action for renal tumor formation by ochratoxin A in rodents. Mol Nutr Food Res 53(4):467–478

    Article  CAS  Google Scholar 

  3. EFSA (European Food Safety Authority) (2004) Opinion of the scientific panel on contaminants in the food Chain on a request from the commission related to ochratoxin A (OTA) as undesirable substance in animal feed. Adopted on 22 September 2004. EFSA J 101:1

    Google Scholar 

  4. Manique R, Pena A, Lino CM, Moltó JC, Mañes J (2008) Ochratoxin A in the morning and afternoon portions of urine from Coimbra and Valencian populations. Toxicon 51(7):1281–1287

    Article  CAS  Google Scholar 

  5. Walker R, Larsen JC (2005) Ochratoxin A: previous risk assessments and issues arising. Food Addit Contam 22(suppl 1):6–9

    Article  CAS  Google Scholar 

  6. Pfohl-Leszkowicz A, Petkova-Bocharova T, Chernozemsky IN, Castegnaro M (2002) Balkan endemic nephropathy and associated urinary tract tumours: a review on aetiological causes and the potential role of mycotoxins. Food Addit Contam 19(3):282–302

    Article  CAS  Google Scholar 

  7. IARC (1993) Monograph on the Evaluation of Carcinogenic Risks to Humans, Some Naturally Occurring Substances: Food Items and Constituents, Heterocyclic Aromatic Amines and Mycotoxins; International Agency for Research on Cancer, Lyon, France, vol. 56, p 489

  8. Duarte SC, Pena A, Lino CM (2011) Human ochratoxin A biomarkers-from exposure to effect. Crit Rev Toxicol 41(3):187–212

    Article  Google Scholar 

  9. Akdemir C, Ulker OC, Basaran A, Ozkaya S, Karakaya A (2010) Estimation of ochratoxin A in some Turkish populations: an analysis in urine as a simple, sensitive and reliable biomarker. Food Chem Toxicol 48(3):877–882

    Article  CAS  Google Scholar 

  10. Vatinno R, Vuckovic D, Zambonin CG, Pawliszyn J (2008) Automated high-throughput method using solid-phase microextraction-liquid chromatography-tandem mass spectrometry for the determination of ochratoxin A in human urine. J Chromatogr A 1201(2):215–221

    Article  CAS  Google Scholar 

  11. Afsah-Hejri L, Jinap S, Mirhosseini H (2012) Ochratoxin A quantification: newly developed HPLC conditions. Food Control 23(1):113–119

    Article  CAS  Google Scholar 

  12. Paiga P, Morais S, Oliva-Teles T, Correia M, Delerue-Matos C, Duarte SC, Pena A, Lino CM (2012) Extraction of Ochratoxin A in bread samples by the QuEChERS methodology. Food Chem 135(4):2522–2528

    Article  CAS  Google Scholar 

  13. Corneli S, Maragos CM (1998) Capillary electrophoresis with laser-induced fluorescence: method for the mycotoxin Ochratoxin A. J Agric Food Chem 46(8):3162–3165

    Article  CAS  Google Scholar 

  14. Köller G, Rolle-Kampczyk U, Lehmann I, Popp P, Herbarth O (2004) Determination of Ochratoxin A in small volumes of human blood serum. J Chromatogr B 804(2):313–317

    Article  Google Scholar 

  15. Köller G, Rolle-Kampczyk U, Lehmann I, Popp P, Herbarth O (2006) Comparison of ELISA and capillary electrophoresis with laser-induced fluorescence detection in the analysis of Ochratoxin A in low volumes of human blood serum. J Chromatogr B 840(2):94–98

    Article  Google Scholar 

  16. Almeda S, Arce L, Benavente F, Sanz-Nebot V, Barbosa J, Valcárcel M (2009) Comparison of off- and in-line solid-phase extraction for enhancing sensitivity in capillary electrophoresis using ochratoxin as a model compound. Anal Bioanal Chem 394(2):609–615

