Abstract
A novel approach for the rapid analysis of ochratoxin A (OTA) in wine samples is presented. Mycotoxin was extracted and concentrated from matrix using dispersive liquid–liquid microextraction (DLLME). The final extract is analyzed by liquid chromatography coupled to positive electrospray ionization tandem mass spectrometry employing [2H5]-ochratoxin A as internal standard. Some important parameters, such as the nature and volume of extraction solvent and dispersive solvent, and salt effect were investigated and optimized to achieve the best extraction efficiency and higher enrichment factor. Under the optimum extraction condition, the method provided enrichment factor around 80 times and showed a high sensitivity with method detection and quantification limits of 0.005 and 0.015 ng mL−1, respectively. To test the accuracy of the analytical procedure, the optimized method was applied to the analysis of reference material T1755 (naturally contaminated white wine), with excellent results (accuracy of 103%) and showing a good precision with a CV (n = 6) of 5.8%. The proposed method, which is demonstrated to be quick, cheap, accurate and highly selective, was successfully applied to the analysis of Italian wines.

Analysis of ochratoxin A in wine by DLLME coupled to LC-MS/MS



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Pfohl-Leszkowicz A, Manderville R (2007) Mol Nutr Food Res 51:61–99
O’Brien E, Dietrich D (2005) CRC Crit Rev Toxicol 35:33–60
Evaluation of certain Mycotoxins: Ochratoxin A, WHO food additives series 47/FAO food and nutrition paper 74, 2001
Petkova-Botcharova T, Chernozemsky IN, Castegnaro M (1988) Food Addit Contam 5:299–301
IARC Monographs on the evaluation of carcinogenic risks to humans, vol 56: 489, IARC, Geneva, Switzerland, 1993
EFSA 2006. European food safety authority. Opinion of the scientific panel on contaminants in the food chain of the EFSA on a request from the commission related to ochratoxin A in food. (2006)EFSA J 365: 1
Commission Regulation (EC) 1881/2006 (2006) Off J Eur Union L 364:5–24
Mateo R, Medina Á, Mateo EM, Mateo F, Jiménez M (2007) Int J Food Microbiol 119:79–83
Visconti A, Perrone G, Cozzi G, Solfrizzo M (2008) Food Addit Contam 25:193–202
Monaci L, Palmisano F (2004) Anal Bioanal Chem 378:96–103
Barna Vetro I, Solti L, Teren L, Gyongyosi A, Szabo E, Wolfling A (1996) J Agric Food Chem 44:4071–4074
Flajs D, Domijan AM, Ivic D, Cvjetkovic B, Peraica M (2009) Food Control 20:590–592
Valenta H (1998) J Chromatogr A 815:75–92
Visconti A, Pascale M, Centonze G (2001) J AOAC Int 84:1818–1827
Flamini R, Panighel A (2006) Mass Spectrom Rev 25:741–774
Leitner A, Zöllner P, Paolillo A, Stroka J, Papadopoulou-Bouraoui A, Jaborek S, Anklam E, Lindner W (2002) Anal Chim Acta 453:33–41
Bacaloni A, Cavaliere C, Faberi A, Pastorini E, Samperi R, Laganà A (2005) J Agric Food Chem 53:5518–5525
Rychlik M, Asam S (2008) Anal Bioanal Chem 390:617–628
Stokvis E, Rosing H, Beijnen JH (2005) Rapid Commun Mass Spectrom 19:401–407
Rezaee M, Assadi Y, Hosseini MRM, Aghaee E, Ahmadi F, Berijani S (2006) J Chromatogr A 1116:1–9
Nagaraju D, Huang S-D (2007) J Chromatogr A 1161:89–97
García-López M, Rodríguez I, Cela R (2007) J Chromatogr A 1166:9–15
Rezaee M, Yamini Y, Shariati S, Esrafili A, Shamsipur M (2009) J Chromatogr A 1216:1511–1514
Fattahi N, Samadi S, Assadi Y, Hosseini MRM (2007) J Chromatogr A 1169:63–69
Montes R, Rodríguez I, Ramil M, Rubí E, Cela R (2009) J Chromatogr A 1216:5459–5466
Zhao E, Zhao W, Han L, Jiang S, Zhou Z (2007) J Chromatogr A 1175:137–140
Commission Decision 2002/657/EC (2002) Off J Eur Communities L 221:8–36
Commission Regulation (EC) 401/2006 (2006) Off J Eur Union L 70:12–34
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Campone, L., Piccinelli, A.L. & Rastrelli, L. 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, 1279–1286 (2011). https://doi.org/10.1007/s00216-010-4347-7
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DOI: https://doi.org/10.1007/s00216-010-4347-7

