Bálint Analitika Ltd., Fehérvári út 144, 1116 Budapest, Hungary.
Program for the Environment and Sustainability, Department of Environmental and Occupational Health, School of Public Health, Texas A&M University, 212 Adriance Lab Rd., 1266 TAMU, College Station, TX 77843, USA.
Molecules. 2021 Feb 15;26(4):1017. doi: 10.3390/molecules26041017.
toxins are emerging mycotoxins whose regulation and standardization are in progress by the European Commission and the European Committee for Standardization. This paper describes a dilute and shoot approach to determine five toxins in selected food samples using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The strategy involves sample extraction with acidified aqueous methanol, followed by a solvent change accomplished via sample evaporation and reconstitution. The quantification is based on isotope dilution, applying all corresponding isotopically labeled internal standards to compensate possible matrix effects of the analysis. The main advantages of the present method over other existing methods includes simple and effective sample preparation, as well as detection with high sensitivity. The five-fold sample dilution can decrease matrix effects, which were evaluated with both external and internal standard methods. The results demonstrated a limit of quantification lower than 1.0 µg/kg for all five analytes for the first time. The newly presented method showed acceptable accuracy (52.7-111%) when analyzing naturally contaminated and spiked standard samples at the described levels. The method was validated for tomato-based and flour samples (wheat, rye, and maize). The absolute recovery ranged from 66.7% to 91.6% (RSD < 10%). The developed method could be an alternative approach for those laboratories that exclude sample cleanup and pre-concentration of state-of-the-art instruments with enhanced sensitivity.
毒素是新兴的真菌毒素,欧盟委员会和欧洲标准化委员会正在对其进行监管和标准化。本文描述了一种使用液相色谱-串联质谱(LC-MS/MS)测定选定食品样品中五种毒素的稀释进样方法。该策略涉及用酸化的甲醇水溶液提取样品,然后通过蒸发和再溶解来完成溶剂转换。定量基于同位素稀释,使用所有相应的同位素标记内标来补偿分析中的可能基质效应。与其他现有方法相比,本方法的主要优点包括简单有效的样品制备以及高灵敏度的检测。五次样品稀释可以降低基质效应,这可以通过外部和内部标准方法进行评估。结果首次表明,对于所有五种分析物,五次稀释后的检出限均低于 1.0µg/kg。当在描述的水平上分析自然污染和添加标准样品时,新提出的方法表现出可接受的准确性(52.7%-111%)。该方法已针对基于番茄和面粉的样品(小麦、黑麦和玉米)进行了验证。绝对回收率在 66.7%-91.6%之间(RSD<10%)。对于那些排除使用具有增强灵敏度的最先进仪器进行样品净化和预浓缩的实验室来说,该方法可能是一种替代方法。