    Article  CAS  Google Scholar 

  17. Almeda S, Arce L, Valcárcel M (2008) Combined use of supported liquid membrane and solid-phase extraction to enhance selectivity and sensitivity in capillary electrophoresis for the determination of ochratoxin A in wine. Electrophoresis 29(7):1573–1581

    Article  CAS  Google Scholar 

  18. Saito K, Ikeuchi R, Kataoka H (2012) Determination of ochratoxins in nuts and grain samples by in-tube solid-phase microextraction coupled with liquid chromatography-mass spectrometry. J Chromatogr A 1220:1–6

    Article  CAS  Google Scholar 

  19. Romero-González R, Frenich AG, Vidal JLM, Aguilera-Luiz MM (2011) Determination of ochratoxin A and T-2 toxin in alcoholic beverages by hollow fiber liquid phase microextraction and ultra high-pressure liquid chromatography coupled to tandem mass spectrometry. Talanta 82(1):171–176

    Article  Google Scholar 

  20. González-Peñas E, Leache C, Viscarret M, Pérez de Obanos A, Araguás C, López de Cerain A (2004) Determination of ochratoxin A in wine using liquid-phase microextraction combined with liquid chromatography with fluorescence detection. J Chromatogr A 1025(2):163–168

    Article  Google Scholar 

  21. Campone L, Piccinelli A, Rastrelli L (2011) Dispersive liquid-liquid microextraction combined with high-performance liquid chromatography-tandem mass spectrometry for the identification and the accurate quantification by isotope dilution assay of Ochratoxin A in wine samples. Anal Bioanal Chem 399(3):1279–1286

    Article  CAS  Google Scholar 

  22. Basheer C, Wong W, Makahleh A, Tameem AA, Salhin A, Saad B, Lee HK (2011) Hydrazone-based ligands for micro-solid phase extraction-high performance liquid chromatographic determination of biogenic amines in orange juice. J Chromatogr A 1218(28):4332–4339

    Article  CAS  Google Scholar 

  23. Kanimozhi S, Basheer C, Narasimhan K, Liu L, Koh S, Xue F, Choolani M, Lee HK (2010) Application of porous membrane protected micro-solid-phase-extraction combined with gas chromatography–mass spectrometry for the determination of estrogens in ovarian cyst fluid samples. Anal Chim Acta 687(1):56–60

    Article  Google Scholar 

  24. Feng Q, Zhao L, Lin JM (2009) Molecularly imprinted polymer as micro-solid phase extraction combined with high performance liquid chromatography to determine phenolic compounds in environmental water samples. Anal Chim Acta 650(1):70–76

    Article  CAS  Google Scholar 

  25. Maier NM, Buttinger G, Welhartizki S, Gavioli E, Lindner W (2004) Molecularly imprinted polymer-assisted sample clean-up of ochratoxin a from red wine: Merits and limitations. J Chromatogr B 804(1):103–111

    Article  CAS  Google Scholar 

  26. Lee TP, Saad B, Khayoon WS, Salleh B (2012) Molecularly imprinted polymer as sorbent in micro-solid phase extraction of ochratoxin A in coffee, grape juice and urine. Talanta 88:129–135

    Article  CAS  Google Scholar 

  27. González-Peñas E, Leache C, López De Cerain A, Lizarraga E (2006) Comparison between capillary electrophoresis and HPLC-FL for ochratoxin A quantification in wine. Food Chem 97(2):349–354

    Article  Google Scholar 

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Acknowledgments

Financial support of the work by a Universiti Sains Malaysia (USM) Postgraduate Research Grant Scheme (USM-RU-PRGS), 1001/PKIMIA/843052 and USM Research Fellowship Program is gratefully acknowledged.

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Correspondence to Bahruddin Saad.

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Lee, T.P., Saad, B., Salleh, B. et al. Micro-solid phase extraction of ochratoxin A, and its determination in urine using capillary electrophoresis. Microchim Acta 180, 1149–1156 (2013). https://doi.org/10.1007/s00604-013-1042-3

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  • DOI: https://doi.org/10.1007/s00604-013-1042-3

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