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Analysis of Ochratoxin A in Wine by High-Resolution UHPLC-MS

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Abstract

A method for determination of ochratoxin A (OTA) in wines using a new-solid phase extraction clean-up procedure followed with ultra performance liquid chromatography (UHPLC)-Orbitrap MS based on two scan events (full-scan Fourier transform mass spectrometer [FTMS] and higher energy-induced collision dissociation[HCD] data-dependent MS/MS) in positive ionization mode has been developed. The limit of detection (LOD) was estimated at 0.46 μg l−1 for white wine, 0.53 and 0.54 μg l−1 for rosé and red wines, respectively. The limit of quantification (LOQ) was estimated at 1.57 μg l−1 in white wine, 1.77 and 1.81 μg l−1 in rosé and red wines. Recovery experiments were carried out with spiked samples at three concentration levels (2, 5 and 10 μg l−1). The OTA recoveries in spiked white wine samples varied from 69.6 % to 99.8 %, while the recoveries for rosé and red wine samples were in the range of 63.0–110.2 % and 63.6–103.2 %, respectively. Finally, based on the results, it is concluded that the combination of C18 cartridge with conventional particle packed columns and UHPLC LTQ-Orbitrap XL is an appropriate procedure for OTA analysis in wines.

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References

  • Alvito PC, Sizoo EA, Almeida CMM, van Egmond JP (2010) Occurrence of aflatoxins and ochratoxin A in baby foods in Portugal. Food Anal Methods 3:22

    Google Scholar 

  • AOAC (1995) Official Methods of Analysis of AOAC International. 16th edition. Arlington, VA, USA, AOAC International. 973.37: 37

  • Aresta A, Vatinno R, Palmisano F, Zambonin CG (2006) Determination of ochratoxin A in wine at sub ng/mL levels by solid-phase microextraction coupled to liquid chromatography with fluorescence detection. J Chromatogr A 1115:196

    Google Scholar 

  • Blesa J, Soriano JM, Moltó JC, Mañes J (2004) Concentration of ochratoxin A in wines from supermarkets and stores of Valencian Community (Spain). J Chromatogr A 1054:397

    Google Scholar 

  • Brera C, Soriano JM, Debegnach F, Miraglia M (2005) Exposure assessment to ochratoxin A from the consumption of Italian and Hungarian wines. Microchem J 79:109

    Google Scholar 

  • European Union (2009) Method validation and quality control procedures for pesticide residues analysis in food and feed. Document No. SANCO/10684/2009. 18

  • European Union (2002) Implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of results. Commission Decision 657/2002/EC. Off J Eur Union L 221:8

  • European Union (2006) Setting maximum levels for certain contaminants in foodstuffs. Commission Regulation 1881/2006/EC. Off J Eur Union L 364:5

    Google Scholar 

  • Folloni S, Bellocchi G, Kagkli DM, Pastor-Benito S, Aguilera M, Mazzeo A, Querci M, Van den Eede G, Ermolli M (2011) Development of an ELISA reverse-based assay to assess the presence of mycotoxins in cereal flour. Food Anal Methods 4:221

    Google Scholar 

  • Herebian D, Zühlke S, Lamshöft M, Spiteller M (2009) Multi-mycotoxin analysis in complex biological matrices using LC-ESI/MS: Experimental study using triple stage quadrupole and LTQ-Orbitrap. J Sep Sci 32:939

    Google Scholar 

  • Hernández MJ, García-Moreno MV, Durán E, Guillén D, Barroso CG (2006) Validation of two analytical methods for the determination of ochratoxin A by reversed-phased high-performance liquid chromatography coupled to fluorescence detection in musts and sweet wines from Andalusia. Anal Chim Acta 566:117

    Google Scholar 

  • Hussein HS, Brasel JM (2001) Toxicity, metabolism, and impact of mycotoxins on humans and animals. Toxicology 167:101

    Google Scholar 

  • JECFA (2001) Safety Evaluation of Certain Mycotoxins in Food: Fifty-sixth report of the Joint FAO/WHO Expert Committee on Food Additives. WHO technical report series no. 906. World Health Organization, Geneva

    Google Scholar 

  • Jornet D, Busto O, Guasch J (2000) Solid-phase extraction applied to the determination of ochratoxin A in wines by reversed-phase high-performance liquid chromatography. J Chromatogr A 882:29

    Google Scholar 

  • Juan C, Lino CM, Pena A, Moltó JC, Mañes J, Silveira I (2007) Determination of ochratoxin A in maize bread samples by LC with fluorescence detection. Talanta 73:246

    Google Scholar 

  • Kokkonen MK, Jestoi MN (2009) A multi-compound LC-MS/MS method for the screening of mycotoxins in grains. Food Anal Methods 2:128

    Google Scholar 

  • Lee HB, Magan N (2000) Impact of environment and interspecific interactions between spoilage fungi and Aspergillus ochraceus on growth and ochratoxin production in maize grain. Int J Food Microbiol 61:11

    Google Scholar 

  • Leitner A, Zöllner P, Paolillo A, Stroka J, Papadopoulou-Bouraoui A, Jaborek S, Anklam E, Lindner W (2002) Comparison of methods for the determination of ochratoxin A in wine. Anal Chim Acta 453:33

    Google Scholar 

  • Li J, Xie H, Yang B, Dong X, Feng L, Chen F, Jiang Y (2010) A comparative identification of ochratoxin A in longan fruit pulp by high performance liquid chromatography-fluorescence detection and electron spray ionization-mass spectrometry. Molecules 15:680

