NHC Key Laboratory of Food Safety Risk Assessment, China National Center for Food Safety Risk Assessment, Beijing 100021, PR China.
NHC Key Laboratory of Food Safety Risk Assessment, China National Center for Food Safety Risk Assessment, Beijing 100021, PR China.
J Adv Res. 2022 Jul;39:15-47. doi: 10.1016/j.jare.2021.10.008. Epub 2021 Oct 19.
Mycotoxins are toxic metabolites produced by fungi that commonly contaminate foods. As recommended by the World Health Organization, total diet study (TDS) is the most efficient and effective way to estimate the dietary intakes of certain chemical substances for general populations. It requires sensitive and reliable analytical methods applicable to a wide range of complex food matrices and ready-to-eat dishes.
A novel strategy with high selectivity and sensitivity, incorporating three methods based on ultra-high-performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS), was designed for measuring 43 mycotoxins in dietary samples in a China TDS.
The 43 mycotoxins were divided into 3 groups for analysis to achieve better performance. For each group, an UHPLC-MS/MS method was developed to determine the target compounds after clean-up by solid phase extraction. A total of 21 isotope internal standards were employed for accurate quantitation. Method validation in terms of linearity, selectivity, sensitivity, accuracy, and precision was performed for all the 43 mycotoxins in 12 complex food matrices.
The limits of detection (LODs) and limits of quantitation (LOQs) were 0.002-1 ng mL and 0.006-3 ng mL, respectively. The method recoveries of the 43 mycotoxins spiked in 12 food categories were in the range of 60.3%-175.9% after internal standard correction, with relative standard deviations (RSDs) below 13.9%. For practical application, this method was utilized for 72 dietary samples collected from 6 provinces in the 6th China TDS. More than 80% of the samples were found contaminated by mycotoxins. DON, SMC, FB, ZEN, BEA, ENNB, and ENNB were most detected.
The proposed methods with high sensitivity, accuracy, and robustness provide powerful tools for multi-mycotoxin monitoring and dietary exposure assessment, allowing 43 mycotoxins, including some emerging mycotoxins, to be accurately investigated in a total diet study for the first time.
真菌产生的霉菌毒素是有毒的代谢物，通常会污染食物。世界卫生组织建议，总膳食研究（TDS）是估计一般人群某些化学物质膳食摄入量最有效和最有效的方法。它需要适用于广泛的复杂食物基质和即食菜肴的灵敏可靠的分析方法。
本研究设计了一种高选择性和高灵敏度的新策略，该策略结合了基于超高效液相色谱-串联质谱（UHPLC-MS/MS）的三种方法，用于测量中国 TDS 中膳食样品中的 43 种霉菌毒素。
将 43 种霉菌毒素分为 3 组进行分析，以获得更好的性能。对于每个组，开发了一种 UHPLC-MS/MS 方法，通过固相萃取净化后测定目标化合物。总共使用了 21 种同位素内标进行准确定量。对 12 种复杂食品基质中的 43 种霉菌毒素进行了线性、选择性、灵敏度、准确性和精密度的方法验证。
43 种霉菌毒素的检出限（LOD）和定量限（LOQ）分别为 0.002-1ng/mL 和 0.006-3ng/mL。经内标校正后，12 种食品类别中 43 种霉菌毒素的加标回收率在 60.3%-175.9%范围内，相对标准偏差（RSD）低于 13.9%。在实际应用中，该方法用于中国第六次 TDS 中从 6 个省份采集的 72 个膳食样本。超过 80%的样品被检测出受到霉菌毒素污染。DON、SMC、FB、ZEN、BEA、ENNB 和 ENNB 是最常被检测到的。
该方法灵敏度高、准确性高、稳健性好，为多霉菌毒素监测和膳食暴露评估提供了有力工具，首次能够准确研究总膳食研究中的 43 种霉菌毒素，包括一些新兴霉菌毒素。
