Optimization of the determination of deoxynivalenol in corn samples by liquid chromatography and a comparison of two clean-up principles

Autor: Abramović Biljana F., Jajić Igor M., Jurić Verica B., Gaál Ferenc F.
Jazyk: angličtina
Rok vydání: 2005
Předmět:
Zdroj: Journal of the Serbian Chemical Society, Vol 70, Iss 7, Pp 1005-1013 (2005)
Druh dokumentu: article
ISSN: 0352-5139
1820-7421
DOI: 10.2298/JSC0507005A
Popis: The determination of deoxynivalenol (DON) in corn by liquid chromatography with DAD detection was optimized. The separations were achieved on a Hypersil ODS column (100 x 4.6 mm; particle size 5 μm) by isocratic elution (0.6 cm3/min), a mobile phase consisting of acetonitrile–water in the ratio of 16:84. UV Detection was performed at 220 nm. Linear calibration curves were constructed in the concentration range of 0.72 – 12.00 ng/μl (equivalent to 0.29 – 4.8 μg/g com). The detection limit measured as the signal-to-noise ratio (3:1) was 0.16 ng/μl for DON (equivalent to 0.06 μg/g corn). The efficiencies of two clean-up principles for crude corn extract were compared solid-phase and immunochemical extraction. The efficiency of solid-phase extraction was found to be higher, with a value of 92.7 % when MycoSep 225 columns were used, while its value was 97.6 % when self-made activated charcoal–alumina–Celite–cationic columns were used. In contrast, the efficiency of the immunochemical columns (IMA) was only 73.8%. It was also found that the self-made columns could be used at least three times in a row in that way differing from the MycoSep 225 columns, which could not be reused either with or without regeneration, as well as from the IMA columns, which had a regeneration efficiency of 53.6 %.
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