利用 UHPLC-Q-Orbitrap HRMS 对宠物食品中的多种真菌毒素进行目标分析和回顾性筛选。
Target Analysis and Retrospective Screening of Multiple Mycotoxins in Pet Food Using UHPLC-Q-Orbitrap HRMS.
机构信息
Department of Pharmacy, Faculty of Pharmacy, University of Naples "Federico II", Via Domenico Montesano 49, 80131 Naples, Italy.
Department of Clinical Medicine and Surgery, University of Naples "Federico II", Via S. Pansini 5, 80131 Naples, Italy.
出版信息
Toxins (Basel). 2019 Jul 24;11(8):434. doi: 10.3390/toxins11080434.
A comprehensive strategy combining a quantitative method for 28 mycotoxins and a post-target screening for other 245 fungal and bacterial metabolites in dry pet food samples were developed using an acetonitrile-based extraction and an ultrahigh-performance liquid chromatography coupled to high-resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) method. The proposed method showed satisfactory validation results according to Commission Decision 2002/657/EC. Average recoveries from 72 to 108% were obtained for all studied mycotoxins, and the intra-/inter-day precision were below 9 and 14%, respectively. Results showed mycotoxin contamination in 99% of pet food samples ( = 89) at concentrations of up to hundreds µg/kg, with emerging mycotoxins being the most commonly detected mycotoxins. All positive samples showed co-occurrence of mycotoxins with the simultaneous presence of up to 16 analytes per sample. In the retrospective screening, up to 54 fungal metabolites were tentatively identified being cyclopiazonic acid, paspalitrem A, fusaric acid, and macrosporin, the most commonly detected analytes.
建立了一种综合策略，结合了一种用于 28 种霉菌毒素的定量方法和一种针对其他 245 种真菌和细菌代谢物的后靶向筛选方法，用于干燥宠物食品样品。该方法采用基于乙腈的提取和超高效液相色谱-高分辨率质谱联用（UHPLC-Q-Orbitrap HRMS）方法。根据委员会决定 2002/657/EC，该方法的验证结果令人满意。所有研究的霉菌毒素的平均回收率为 72%至 108%，日内和日间精密度分别低于 9%和 14%。结果表明，在 99%的宠物食品样品（=89）中检测到霉菌毒素污染，浓度高达数百 µg/kg，新兴霉菌毒素是最常见的检测到的霉菌毒素。所有阳性样品均显示出霉菌毒素的共同存在，每个样品中同时存在多达 16 种分析物。在回顾性筛选中，共暂定鉴定出 54 种真菌代谢物，分别为环匹阿尼酸、帕斯帕尔曲霉素 A、伏马酸和大孢子素，是最常见的检测到的分析物。
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