School of Food and Environment, Dalian University of Technology, Panjin 124221, China.
School of Sports and Health, Dalian University of Technology, Panjin 124221, China.
J Chromatogr A. 2020 Feb 22;1613:460712. doi: 10.1016/j.chroma.2019.460712. Epub 2019 Nov 15.
A simple magnetization method was developed for the preparation of magnetic materials from conventional solid phase packing though coprecipitation and solvothermal approaches. And the prepared magnetic materials were used for magnetic solid phase extraction (MSPE) of biogenic amines (BAs) from beers. Furthermore, to improve the analytical throughput, a solid phase "on-situ" quadraplex isotope dimethyl labeling method was developed for the quantification of BAs by liquid chromatography-high resolution mass spectrometry (LCHRMS). Compared to conventional in-solution labeling, the "on-situ" labeling could simplify the sample preparation procedure and efficiently remove the residuals such as inorganic salts and excessive labeling reagents. The quadraplex labeling, which enabled three real samples and one internal standard sample to be analyzed simultaneously in a single LCHRMS run. For the tested 8 BAs (cadaverine, phenethylamine, spermine, spermidine, tyramine, histamine, putrescine and tryptamine), LODs of 0.02-0.05 μg/L and LOQs of 0.05-0.1 μg/L were achieved at good reproducibility (RSD of 0.5-4.6% and 2.2-7.0% for intra- and inter-day reproducibility, respectively). With this method, six beer samples were analyzed, and these 8 BAs were all detected in the range of low μg/L to 2.9 mg/L, which were lower than maximal residual level (MRL) required in the regulations of China and EU.
开发了一种简单的磁化方法，通过共沉淀和溶剂热方法，从常规固相包装制备磁性材料。并将制备的磁性材料用于从啤酒中磁固相萃取（MSPE）生物胺（BAs）。此外，为了提高分析通量，开发了一种固相“原位”四重同位素二甲标记方法，通过液相色谱-高分辨质谱（LCHRMS）对 BAs 进行定量。与传统的溶液标记相比，“原位”标记可以简化样品制备程序，并有效地去除无机盐和过量标记试剂等残留物质。四重标记可以同时分析三个实际样品和一个内标样品，在单个 LCHRMS 运行中。对于测试的 8 种 BAs（尸胺、苯乙胺、亚精胺、精胺、酪胺、组胺、腐胺和色胺），在良好的重现性下（日内和日间重现性的 RSD 分别为 0.5-4.6%和 2.2-7.0%），LOD 为 0.02-0.05μg/L，LOQ 为 0.05-0.1μg/L。采用该方法分析了 6 个啤酒样品，这些 BAs 的检测范围为低μg/L 至 2.9mg/L，均低于中国和欧盟法规规定的最大残留限量（MRL）。
