超高效液相色谱-电喷雾串联质谱法同时测定鱼类加工品中12种杂环胺类化合物

建立了超高效液相色谱-电喷雾串联质谱法同时测定鱼类加工品中12种杂环胺类化合物（HAAs）的分析方法。经过条件优化,肉样选用乙酸乙酯、氨水和三乙胺提取,提取液经MCX固相萃取小柱净化,按V（甲醇）∶V（氨水）=9∶1洗脱,采用Thermo Hypersil Gold C18色谱柱,以甲醇和5 mmol.L-1乙酸铵溶液为流动相进行梯度洗脱分离,电喷雾离子源（ESI）,正离子模式,采用选择反应监测（SRM）扫描模式,内标法进行定量分析。结果表明,12种HAAs在1.0～100.0μg.L-1范围内线性关系良好,相关系数R〉0.99,在12 min内实现分离,3个加标水平的平均回收率为42.98%～125.00%（n=6）,相对标准偏差（RSD）为1.49%～9.88%,检测限（LOD）为0.3～1.0μg.kg-1。该方法简便快捷,准确度高,易推广应用,可作为快速测定鱼类加工品中多种HAAs的有效方法。

Simultaneous determination of 12 heterocyclic aromatic amines in fish processing products by UPLC/ESI-MS/MS

We established a method for simultaneous determination of 12 heterocyclic aromatic amines（HAAs） in fish processing products using ultra-high performance liquid chromatography-electrospray ionization tandem mass spectrometry（UPLC/ESI-MS/MS）.After optimizing the conditions,taking ethyl acetate,ammonia and triethylamine as extraction solutions,we purified the extract with MCX SPE column,and eluted by V（methanol）：V（ammonia）=9：1.Based on a Thermo Hypersil Gold C18 column,we performed a gradient elution separation by methanol and a gradient elution with the mobile phase of 5 mmol · L-1 ammonium acetate.Electrospray ionization source was applied and operated in positive ion mode,using selected reaction monitoring（SRM） scan mode and internal standard method for quantitative analysis.The results reveal that 12 HAAs show a good linear relationship within 1.0~100.0 μg · L-1（R〉0.99）.The separation was finished within 12 min.The average recovery（n= 6） of the 12 HAAs spiked in tested samples at 3 levels ranged from 42.98% to 125.00% with the relative standard deviation（RSD） between 1.49% and 9.88%,and the limit of detection（LOD） was in the range of 0.3~1.0 μg · kg-1.This simple,rapid and highly accurate method can effectively determine various HAAs in fish processing products,easily be applied and popularized.