A fundamental step in addressing the global problem of mycotoxins is the development of highly sensitive, multi-class extraction and detection methods. This constitutes a field of research that has in recent years enjoyed a steady advance. Such methods, generally based on liquid chromatography coupled to mass spectrometry, are widely reported successfully detecting various mycotoxins in different food and feed samples. In this work, an innovative approach to multi-class mycotoxin control is proposed, offering specific advantages: a broader inclusion of more mycotoxin classes, robust and thorough extraction for all target compounds despite their varied chemical properties, and determination of all analytes from a single injection. The method involved the extraction and quantification of the main mycotoxins produced by Aspergillus, Fusarium, and Penicillium fungi, as well as their reported derivatives, together with 12 other compounds most commonly produced by Claviceps purpurea. The popularly reported QuEChERS technique has been reduced to a simple “salting-out liquid-liquid extraction” (SO-LLE) to obtain the most efficient extraction of the aforementioned mycotoxin classes in a very short time. This is in particular extremely important in ensuring correct determination of individual ergot alkaloids, for which short and robust sample preparation as well as short analytical sequences were key for minimizing the epimerization during analysis. The analyses of wheat and maize samples were performed using ultra-high performance liquid chromatography coupled with tandem mass spectrometry. Matrix-matched calibration curves were established and limits of quantification were below the maximum levels established by the EU regulation. The precision (repeatability and intermediate precision) was lower than 13% in all cases and recoveries ranged between 60 and 98% in maize and between 62 and 103% in wheat, fulfilling the current legislation. The method was applied to study the co-occurrence of these mycotoxins in wheat (n = 13) and maize (n = 15) samples from six European countries. A successful quantification of 23 different mycotoxins, from all major classes, in 85% of wheat and 93% of maize samples was achieved.

解决真菌毒素这一全球性问题的基本步骤是开发高度敏感的多类提取和检测方法。这构成了近年来稳步发展的研究领域。通常基于液相色谱与质谱联用的这种方法被广泛报道，可以成功地检测出不同食品和饲料样品中的各种霉菌毒素。在这项工作中，提出了一种控制多类霉菌毒素的创新方法，该方法具有以下特殊优点：包括更多种类的霉菌毒素，尽管目标化合物的化学性质各不相同，但仍能对所有目标化合物进行稳健而彻底的提取，并能从单一样品中测定所有分析物注射。该方法涉及提取和定量由曲霉，镰刀菌和青霉菌真菌，及其报道的衍生物，以及最常见的是紫癜的12种其他化合物。流行报道的QuEChERS技术已简化为简单的“盐析液液提取”（SO-LLE），可以在很短的时间内最有效地提取上述真菌毒素。这对于确保正确确定各个麦角生物碱尤为重要，为此，短而稳健的样品制备以及较短的分析序列是最小化分析过程中差向异构化的关键。小麦和玉米样品的分析采用超高效液相色谱-串联质谱联用。建立了与基质匹配的校准曲线，定量限低于欧盟法规确定的最大水平。在所有情况下，精度（可重复性和中等精度）均低于13％，玉米的回收率介于60％至98％之间，小麦的回收率介于62％至103％之间，符合现行法规。该方法用于研究小麦中这些霉菌毒素的共存（n  = 13）和 来自六个欧洲国家的玉米（n = 15）样本。在85％的小麦和93％的玉米样品中成功地定量了所有主要类别的23种不同霉菌毒素。