徐琦, 杨洪生, 吴光红, 张美琴. 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[J]. 南方水产科学, 2012, 8(4): 7-15. DOI: 10.3969/j.issn.2095-0780.2012.04.002
引用本文: 徐琦, 杨洪生, 吴光红, 张美琴. 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[J]. 南方水产科学, 2012, 8(4): 7-15. DOI: 10.3969/j.issn.2095-0780.2012.04.002
XU Qi, YANG Hongsheng, WU Guanghong, ZHANG Meiqin. Simultaneous determination of 12 heterocyclic aromatic amines in fish processing products by UPLC/ESI-MS/MS[J]. South China Fisheries Science, 2012, 8(4): 7-15. DOI: 10.3969/j.issn.2095-0780.2012.04.002
Citation: XU Qi, YANG Hongsheng, WU Guanghong, ZHANG Meiqin. Simultaneous determination of 12 heterocyclic aromatic amines in fish processing products by UPLC/ESI-MS/MS[J]. South China Fisheries Science, 2012, 8(4): 7-15. DOI: 10.3969/j.issn.2095-0780.2012.04.002

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

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

  • 摘要: 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 mmolL-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1.0~100.0 gL-1范围内线性关系良好,相关系数R0.99,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0.3~1.0 gkg-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。

     

    Abstract: 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 solution, 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 mmolL-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 resultsrevealthat 12 HAAs show a good linear relationship within 1.0~100.0 gL-1 (R0.99). The separationwas 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 gkg-1. This simple, rapid and highly accurate method can effectively determine various HAAs in fish processing products, easily be applied and popularized.

     

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