Development of a multiresidue method for analysis of major Fusarium mycotoxins in corn meal using liquid chromatography/tandem mass spectrometry

A sensitive and reliable liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI‐MS/MS) method has been developed to determine, in a single run, eight trichothecenes, three fumonisins, zearalenone and α ‐zearalenol, in corn meal samples. LC and MS conditions were varied to find the best compromise in terms of sensitivity and separation. An acceptable compromise was obtained using a C 18 column thermostatted at 45°C and a mobile phase gradient of methanol/water with 10 mmol/L formate buffer (pH 3.8). A multiple reaction monitoring program, in which fumonisins and trichothecenes (except nivalenol and deoxynivalenol) are acquired in positive ESI as [M+H] + or [M+NH 4 ] + , and all other compounds in negative ESI, was developed to match appropriate retention time windows. Sample preparation used a simple homogenization of the corn meal sample with acetonitrile/water (75:25, v/v) followed by extraction on a C 18 cartridge and clean‐up on a cartridge containing graphitized carbon black. Method detection limits were in the range 2–14 ng/g, with the exception of nivalenol (27 ng/g), deoxynivalenol (40 ng/g) and 15‐acetyldeoxynivalenol (30 ng/g). Good accuracy (recoveries 81–104%) and precision (RSD 4–11%) were obtained by performing calibration using a spiked analyte‐free extract. Copyright © 2005 John Wiley & Sons, Ltd.