Li Peipei, Chen Yu, Bai Junlu, Yang Huicheng, He Pengfei, Zeng Junjie
Zhejiang Marine Fisheries Research Institute, Tiyu Road 28, Zhoushan 316021, China.
College of Food and Pharmacy, Zhejiang Ocean University, 1 South Haida Road, Zhoushan 316000, China.
Molecules. 2025 Mar 18;30(6):1353. doi: 10.3390/molecules30061353.
In this study, a method for the determination of eight biogenic amines (BAs), including tyramine (Tyr), 2-phenylethylamine (2-Phe), histamine (His), tryptamine (Trp), spermidine (Spd), spermine (Spm), cadaverine (Cad), and putrescine (Put), in crab was established using ultra-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS), using a magnetic solid-phase extraction (MSPE) pretreatment, without derivatization, and the content changes in regard to these eight biogenic amines in the traditional Chinese dish, pickled swimming crabs, were investigated. The samples were purified via MSPE, using C nanofiber-coated magnetic nanoparticles (FeO@C-NFs) as sorbents. The experimental variables involved in the MSPE, including the solution pH, adsorption and desorption time, adsorbent usage, and type and volume of the eluent, were investigated and optimized. Method validation indicated that the developed method showed good linearity (R > 0.995); the average recovery rates were 84.7% to 115%, with the intra-day and inter-day relative standard deviations (RSD, = 6) ranging from 3.7% to 7.5% and 4.2% to 7.7%, respectively. The limit of detection (LOD) and limit of quantification (LOQ) for the eight BAs were 0.1 mg/kg1.0 mg/kg and 0.3 mg/kg3.0 mg/kg, respectively. Finally, this method was applied to determine the changes in the eight biogenic amines in pickled swimming crabs () during storage at 20 °C and 400 BAC. Among the BAs evaluated, Cad, Put, and Tyr were the predominant amines formed during storage. The final content of Cad, Put, and Tyr reached 22.9, 20.1, and 29.0 mg/100 g at 4 °C for 16 d, and 47.1, 52.3, and 72.0 mg/100 g at 20 °C for 96 h, respectively. The results from this study can be used to expand the application range of magnetic materials in biogenic amine pretreatment and to strengthen the quality control of the traditional Chinese dish, pickled swimming crabs.
本研究建立了一种采用超高效液相色谱串联质谱法（UHPLC-MS/MS）测定蟹中8种生物胺（BAs）的方法，该方法采用磁性固相萃取（MSPE）进行预处理，无需衍生化，并对传统中式菜肴醉蟹中这8种生物胺的含量变化进行了研究。样品通过MSPE进行净化，使用碳纳米纤维包覆的磁性纳米颗粒（FeO@C-NFs）作为吸附剂。对MSPE过程中涉及的实验变量，包括溶液pH值、吸附和解吸时间、吸附剂用量以及洗脱剂的类型和体积进行了研究和优化。方法验证表明，所建立的方法具有良好的线性（R>0.995）；平均回收率为84.7%至115%，日内和日间相对标准偏差（RSD，n = 6）分别为3.7%至7.5%和4.2%至7.7%。8种生物胺的检测限（LOD）和定量限（LOQ）分别为0.1 mg/kg1.0 mg/kg和0.3 mg/kg3.0 mg/kg。最后，该方法用于测定醉蟹在20℃和400 BAC条件下储存期间8种生物胺的变化。在所评估的生物胺中，尸胺、腐胺和酪胺是储存过程中形成的主要胺类。在4℃下储存16 d时，尸胺、腐胺和酪胺的最终含量分别达到22.9、20.1和29.0 mg/100 g，在20℃下储存96 h时分别达到47.1、52.3和72.0 mg/100 g。本研究结果可用于扩大磁性材料在生物胺预处理中的应用范围，并加强传统中式菜肴醉蟹的质量控制。
