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

作　　者：张峰[1] 吕泉福[1,2] 储晓刚[1] 李竞[2] 孙利[1] 凌云[1] 杨敏莉[1] 王秀娟[1] 丁菲[1,3] 许成保 

机构地区：[1]中国检验检疫科学研究院,北京100123 [2]西南大学,重庆400715 [3]浙江中医药大学,杭州310053 [4]河北农业大学,保定071000

出　　处：《分析化学》2011年第4期501-505,共5页Chinese Journal of Analytical Chemistry

基　　金：国家科技支撑计划项目(No.2009BADB9B02);质检公益性行业科研项目(No.200910145);国家质检总局科技计划项目(No.2008IK167);北京市科技计划(No.D08050200310803)资助

摘　　要：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.

关 键 词：固相萃取 超高效液相色谱-电喷雾串联质谱 杂环胺 烤鱼 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程]