固相萃取-超高效液相色谱-电喷雾串联质谱法同时测定烤鱼中15种杂环胺含量

Simultaneous Determination of 15 Heterocyclic Amines in Grilled Fish Using Solid Phase Extraction and Ultra Performance Liquid Chromatography with Electrospray Ionization Tandem Mass Spectrometry

建立了固相萃取-超高效液相色谱-电喷雾串联质谱同时分析烤鱼中15种杂环胺（HAs）含量的方法。样品经甲醇-1.0 mol/L NaOH均质、涡旋振荡、超声提取,采用Lichrolut EN固相萃取柱净化,用乙醇-二氯甲烷溶液洗脱,收集洗脱液,水浴下用氮气吹干,加入乙酸-乙酸铵缓冲液涡旋溶解,以乙腈定容,微孔滤膜过滤,UPLC-ESI-MS/MS检测。采用内标法进行定量分析,结果表明,15种杂环胺在1.0~50.0 mg/L范围内线性关系良好,相关系数r〉0.99,定量限（LOQ）为1.0 mg/kg。杂环胺回收率多在79.0%~118.8%之间,相对标准偏差多在1.3%~10.0%之间。

A method based on solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry（UPLC-ESI-MS/MS） has been developed for the analysis of 15 heterocyclic amines（HAs） in grilled fish with multiple reaction monitoring（MRM）.The analytes were extracted from the sample using methanolic NaOH,and purified by solid-phase extraction cartridge,then eluted with ethanolic methylene chloride.The residue was dried under nitrogen and dissolved in acetic acid and ammonium acetate solution before transferring to UPLC-MS/MS.The quantitation was carried out using internal standard method.The linear range was from 1.0 mg/L to 50.0 mg/L for 15 HAs with the good correlation coefficients（r≥0.99）.The limit of quantitation was 1.0 mg/Kg.The recoveries for most compounds were between 79.0%-118.8% and the relative standard deviations were between 1.3% and 10.0%.The method is simple,accurate and sensitive for the simultaneous determination of 15 HAs.