Experiment Research Institute, National Agricultural Products Quality Management Service, 141, Yongjeon-ro, Gimcheon-si 39660, Korea.
Hansalim Agro-Food Analysis Center, Hankyong National University Industry Academic Cooperation Foundation, Suwon 16500, Korea.
Toxins (Basel). 2021 Oct 29;13(11):767. doi: 10.3390/toxins13110767.
Mycotoxins are toxic substances naturally produced by various fungi, and these compounds not only inflict economic damage, but also pose risks to human and animal health. The goal of the present study was to optimize the QuEChERS-based extraction and liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the analysis of 11 mycotoxins, such as aflatoxins (AFs), ochratoxin A (OTA), fumonisins (FBs), T-2 toxin, HT-2 toxin, zearalenone (ZEN), and deoxynivalenol (DON), commonly found in feed. The QuEChERS method, characterized by being "quick, easy, cheap, effective, rugged, and safe", has become one of the most common extractions and clean-up procedures for mycotoxin analyses in food. Therefore, in this experiment, an optimal method for the analysis of 11 mycotoxins in feed was established by modifying the general QuEChERS method. In this process, it was confirmed that even if feed samples of different weights were extracted, the quantitative value of mycotoxins in the feed was not affected. To reduce matrix effects, 13C-labeled compounds and deuterium were used as internal standards. This optimized method was then applied in the determination of 11 mycotoxins in 736 feed ingredients and compound feeds obtained from South Korea. The results showed that the occurrence rates of FBs, ZEN, and DON were 59.4%, 38.0%, and 32.1%, respectively, and OTA, AFs, and T-2 toxin and HT-2 toxin were found in fewer than 1% of the 736 feeds. The mean concentration ranges of FBs, ZEN, and DON were 757-2387, 44-4552, and 248-9680 μg/kg, respectively. Among the samples in which DON and ZEN were detected, 10 and 12 samples exceeded the management recommendation standards presented by the Ministry of Agriculture, Food and Rural Affairs (MAFRA). However, when the detected concentrations of DON and ZEN were compared with guideline levels in foreign countries, such as the US, Japan, China, and the EU, the number of positive samples changed. In addition, the co-occurrence of mycotoxins in the feed was analyzed, and the results showed that 43.8% of the samples were contaminated with two or three mycotoxins, among which the co-occurrence rate of FBs, ZEN, and DON was the highest. In conclusion, these results suggest the need for stricter management standards for FBs, DON, and ZEN in South Korea, and emphasize the importance of the continuous monitoring of feeds.
真菌自然产生的有毒物质称为真菌毒素，这些化合物不仅造成经济损失，还会对人类和动物健康构成威胁。本研究的目的是优化基于 QuEChERS 的提取和液相色谱-串联质谱（LC-MS/MS）方法，用于分析饲料中常见的 11 种真菌毒素，如黄曲霉毒素（AFs）、赭曲霉毒素 A（OTA）、伏马菌素（FBs）、T-2 毒素、HT-2 毒素、玉米赤霉烯酮（ZEN）和脱氧雪腐镰刀菌烯醇（DON）。QuEChERS 方法具有“快速、简便、廉价、有效、耐用和安全”的特点，已成为食品中真菌毒素分析最常用的提取和净化程序之一。因此，在本实验中，通过修改通用 QuEChERS 方法，建立了一种分析饲料中 11 种真菌毒素的最佳方法。在这个过程中，即使提取不同重量的饲料样品，饲料中真菌毒素的定量值也不受影响。为了减少基质效应，使用 13C 标记化合物和氘作为内标。然后将优化后的方法应用于韩国获得的 736 种饲料成分和配合饲料中 11 种真菌毒素的测定。结果表明，FBs、ZEN 和 DON 的发生率分别为 59.4%、38.0%和 32.1%，而 736 种饲料中少于 1%的饲料中发现了 OTA、AFs 和 T-2 毒素和 HT-2 毒素。FBs、ZEN 和 DON 的平均浓度范围分别为 757-2387μg/kg、44-4552μg/kg和 248-9680μg/kg。在检测到 DON 和 ZEN 的样品中，有 10 个和 12 个样品超过了农业、食品和农村事务部（MAFRA）提出的管理建议标准。然而，当将 DON 和 ZEN 的检测浓度与美国、日本、中国和欧盟等国外的指导水平进行比较时，阳性样品的数量发生了变化。此外，还分析了饲料中真菌毒素的共同存在情况，结果表明，43.8%的样品受到两种或三种真菌毒素的污染，其中 FBs、ZEN 和 DON 的共同存在率最高。总之，这些结果表明，韩国需要对 FBs、DON 和 ZEN 实施更严格的管理标准，并强调需要持续监测饲料。
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