RAPID, SENSITIVE LIQUID-CHROMATOGRAPHIC METHOD FOR DETERMINATION OF ZEARALENONE AND ALPHA-ZEARALENOL AND BETA-ZEARALENOL IN WHEAT

  • 1 January 1984
    • journal article
    • research article
    • Vol. 67  (5) , 968-972
Abstract
A rapid, sensitive liquid chromatographic (LC) method is described for quantitative determination of zearalenone and .alpha.- and .beta.-zearalenol in wheat. The procedure incorporates an internal standard, zearalenone oxime, to facilitate quantitation and automated analysis. A sample, buffered with pH 7.8 phosphate, is extracted with water-ethanol-chloroform (2 + 50 + 75) and cleaned up. The final residue is dissolved in LC mobile phase and injected onto a reverse phase RP-18 column under the following conditions: water-methanol-acetonitrile (5 +3 + 2) mobile phase; fluorescence (excitation wavelength 236 nm, 418 nm cut-off emission filter)and UV (254 nm, range 0.0025 AU) detectors. The limit of detectability (twice backgroung) is 0.5 ng for zearalenone and .alpha.-zearalenol standards on the fluorescence detector and 4 ng for .beta.-zearalenol on the UV detector, which is equivalent to 20 .mu.g zearalenone and 20 .mu.g .alpha.-zearalenol/kg, and 160 .mu.g .beta.-zearalenol/kg feed. Standard curves are linear over the range 0-35 ng zearalenone and .alpha.-zearalenol on the fluorescence detector and 0-50 ng .beta.-zearalenol on the UV detector. Recoveries of all compounds are 87.5-101% in the range 0.1-3.0 mg/kg (ppm).