    Google Scholar 

  • Liu X, Yang JL, Li JH, Li XL, Li J, Lu XY, Shen JZ, Wang YW, Zhang ZH (2011) Analysis of water-soluble azo dyes in soft drinks by high resolution UPLC–MS. Food Addit Contam A 28:1315

  • 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 804:103

    Google Scholar 

  • Markaki P, Delpont-Binet C, Grosso F, Dragacci S (2001) Determination of ochratoxin A in red wine and vinegar by immunoaffinity high-pressure liquid chromatography. J Food Prot 64:533

    Google Scholar 

  • Nielen MW, van Engelen MC, Zuiderent R, Ramaker R (2007) Screening and confirmation criteria for hormone residue analysis using liquid chromatography accurate mass time-of-flight, fourier transform ion cyclotron resonance and orbitrap mass spectrometry techniques. Anal Chim Acta 586:122

    Google Scholar 

  • Pitt JJ (2009) Principles and applications of liquid chromatography-mass spectrometry in clinical biochemistry. Clin Biochem Rev 30:19

    Google Scholar 

  • Pohland AE, Schuller PL, Steyn PS, Van Egmond HP (1982) Physicochemical data for some selected mycotoxins. Pure Appl Chem 54:2219

    Google Scholar 

  • Ramos AJ, Labernia N, Marín S, Sanchis V, Magan N (1998) Effect of water activity and temperature on growth and ochratoxin production by three strains of Aspergillus ochraceus on a barley extract medium and on barley grains. Int J Food Microbiol 44:133

    Google Scholar 

  • Serra R, Mendonça C, Abrunhosa L, Pietri A, Venâncio A (2004) Determination of ochratoxin A in wine grapes: comparison of extraction procedures and method validation. Anal Chim Acta 513:41

    Article  CAS  Google Scholar 

  • Skrabáková Z, O'Halloran J, van Pelt FNAM, James KJ (2010) Food contaminant analysis at ultra-high mass resolution: application of hybrid linear ion trap-orbitrap mass spectrometry for the determination of the polyether toxins, azaspiracids, in shellfish. Rapid Commun Mass Spectrom 24:2966

    Article  Google Scholar 

  • Soleas GJ, Yan J, Goldberg DM (2001) Assay of ochratoxin A in wine and beer by high-pressure liquid chromatography photodiode array and gas chromatography mass selective detection. J Agric Food Chem 49:2733

    Google Scholar 

  • Studer-Rohr I, Dietrich DR, Schlatter J, Schlatter C (1995) The occurrence of ochratoxin A in coffee. Food Chem Toxicol 33:341

    Google Scholar 

  • van der Heeft E, Bolck YJC, Beumer B, Nijrolder AWJM, Stolker AAM, Nielen MWF (2009) Full-scan accurate mass selectivity of ultra-performance liquid chromatography combined with time-of-flight and orbitrap mass spectrometry in hormone and veterinary drug residue analysis. J Am Soc Mass Spectrom 20:451

    Google Scholar 

  • Var I, Kabak B (2007) Occurrence of ochratoxin A in Turkish wines. Microchem J 86:241

    Article  CAS  Google Scholar 

  • Visconti A, Pascale M, Centonze G (1999) Determination of ochratoxin A in wine by means of immunoaffinity column clean-up and high-performance liquid chromatography. J Chromatogr A 864:89

    Google Scholar 

  • Zain ME (2011) Impact of mycotoxins on humans and animals. J Saudi Chem Soc 15:129

    Google Scholar 

  • Zimmerli B, Dick R (1996) Ochratoxin A in table wine and grape-juice: Occurrence and risk assessment. Food Addit Contam 13:655

    Article  CAS  Google Scholar 

  • Zöllner P, Leitner A, Lubda D, Cabrera K, Lidner W (2000) Application of a chromolith speedROD RP-18e HPLC column: Determination of ochratoxin A in different wines by high-performance liquid chromatography-tandem mass spectrometry. Chromatographia 52:818

    Google Scholar 

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Acknowledgements

This work was funded by Science and Technology Planning Project of General Administration of Quality Supervision, Inspection and Quarantine (AQSIQ) of P.R. China (2011IK190, 2012IK145); and AQSIQ Industrial Public Service Scientific Research Project of P. R. China (201210029).

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Authors and Affiliations

  1. Beijing Entry–Exit Inspection and Quarantine Bureau, 6 Tianshuiyuan Jie, Chaoyang District, 100026, Beijing, China

    Jianhui Li, Xin Liu, Shen Han, Jing Li & Zhaohui Zhang

  2. Shandong Entry–Exit Inspection and Quarantine Bureau, No. 2, ZhongShan RD, ShiNan district, Qingdao, China

    Qin Xu

  3. Tianjin Entry–Exit Inspection and Quarantine Bureau, 30 Youyi Lu, Hexi District, 300201, Tianjin, China

    Hong Xu

  4. Thermo Fisher Scientific China, 27 Xinjinqiao Lu, Pudong District, 201206, Shanghai, China

    Yongwei Wang & Fei Liu

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  1. Jianhui Li
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  2. Xin Liu
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  3. Shen Han
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  4. Jing Li
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  5. Qin Xu
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  6. Hong Xu
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  7. Yongwei Wang
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  8. Fei Liu
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  9. Zhaohui Zhang
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Correspondence to Zhaohui Zhang.

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Li, J., Liu, X., Han, S. et al. Analysis of Ochratoxin A in Wine by High-Resolution UHPLC-MS. Food Anal. Methods 5, 1506–1513 (2012). https://doi.org/10.1007/s12161-012-9403-9

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  • DOI: https://doi.org/10.1007/s12161-012-9403-9

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