Sattler Melinda, Müller Volker, Bunzel Diana, Kulling Sabine E, Soukup Sebastian T
Department of Safety and Quality of Fruit and Vegetables, Max Rubner-Institut, Federal Research Institute of Nutrition and Food, Haid-und-Neu-Straße 9, 76131, Karlsruhe, Germany.
Department of Safety and Quality of Fruit and Vegetables, Max Rubner-Institut, Federal Research Institute of Nutrition and Food, Haid-und-Neu-Straße 9, 76131, Karlsruhe, Germany.
Talanta. 2023 Jun 1;258:124425. doi: 10.1016/j.talanta.2023.124425. Epub 2023 Mar 7.
Pyrrolizidine alkaloids (PA) from borage (Borago officinalis) consumed as herb and tea, may pose a food safety risk. Therefore, the European Union (EU) set maximum levels of PA in borage, among other foodstuffs, which are applicable since July 1, 2022. Here, a comprehensive LC-MS/MS based profiling of PA and their N-oxides (PANO) in B. officinalis leaves is presented. Based on these results a targeted, quantitative LC-MS/MS method for the determination of individual PA/PANO present in borage was developed. Chromatographic separation was achieved for all PA/PANO detected in B. officinalis. An easy and fast extraction procedure was developed using a design of experiments approach (DOE). The most efficient extraction was achieved using 0.2% formic acid in 10% methanol at a temperature of 47.5 °C for 60 min. The final method was validated and showed good overall accuracy (recoveries 85-121%) and precision (RDS ≤11%). The method was applied to B. officinalis leave material, demonstrating its suitability for the intended purpose. In these borage samples, the acetylated forms, which are not regulated by EU, were among the quantitatively most relevant PA.
作为草药和茶饮用的琉璃苣（Borago officinalis）中的吡咯里西啶生物碱（PA）可能会带来食品安全风险。因此，欧盟（EU）设定了琉璃苣以及其他食品中PA的最大限量，自2022年7月1日起适用。本文介绍了一种基于液相色谱-串联质谱（LC-MS/MS）的琉璃苣叶片中PA及其N-氧化物（PANO）的全面分析方法。基于这些结果，开发了一种靶向定量LC-MS/MS方法，用于测定琉璃苣中存在的单个PA/PANO。实现了对琉璃苣中检测到的所有PA/PANO的色谱分离。采用实验设计方法（DOE）开发了一种简单快速的提取程序。在47.5℃下，使用含0.2%甲酸的10%甲醇提取60分钟，提取效率最高。最终方法经过验证，显示出良好的总体准确度（回收率85-121%）和精密度（相对标准偏差≤11%）。该方法应用于琉璃苣叶片材料，证明了其适用于预期目的。在这些琉璃苣样品中，不受欧盟监管的乙酰化形式是定量上最相关的PA之一。
