Izcara Sergio, Casado Natalia, Morante-Zarcero Sonia, Sierra Isabel
Departamento de Tecnología Química y Ambiental, E.S.C.E.T, Universidad Rey Juan Carlos, C/Tulipán s/n, Móstoles, 28933 Madrid, Spain.
Foods. 2020 Sep 18;9(9):1319. doi: 10.3390/foods9091319.
Recent and unexpected food alerts about relatively high amounts of pyrrolizidine alkaloids in oregano samples have stressed the need to develop analytical strategies to ensure food safety in this type of foodstuff. Accordingly, this work presents the development of a miniaturized strategy based on the QuEChERS (quick, easy, cheap, effective, rugged and safe) method combined with ultrahigh liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) for the determination of 21 pyrrolizidine alkaloids suggested by the European Food Safety Authority to be monitored in food. The analytical method was properly validated, with overall average recoveries from 77 to 96% and relative standard deviations <13% ( = 9). The method proved to be a sustainable analytical strategy which meets green analytical chemistry principles as it showed good performance by using small amounts of sample (0.2 g), organic solvents (1000 µL), clean-up sorbents (175 mg) and partitioning salts (0.65 g). Its feasibility was verified through the analysis of 23 oregano samples. Of the samples analyzed, 100% were contaminated, with an average concentration of 1254 µg/kg. Lasiocarpine, lasiocarpine N-oxide, europine, europine N-oxide, senecivernine, senecionine, echimidine N-oxide, lycopsamine N-oxide and intermedine N-oxide were the alkaloids which significantly contributed to the contamination of the samples.
最近，牛至样本中吡咯里西啶生物碱含量相对较高这一出人意料的食品警报，凸显了制定分析策略以确保此类食品的食品安全的必要性。因此，本研究提出了一种基于QuEChERS（快速、简便、廉价、高效、耐用且安全）方法的小型化策略，该方法结合了超高效液相色谱-串联质谱联用技术（UHPLC-MS/MS），用于测定欧洲食品安全局建议在食品中监测的21种吡咯里西啶生物碱。该分析方法经过了适当验证，总体平均回收率为77%至96%，相对标准偏差<13%（ = 9）。该方法被证明是一种符合绿色分析化学原则的可持续分析策略，因为它通过使用少量样品（0.2 g）、有机溶剂（1000 µL）、净化吸附剂（175 mg）和分配盐（0.65 g）就表现出了良好的性能。通过对23个牛至样品的分析验证了其可行性。在分析的样品中，100%受到污染，平均浓度为1254 µg/kg。拉斯可匹宁、拉斯可匹宁氮氧化物、欧洲千里光碱、欧洲千里光碱氮氧化物、异西维宁、千里光碱、刺苞碱氮氧化物、石蒜碱氮氧化物和中节千里光碱氮氧化物是对样品污染有显著贡献的生物碱。
