Department of Microbiology and Ecology, Universitat de València, Dr. Moliner 50, E-46100 Burjassot, Valencia, Spain.
Department of Analytical Chemistry, Universitat de València, Dr. Moliner 50, E-46100 Burjassot, Valencia, Spain.
Food Chem. 2018 Nov 30;267:140-148. doi: 10.1016/j.foodchem.2017.11.040. Epub 2017 Nov 11.
In this report, a UPLC-ESI-MS/MS method for the simultaneous determination of aflatoxins, ochratoxin A, zearalenone, deoxynivalenol, fumonisins, T-2 and HT-2 toxins, fusarenone X, diacetoxyscirpenol, and 3- and 15-acetyldeoxynivalenol in feedstuffs was developed. A quadrupole-time-of-flight mass spectrometer detector (QTOF-MS) operating in full scan mode was combined with the UPLC-ESI-MS/MS system to confirm the identity of detected mycotoxins and to identify other possible microbial metabolites occurring in samples. Sixty-two feed samples from the Spanish market were analyzed. Extraction of metabolites was carried out with acetonitrile-water-formic acid (80:19:1, v/v/v). Method detection and quantification limits and performance criteria set by Commission Regulation (EC) No 401/2006 were fulfilled. Relatively high levels of the main regulated mycotoxins and presence of non-regulated mycotoxins in feed samples were found. This is the first study in which mycotoxins and other microbial metabolites occurring in feed are studied using a UPLC-QTOF-MS system being therefore a reference report.
本报告建立了一种超高效液相色谱-电喷雾串联质谱法（UPLC-ESI-MS/MS），用于同时测定饲料中的黄曲霉毒素、赭曲霉毒素 A、玉米赤霉烯酮、脱氧雪腐镰刀菌烯醇、伏马菌素、T-2 和 HT-2 毒素、玉米赤霉烯酮 X、二乙酰基交链孢酚和 3- 和 15-乙酰基脱氧雪腐镰刀菌烯醇。四极杆飞行时间质谱（QTOF-MS）检测器与 UPLC-ESI-MS/MS 系统相结合，用于确证所检测霉菌毒素的身份，并鉴定样品中可能存在的其他微生物代谢产物。分析了来自西班牙市场的 62 个饲料样本。采用乙腈-水-甲酸（80:19:1，v/v/v）提取代谢物。方法检测限和定量限以及委员会法规（EC）No 401/2006 设定的性能标准均得到满足。在饲料样品中发现了主要受监管霉菌毒素的相对高含量以及非受监管霉菌毒素的存在。这是首次使用 UPLC-QTOF-MS 系统研究饲料中存在的霉菌毒素和其他微生物代谢产物的研究，因此是一份参考报告。
