Background Natural contamination with mycotoxins in dried distiller’s grains with solubles (DDGS) as a mainstream animal feed ingredient poses a risk to animal health. Objective A regulatory method was needed for the agency to simultaneously detect 11 mycotoxins of high regulatory priority in DDGS. Methods A DDGS sample (10 g) was extracted twice with acetonitrile-water under mildly acidic condition. Two aliquots from the combined crude extract were taken and processed separately: (1) diluted 400-fold with solvent for analysis of deoxynivalenol and fumonisins B1 and B2; and (2) with the pH adjusted to 7.5, and then diluted 15.7-fold for analysis of aflatoxins B1, B2, G1, and G2, ochratoxin A, zearalenone, and T-2 and HT-2 toxins. Uniformly labeled 13C-isotopologues of these mycotoxins were added as internal standards to the diluted extracts for quantitative analysis by ultra-high-performance LC–tandem MS. Results The linear quantitation ranges (µg/kg) were: aflatoxins B1, B2, G1, and G2, 1.57–105; zearalenone, 16.3–1090; T-2 toxin, 3.14–208; HT-2 toxin, 48.2–3220; ochratoxin A, 0.47–31.4; deoxynivalenol, 240–16 000; fumonisin B1 and B2, 320–21 200. Accuracies for these analytes at each of three fortification levels ranged from 70.7 to 100%, with corresponding RSDs between 1.4 and 10.5%. True recoveries were all higher than 83%. Conclusion This method was successfully validated to meet the agency’s performance guidelines for regulatory methods. Highlights This method is easy, quick, and robust to simultaneously quantify and confirm the presence of 11 regulated mycotoxins in DDGS.

中文翻译：

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一种同时测定和确证干燥酒糟中可溶物的 11 种真菌毒素的稀释和喷射 UHPLC-MS/MS 同位素稀释方法

背景 作为主流动物饲料成分的干酒糟和可溶物 (DDGS) 中真菌毒素的天然污染会对动物健康构成风险。目的 该机构需要一种监管方法来同时检测 DDGS 中监管优先的 11 种真菌毒素。方法 10 g DDGS 样品在弱酸性条件下用乙腈-水萃取两次。从合并的粗提物中取出两份并分别处理： (1) 用溶剂稀释 400 倍，用于分析脱氧雪腐镰刀菌烯醇和伏马菌素 B1 和 B2；(2) 将 pH 调至 7.5，稀释 15.7 倍用于黄曲霉毒素 B1、B2、G1 和 G2、赭曲霉毒素 A、玉米赤霉烯酮和 T-2 和 HT-2 毒素的分析。将这些霉菌毒素的统一标记的 13C 同位素体作为内标添加到稀释的提取物中，以通过超高性能 LC-串联 MS 进行定量分析。结果 线性定量范围 (µg/kg) 为：黄曲霉毒素 B1、B2、G1 和 G2，1.57–105；玉米赤霉烯酮, 16.3–1090; T-2 毒素，3.14–208；HT-2 毒素，48.2–3220；赭曲霉毒素 A，0.47–31.4；脱氧雪腐镰刀菌烯醇，240–16 000；伏马菌素 B1 和 B2，320–21 200。这些分析物在三个加标浓度水平的准确度范围为 70.7% 到 100%，相应的 RSD 介于 1.4% 和 10.5% 之间。真实回收率均高于 83%。结论 该方法已成功验证，符合该机构的监管方法性能指南。亮点此方法简单、快捷、