Chair of Analytical Food Chemistry, Technical University of Munich, Maximus-Von-Imhof Forum 2, 85354, Freising, Germany.
Anal Bioanal Chem. 2024 Nov;416(26):5619-5637. doi: 10.1007/s00216-024-05486-4. Epub 2024 Sep 2.
A QuEChERS (quick, easy, cheap, effective, rugged, and safe)-based multi-mycotoxin method was developed, analyzing 24 (17 free and 7 modified) Alternaria and Fusarium toxins in cereals via ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). A modified QuEChERS approach was optimized for sample preparation. Quantification was conducted using a combination of stable isotope dilution analysis (SIDA) for nine toxins and matrix-matched calibration for ten toxins. Quantification via a structurally similar internal standard was conducted for four analytes. Alternariol-9-sulfate (AOH-9-S) was measured qualitatively. Limits of detection (LODs) were between 0.004 µg/kg for enniatin A1 (ENN A1) and 3.16 µg/kg for nivalenol (NIV), while the limits of quantification were between 0.013 and 11.8 µg/kg, respectively. The method was successfully applied to analyze 136 cereals and cereal-based foods, including 28 cereal-based infant food products. The analyzed samples were frequently contaminated with Alternaria toxins, proving their ubiquitous occurrence. Interestingly, in many of those samples, some modified Alternaria toxins occurred, mainly alternariol-3-sulfate (AOH-3-S) and alternariol monomethyl ether-3-sulfate (AME-3-S), thus highlighting the importance of including modified mycotoxins in the routine analysis as they may significantly add to the total exposure of their parent toxins. Over 95% of the analyzed samples were contaminated with at least one toxin. Despite the general contamination, no maximum or indicative levels were exceeded.
建立了一种基于 QuEChERS(快速、简单、廉价、有效、耐用和安全)的多真菌毒素方法,通过超高效液相色谱-串联质谱法(UHPLC-MS/MS)分析谷物中的 24 种(17 种游离和 7 种修饰)链格孢菌和镰刀菌毒素。对样品制备进行了优化,采用稳定同位素稀释分析(SIDA)对 9 种毒素和基质匹配校准对 10 种毒素进行定量。对 4 种分析物采用结构类似的内标进行定量。定性测定了 Alternariol-9-sulfate (AOH-9-S)。检测限(LOD)在 0.004μg/kg 之间,Enniatin A1 (ENN A1) 的检测限为 0.004μg/kg,Nivalenol (NIV) 的检测限为 3.16μg/kg,定量限分别在 0.013μg/kg 和 11.8μg/kg 之间。该方法成功应用于分析 136 种谷物及其衍生食品,包括 28 种谷物衍生婴儿食品。分析样品经常受到链格孢菌毒素的污染,证明其广泛存在。有趣的是,在许多这些样品中,出现了一些修饰的链格孢菌毒素,主要是 alternariol-3-sulfate (AOH-3-S) 和 alternariol monomethyl ether-3-sulfate (AME-3-S),因此强调了在常规分析中纳入修饰真菌毒素的重要性,因为它们可能会显著增加其母体毒素的总暴露量。超过 95%的分析样品至少受到一种毒素的污染。尽管存在普遍污染,但没有超过最高或指示性水平。