PMID- 22293971 OWN - NLM STAT- MEDLINE DCOM- 20120611 LR - 20220316 IS - 1618-2650 (Electronic) IS - 1618-2642 (Print) IS - 1618-2642 (Linking) VI - 402 IP - 9 DP - 2012 Mar TI - Stable isotope dilution assay for the accurate determination of mycotoxins in maize by UHPLC-MS/MS. PG - 2675-86 LID - 10.1007/s00216-012-5757-5 [doi] AB - A fast, easy-to-handle and cost-effective analytical method for 11 mycotoxins currently regulated in maize and other cereal-based food products in Europe was developed and validated for maize. The method is based on two extraction steps using different acidified acetonitrile-water mixtures. Separation is achieved using ultrahigh-performance liquid chromatography (UHPLC) by a linear water-methanol gradient. After electrospray ionisation, tandem mass spectrometric detection is performed in dynamic multiple reaction monitoring mode. Since accurate mass spectrometric quantification is hampered by matrix effects, uniformly [(13)C]-labelled mycotoxins for each of the 11 compounds were added to the sample extracts prior to UHPLC-MS/MS analysis. Method performance parameters were obtained by spiking blank maize samples with mycotoxins before as well as after extraction on six levels in triplicates. The twofold extraction led to total recoveries of the extraction steps between 97% and 111% for all target analytes, including fumonisins. The [(13)C]-labelled internal standards efficiently compensated all matrix effects in electrospray ionisation, leading to apparent recoveries between 88% and 105% with reasonable additional costs. The relative standard deviations of the whole method were between 4% and 11% for all analytes. The trueness of the method was verified by the measurement of several maize test materials with well-characterized concentrations. In conclusion, the developed method is capable of determining all regulated mycotoxins in maize and presuming similar matrix effects and extraction recovery also in other cereal-based foods. FAU - Varga, Elisabeth AU - Varga E AD - Christian Doppler Laboratory for Mycotoxin Metabolism, Department for Agrobiotechnology, University of Natural Resources and Life Sciences Vienna, Tulln, Austria. FAU - Glauner, Thomas AU - Glauner T FAU - Koppen, Robert AU - Koppen R FAU - Mayer, Katharina AU - Mayer K FAU - Sulyok, Michael AU - Sulyok M FAU - Schuhmacher, Rainer AU - Schuhmacher R FAU - Krska, Rudolf AU - Krska R FAU - Berthiller, Franz AU - Berthiller F LA - eng PT - Evaluation Study PT - Journal Article PT - Research Support, Non-U.S. Gov't PL - Germany TA - Anal Bioanal Chem JT - Analytical and bioanalytical chemistry JID - 101134327 RN - 0 (Carbon Isotopes) RN - 0 (Mycotoxins) SB - IM MH - Carbon Isotopes/*analysis MH - Chromatography, High Pressure Liquid/*methods MH - Food Contamination/*analysis MH - *Indicator Dilution Techniques MH - Mycotoxins/*analysis MH - Spectrometry, Mass, Electrospray Ionization/*methods MH - Tandem Mass Spectrometry/methods MH - Zea mays/*chemistry PMC - PMC3292730 EDAT- 2012/02/02 06:00 MHDA- 2012/06/12 06:00 PMCR- 2012/02/02 CRDT- 2012/02/02 06:00 PHST- 2011/12/09 00:00 [received] PHST- 2012/01/16 00:00 [accepted] PHST- 2012/01/13 00:00 [revised] PHST- 2012/02/02 06:00 [entrez] PHST- 2012/02/02 06:00 [pubmed] PHST- 2012/06/12 06:00 [medline] PHST- 2012/02/02 00:00 [pmc-release] AID - 5757 [pii] AID - 10.1007/s00216-012-5757-5 [doi] PST - ppublish SO - Anal Bioanal Chem. 2012 Mar;402(9):2675-86. doi: 10.1007/s00216-012-5757-5.