Determination of Penicillium mycotoxins in foods and feeds using liquid chromatography–mass spectrometry

Abstract

New LC–MS (full scan) and LC–MS–MS (selected ion reaction monitoring) methods for the simultaneous determination of mycophenolic acid, griseofulvin, roquefortine C, chaetoglobosin B, verruculogen and penitrem A, and other Penicillium derived mycotoxins in food and feed samples are described. The methodologies involve sample extraction with acetonitrile–water, defatting with hexane and quantification using LC–MS with atmospheric pressure chemical ionisation or LC–MS–MS. Detector responses, for each of the methods and mycotoxins, were found to be linear over the range 10–1000 ng of mycotoxin/g of extracted food mixture material. The mean recoveries ( n=3 to 6) of the mycotoxins from spiked food mixture samples determined using MS and MS–MS detection were 87–116 and 91–112%, respectively, for mycophenolic acid, 104–109 and 91–112%, respectively, for griseofulvin, 70–85 and 75–110%, respectively, for roquefortine C, 94–109 and 81–116%, respectively, for chaetoglobosin B, 110–115 and 90–106%, respectively, for verruculogen and 78–97 and 99–108%, respectively, for penitrem A. RSDs varied from 5.6% at the 1000 ng/g level to 23.1% at the 10 ng/g level. The limits of detection for the mycotoxins using MS and MS–MS were 70 and 10 ng/g, respectively, for mycophenolic acid, 10 and 5 ng/g, respectively, for griseofulvin, 50 and 20 ng/g, respectively, for roquefortine C, 25 and 20 ng/g, respectively, for chaetoglobosin B, 25 and 20 ng/g, respectively, for verruculogen and 10 and 5 ng/g, respectively, for penitrem A.