Muzaffer TUNÇEL, Elif Mine Öncü KAYA, Ülkü Dilek UYSAL, Tufan GÜRAY

HPLC fluorescence determination of ochratoxin A utilizing a double internal standard and its application to poultry feed

A validated liquid chromatography method employing a fluorescence detector for the determination of ochratoxin A (OTA) was developed with double internal standard and it was applied to ten different poultry feeds. The analysis was performed in an octadecyl silane column using a solvent system [ACN:water:formic acid (50:50:1.25, v/v/v)] by isocratic elution. The flow rate and injection volume were 1 mL min^{-1} and 12 \mu L, respectively. Signals were detected at 278(\lambda_{ex})/315(\lambda_{em}) and 330(\lambda_{ex})/450(\lambda_{em}) nm between 0 and 8, and 8.01 and 20.0 min, respectively. The method was validated with precision, linearity, accuracy, limit of detection, limit of quantification, robustness, and stability. Good linearity (r^2 = 0.9998--0.9999) was achieved over a concentration range of 1.60 \times 10^{-8} M to 6.40 \times 10^{-6} M for OTA. LOD and LOQ values were 7.83 \times 10^{-10} M and 2.37 \times 10^{-9} M, and 2.01 \times 10^{-9} M and 6.10 \times 10^{-9} M for internal standard 1 (IS1) and internal standard 2 (IS2), respectively, on an interday basis. The method was applied to poultry feed samples. Good recovery data ranged between 79.10% and 85.57%, and 71.98% and 76.66%, and the RSD% values were in the range of 1.36--11.70 and 2.07--2.34 for IS1 and IS2, respectively.

Anahtar Kelimeler:

Animal feed and poultry feed, fluorescence detector, HPLC, mycotoxin, ochratoxin A

HPLC fluorescence determination of ochratoxin A utilizing a double internal standard and its application to poultry feed

Keywords:

Animal feed and poultry feed, fluorescence detector, HPLC, mycotoxin, ochratoxin A,

PDF

___

Kumar, V.; Basu, M.; Rajendran, T. Crop Protection 2008, 27, 891–905.
Grollman, A. P.; Jelakovic, B. J. Am. Soc. Nephro. 2007, 18, 2817.
Karbancioglu-G¨uler, F.; Heperkan, D. Anal. Chim. Acta 2008, 617, 32–36.
Toscani, T.; Moseriti, A.; Dossena, A.; Dall’Asta, C.; Simoncini, N.; Virgili, R. J. Chromatog. B 2007, 855, 242–248.
Araguas, C.; Gonz´alez-Pe˜nas, E.; L´opez de Cerain, A. Food Chem. 2005, 92, 459–464.
Vega, M.; Mu˜noz, K.; Sep´ulveda, C.; Aranda, M.; Campos, V.; Villegas, R.; Villarroel, O. Food Control 2009, 20, 631–634.
Kabak, B. Food Chem. Toxicol. 2009, 47, 348–352.
Aboul Enein, H. Y.; Kutluk, ¨O. B.; Altiokka, G.; Tun¸cel, M. Biomed. Chromatogr. 2002, 16, 470–474.
Commission Recommendation 2006/576/EC of 17 August 2006 on the Presence of Deoxynivalenol, Zearalenone,
OTA, T–2 and HT–2 and Fumonisins in Products Intended for Animal Feeding, L229 3–5, 2006.
Bragulat, M.; Mart´ınez, E.; Castell´a, G.; Caba˜nes, F. Int. J. Food. Microbiol. 2008, 126, 43–48.
Olsson, J.; Borjesson, T.; Lundstedt, T.; Schnurer, J. Int. J. Food. Microbiol. 2002, 72, 203–214.
Zollner, P.; Mayer-Helm, B. J. Chromatogr. A 2006, 1136, 123–169.
Gonz´alez-Pe˜nas, E.; Leache, C.; L´opez de Cerain, A.; Lizarraga, E. Food Chem. 2006, 97, 349–354.
Validation of Analytical Procedures: Methodology, The International Conference on Harmonization (ICH), Topic Q2B, CPMP/ICH/281/95, 1996.
Brera, C.; Soriano, J.; Debegnach, F.; Miraglia, M. Microchem. J. 2005, 79, 109–113.
Peraica, M.; Domijan, A. M.; Fuchs, R.; Luci, A.; Radi, B. Toxicol. Lett. 1999, 110, 105–112.
Koller, G.; Wichmann, G.; Rolle-Kampczyk, U.; Popp, P.; Herbarth, O. J. Chromatogr. B 2006, 840, 94–98.
Commission Directive 2002/26/EC of 13 March 2002, Laying Down the Sampling Methods and the Methods of
Analysis for the Official Control of the Levels of Ochratoxin a in Foodstuff, L75 38–43, 2002.
Scott, P.; Kanhere, S.; Lau, B. P. Y.; Lewis, D.; Hayward, S.; Ryan, J.; Kuiper-Goodman, T. Food Addit. Contam. 1998, 15, 555–562.