中文摘要：本研究首要目的在于，通过反相液相色谱-电喷雾三重四极杆质谱联用(LC-HESI-MS/MS)，验证一种有效的、同时检测并量化玉米青贮中霉菌毒素多种组分的方法。用简单的液/固相萃取法提取样品，不净化或经Mycospin 400净化柱净化。几乎所有的目标毒素在其基质中都显示高度抑制信号，非常需要通过基质匹配校准法定量测定霉菌毒素。运用了另一种基于ISO 11843和单因素平衡设计验证该方法。用验证后的方法分析了两年多从加利西亚（西班牙西北部）19个乳牛场采集的148个样品，发现其中62%至少受到一种霉菌霉素污染；定量测定玉米赤霉烯酮（ZEN）、脱氧雪腐镰刀菌烯醇（DON）、伏马菌素B1和B2、异烟棒曲霉素C、α-玉米赤霉烯醇、β-玉米赤霉烯醇、恩镰孢菌素B1和B2、andrastin A、麦可弗汀A、震颤毒素及霉酚酸，发现恩链孢霉素B具有最高平均检测频率（51%）；DON、霉酚酸和ZEA及其代谢物（α-玉米赤霉烯醇、β-玉米赤霉烯醇）是最多的霉菌毒素。
外文摘要：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 to electrospray ionization 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 presence of matrix, emphasizing 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 µg kg-1 and 0.06-57 µg 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, CCα and CCβ, 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, α-zearalenol, β-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 (α-zearalenol, β-zearalenol) were the most abundant mycotoxins.
外文关键词：Multi-mycotoxin method；clean-up free extraction；validation strategy；monitoring；maize silage；mass spectrometry
作者：Dagnac, T；Latorre, A；Lorenzo, BF；Llompart, M
作者单位：CIAM Agr & Agron Res Ctr
期刊名称：Food Additives and Contaminants Part A-Chemistry Analysis Control Exposure & Risk Assessment
期刊影响因子：1.878
出版年份：2016
出版刊次：12
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