A rugged high-throughput analytical approach for the determination and quantification of multiple mycotoxins in complex feed
A rugged high-throughput analytical approach for the determination and quantification of multiple mycotoxins in complex feed
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DOI：
10.1016/j.talanta.2013.12.064
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发表时间：
2014-04-01
期刊：
影响因子：
6.1
通讯作者：
Hajslova, Jana
中科院分区：
文献类型：
--
作者：
Dzuman, Zbynek;Zachariasova, Milena;Hajslova, Jana
我们开发并优化了高通量方法，可可靠地检测和定量各种动物饲料样品中的 56 种镰孢菌、链格孢菌、青霉菌、曲霉和麦角菌毒素，这些样品包括谷物、复合饲料、提取油饼、发酵青贮饲料、麦芽芽或干酒糟（DDGS）。从三种测试的萃取方法（乙腈、乙腈/水和 QuEChERS）中，基于 QuEChERS 的方法（快速、简单、便宜、有效、坚固和安全）被选为分析物回收率和低基质效应方面最好的方法。为了分离和检测目标霉菌毒素，采用了基于超高效液相色谱与灵敏串联质谱（U-HPLC-MS/MS）的方法。鉴于大多数研究的饲料样品的高度复杂性，需要在第一阶段优化提取/纯化过程，以保持方法尽可能坚固。特别关注提取溶剂的 pH 值，尤其是 pH 值敏感的青贮饲料。此外，还评估了通过分散固相净化对乙腈提取物的纯化。使用 C-18 二氧化硅吸附剂时，观察到脂质化合物的显着消除。通过超高效液相色谱结合超高分辨率质谱 (U-HPLC-HRMS) 对基质共提取物进行了表征。基质效应的巨大变化取决于所检查饲料的性质，这在广泛的样品中得到了深入的证明。建议采取简单且公正的补偿策略。 (C) 2014 Elsevier B.V. 保留所有权利。
We have developed and optimized high throughput method for reliable detection and quantification of 56 Fusarium, Alternaria, Penicillium, Aspergillus and Claviceps mycotoxins in a wide range of animal feed samples represented by cereals, complex compound feeds, extracted oilcakes, fermented silages, malt sprouts or dried distillers' grains with solubles (DDGS). From three tested extraction approaches (acetonitrile, acetonitrile/water, and QuEChERS), the QuEChERS-based method (Quick, Easy, Cheap, Effective, Rugged and Safe) was selected as the best in terms of analytes recoveries and low matrix effects. For separation and detection of target mycotoxins, method based on ultra-high performance liquid chromatography coupled with sensitive tandem mass spectrometry (U-HPLC-MS/MS) was employed. With regards to a high complexity of most of investigated feed samples, optimization of extraction/purification process was needed in the first phase to keep the method as rugged as possible. A special attention was paid to the pH of extraction solvents, especially with regard to the pH-sensitive silages. Additionally, purification of the acetonitrile extract by dispersive solid phase clean-up was assessed. Significant elimination of lipidic compounds was observed when using C-18 silica sorbent Matrix co-extracts were characterized by ultra-high performance liquid chromatography coupled with ultra-high resolution mass spectrometry (U-HPLC-HRMS). Large variability of matrix effects depending on the nature of examined feed was demonstrated in depth on a broad set of samples. Simple and unbiased strategies for their compensation were suggested. (C) 2014 Elsevier B.V. All rights reserved.