PMID- 27707355 OWN - NLM STAT- MEDLINE DCOM- 20170316 LR - 20191210 IS - 1944-0057 (Electronic) IS - 1944-0057 (Linking) VI - 33 IP - 12 DP - 2016 Dec TI - Validation and application of a liquid chromatography-tandem mass spectrometry based method for the assessment of the co-occurrence of mycotoxins in maize silages from dairy farms in NW Spain. PG - 1850-1863 AB - The first objective of this study was the validation of an efficient multi-analyte method for the simultaneous detection and quantification of mycotoxins in maize silage, by reverse-phase liquid chromatography coupled with electrospray ionisation triple quadrupole mass spectrometry (LC-HESI-MS/MS). A simple liquid/solid extraction was performed either with clean-up on Mycospin 400 columns or without any clean-up. Almost all the target mycotoxins showed highly-suppressed signals in the presence of a matrix, emphasising the need to quantitate mycotoxins by means of matrix-matched calibrations. An alternative validation method based on ISO 11843 and on a single factor balanced design was implemented. The achieved average recoveries from spiked samples at three levels ranged from 60% to 122% with relative standard deviations (rsd) below 11%. Limits of Detection (LODs) and Limits of Quantification (LOQs) were between 0.02-17.1 microg kg(-1) and 0.06-57 microg kg(-1). The calculated repeatability and within-lab reproducibility ranged from 5.2 to 23.2% and from 7.2 to 23.9%, respectively. Finally, the decision limit and detection capacity, CCalpha and CCbeta, were calculated for all mycotoxins having regulated/recommended contents in feed. The validated method was applied to 148 samples collected over two years in 19 dairy farms from Galicia (NW Spain). Of the analysed samples, 62% contained at least one mycotoxin. Zearalenone (ZEA), deoxynivalenol (DON), fumonisins B1 and B2, roquefortine C, alpha-zearalenol, beta-zearalenol, enniatins B and B1, andrastin A, marcfortine A, verruculogen and mycophenolic acid were quantified, the highest average detection frequency being for enniatin B (51%). DON, mycophenolic acid and ZEA plus metabolites (alpha-zearalenol, beta-zearalenol) were the most abundant mycotoxins. FAU - Dagnac, Thierry AU - Dagnac T AD - a Department of Animal Production , INGACAL (Galician Institute for Food Quality) -CIAM (Agrarian and Agronomic Research Centre), Laboratory of Food/Feed Safety and Organic Contaminants , A Coruna , Spain. FAU - Latorre, Alicia AU - Latorre A AD - a Department of Animal Production , INGACAL (Galician Institute for Food Quality) -CIAM (Agrarian and Agronomic Research Centre), Laboratory of Food/Feed Safety and Organic Contaminants , A Coruna , Spain. FAU - Fernandez Lorenzo, Bruno AU - Fernandez Lorenzo B AD - a Department of Animal Production , INGACAL (Galician Institute for Food Quality) -CIAM (Agrarian and Agronomic Research Centre), Laboratory of Food/Feed Safety and Organic Contaminants , A Coruna , Spain. FAU - Llompart, Maria AU - Llompart M AD - b Department of Analytical Chemistry, Nutrition and Food Science. Faculty of Chemistry , Campus Vida. University of Santiago de Compostela , Santiago de Compostela , Spain. LA - eng PT - Journal Article PT - Validation Study DEP - 20161026 PL - England TA - Food Addit Contam Part A Chem Anal Control Expo Risk Assess JT - Food additives & contaminants. Part A, Chemistry, analysis, control, exposure & risk assessment JID - 101485040 RN - 0 (Mycotoxins) SB - IM MH - Chromatography, Liquid MH - *Dairying MH - *Farms MH - Food Contamination/*analysis MH - Mycotoxins/*analysis MH - Silage/*analysis MH - Spain MH - Tandem Mass Spectrometry MH - Zea mays/*chemistry OTO - NOTNLM OT - Multi-mycotoxin method OT - clean-up free extraction OT - maize silage OT - mass spectrometry OT - monitoring OT - validation strategy EDAT- 2016/10/07 06:00 MHDA- 2017/03/17 06:00 CRDT- 2016/10/07 06:00 PHST- 2016/10/07 06:00 [pubmed] PHST- 2017/03/17 06:00 [medline] PHST- 2016/10/07 06:00 [entrez] AID - 10.1080/19440049.2016.1243806 [doi] PST - ppublish SO - Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2016 Dec;33(12):1850-1863. doi: 10.1080/19440049.2016.1243806. Epub 2016 Oct 26.