Wu Yunhui, Zhou Shuang, Xu Dunming
Xiamen Ocean Vocational College, Xiamen 361100, China.
Se Pu. 2013 Feb;31(2):111-6. doi: 10.3724/sp.j.1123.2012.09037.
Abstract: A method for the determination of histamine (HIS), tryptamine (TRP), 2-phenylethylamine (2-PHE), putrescine (PUT), cadaverine (CAD), tyramine (TYR), spermidine (SPD), spermine (SPM) in animal-derived foodstuffs was established using high performance liquid chromatography-tandem mass spectrometry. The samples were extracted with acetonitrile-formic acid aqueous solution, and purified with strong cationic exchange (MCX) cartridge. Without derivatization, the eight biogenic amines (BAs) were separated by hydrophilic interaction chromatographic (HILIC) column with the mobile phases of 5 mmol/L ammonium acetate and methanol. The linearities were excellent in the range of 0. 001-100 microg/L with the correlation coefficients above 0.99. The limits of detection (LODs, S/N = 3) of the method were between 0. 001 microg/kg and 1 microg/kg, and the limits of quantification (LOQs, S/N = 10) were between 0.003 microg/kg and 5 microg/kg. The recoveries of BAs spiked in eight matrices were between 73.9% and 106.3% at the spiked levels ranged from 0.003 microg/kg to 50 microg/kg. The relative standard deviations (RSDs, n = 6) were in the ranges of 5.65%-18.6%. The method can meet the requirements of the daily work for the determination of BAs in animal-derived foodstuffs.
建立了一种采用高效液相色谱 - 串联质谱法测定动物源性食品中组胺(HIS)、色胺(TRP)、2 - 苯乙胺(2 - PHE)、腐胺(PUT)、尸胺(CAD)、酪胺(TYR)、亚精胺(SPD)、精胺(SPM)的方法。样品用乙腈 - 甲酸水溶液提取,并用强阳离子交换(MCX)柱净化。无需衍生化,8种生物胺(BAs)通过亲水作用色谱(HILIC)柱,以5 mmol/L醋酸铵和甲醇为流动相进行分离。在0.001 - 100 μg/L范围内线性良好,相关系数高于0.99。该方法的检测限(LODs,S/N = 3)在0.001 μg/kg至1 μg/kg之间,定量限(LOQs,S/N = 10)在0.003 μg/kg至5 μg/kg之间。在8种基质中添加BAs,添加水平为0.003 μg/kg至50 μg/kg时,回收率在73.9%至106.3%之间。相对标准偏差(RSDs,n = 6)在5.65% - 18.6%范围内。该方法能够满足动物源性食品中BAs日常检测工作的要求。