Determination of ochratoxin a in grape wines after dispersive liquid–liquid microextraction using high performance thin layer and liquid chromatography– fluorescence detection

Bu çalışmada, kırmızı ve beyaz üzüm şaraplarında okratoksin A analizine yönelik dispersif sıvı-sıvı mikroekstraksiyon yöntemi geliştirildi. En iyi ekstraksiyon verimini elde etmek için ekstraksiyon çözücüsü ve dispersif çözücünün türü ve hacmi, ekstraksiyon zamanı, tuz etkisi gibi parametrelerin optimizasyonu gerçekleştirildi. Yöntemin 0.03-1.00 μg L-1 derişim aralığında doğrusal olduğu belirlenmiştir. Optimum koşullar altında, ekstraksiyon geri kazanımı % 63.9 ve zenginleştirme faktörü 34.5 olarak belirlendi.

Türk üzüm şaraplarındaki okratoksin a’ nın dispersif sıvı-sıvı mikroekstraksiyonu sonrası yüksek performanslı ince tabaka ve sıvı kromatografisi- floresans yöntemiyle tayini

In this study, a method was developed for analyzing ochratoxin A in wines using dispersive liquid–liquid microextraction combined with thin layer and liquid chromatography. Parameters such as type and volume of extraction solvent and dispersive solvent, extraction time and effect of salt were optimized to obtain the best extraction result. The linearity of response was employed in the concentration range of ochratoxin A in wines from 0.03-1.00 μg L-1. Under the optimum conditions, the extraction recovery as 63.9% and the enrichment factor as 34.5 were established.

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1. JECFA (Joint FAO/WHO Expert Committee on Food Additives), Ochratoxin A, Safety evaluation of certain mycotoxins in food, IPCS-WHO, Geneva (2001) 281. Series 47.
2. European Commission Report (1999), Opinion on the relationship between the use of plant protection products on food plants and the occurrence of mycotoxins in foods, European Commission SCP/RESI063, Belgium.
3. Commission Regulation EC No. 472/2002 of 12 March 2002 amending Regulation (EC) No 466/2001 setting maximum levels for certain contaminants in foodstuffs, Official J. EU, L75, 18–20, 16.03.2002.
4. European Commission, Directorate-General Health and Consumer Protection, Assessment of dietary intake of ochratoxin A by the population of EU member states (2002) Scientific Cooperation Task Reports. Task 3.2.7.
5. E. Petzinger, K. Ziegler, Ochratoxin A from a toxicological perspective, J. Vet. Pharmacol. Ther., 23 (2000) 91.
6. A. Pfohl-Leszkowicz, T. Petkova-Bocharova, IN. Chermozemsky, M. Castegnaro, Balkan endemic nephropathy and associated urinary tract tumours: a review on aetiological causes and the potential role of mycotoxins, Food Addit. Contam. A, 19 (2002) 282.
7. T. Horvath, B.L. Upham, V. Ganev, J.E. Trosko, Determination of the epigenetic effects of ochratoxin in a human kidney and a rat liver epithelial cell line, Toxicon, 40 (2002) 273.
8. T. Kuiper-Goodman, PM. Scott, Risk assess- ment of the mycotoxin ochratoxin A. App. Biomed. Enviro. Sci., 2 (1989) 179.
9. Official Journal of the European Union, Commision Regulation (EC) No 123/2005 of 26 January 2005 amending Regulation (EC) No 466/2001 as regards ochratoxin A.
10. C. Brera, S. Grossi, B. De Santis, A. Miraglia, Automated HPLC Method for the Determination of Ochratoxin A in Wine Samples, J. Liq. Chromatogr., Related Technol. 26 (2003) 119.
11. N. Ratola Barros, T. Simões, A. Cerdeira, A. Venâncio, A. Alves, Worlwide in ter- laboratory study on the determination of ochratoxin A in different wine type samples, Talanta, 70(2006)720.
12. Official Methods of Analysis, J of AOAC International, 59, 666 (1990), Section 976, 22.
13. A.W. Schaafsma, R.W. Nicol, M.E. Savard, R.C. Sinha, L.M. Reid, G. Rottinghaus, Analysis of Fusarium toxins in maize and wheat using thin layer chromatography, Mycopathologia, 142 (1998) 107.
14. L. Lin, J. Zhang Wang, Y. Wang, J. Chen, Thin layer chromatography of mycotoxins and comparison with other chromotographic methods, J. Chromatogr., A, 815 (1998) 3.
15. M.L. Martinsy, A. Gimeno, H.M. Martinsy, F. Bernardo, Co- occurance of patulin and citrinin in Portuguese apples with rotten spots, Food Addit. Contam. A, 19 (2002) 568.
16. I. Var, B. Kabak, Occurance of ochratoxin A in Turkish wines, Microchem. J., 86 (2007) 241.
17. E. González-Peñas, C. Leache, A López de Cerain, E. Lizarraga, Comparison between capillary electrophoresis and HPLC-FL for ochratoxin A quantification in wine, Food Chem., 97 (2006) 349.
18. M.A. Hernandez, GM. Valme, E. Duran, D. Guillen, C.G. Barroso, Validation of two analytical methods fot 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 (2006) 117.
19. D. Briones-Reyes, L. Gomez-Martinez, R. Cueva-Rolon, Zearalenone contamination in corn for human consumption in the state of Tlaxcala, Mexico, Food CHem., 100 (2007) 693.
20. M. Rezaee, Y. Assadi, M.R.M. Hosseini, E. Aghaee, F. Ahmadi, S. Berijani, Determination of organic compounds in water using dispersive liquid–liquid microextraction, J. Chromatogr. A, 1116 (2006) 1.
21. M.A. Farajzadeh, M. Bahram, J.A. Jonsson, Dispersive liquid- liquid microextraction followed by high-performance liquid chromatgoraphy- diode array detection as an efficient and sensitive technique for determination of antioxidants, Anal. Chim. Acta, 591 (2007) 69.
22. R. Montes, I. Rodríguez, E. Rubí, R. Cela, Dispersive liquid -liquid microextraction applied to the simultaneous derivatization and concentration of triclosan and methyltriclosan in water samples, J. Chroma. A, 1216 (2009) 205.
23. H. Farahani Norouzi, R. Dinarvand, M.R. Ganjali, Development of dispersive liquid- liquid microextraction combined with gas chromatgraphy- mass spectrometry as a simple, rapid and highly sensitive method for the determination of phthalate esters in water samples, J. Chroma. A, 1172 (2007) 105.
24. J. Xiong, B. Hu, Comparison of hollows fiber liquid phase microextraction and dispersive liquid-liquid microextraction for the deter- mination of organosulfur pesticides in environmental and beverage samples by gas chromatography with flame photometic detection, J. Chroma. A, 1193 (2008) 7.
25. R.R. Kozani, Y. Assadi, F. Shemirani, M.R.M. Hosseini, M.R. Jamali, Determination of Trihalomethanes in Drinking Water by Dispersive Liquid-Liquid Microextraction then Gas Chromatography with Electron- Capture Detection, Chromatographia, 66 (2007) 81.
26. H. Sereshti, M. Karimi, S. Samadi, Application of response surface method for optimization of dispersive liquid-liquid microextraction of water-soluble components of Rosa damascena Mill. essential oil, J. Chroma. A, 1216 (2009) 198.
27. K. Helrich (1990) Official Methods of Analysis, AOAC Int., 15th edn. Section 974.18.