1. 上海海洋大学食品学院
2. 上海出入境检验检疫局
3. 岛津国际贸易(上海)有限公司
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王敏, 郭德华, 丁卓平, 等. 液相色谱-离子阱-飞行时间串联质谱同时检测肉制品中14种杂环胺[J]. 分析测试学报, 2011,30(12):1377-1381.
Determination of 14 Heterocyclic Aromatic Amines in Meat Products by Liquid Chromatography-Ion Trap-Time of Flight Tandem Mass Spectrometry[J]. 2011,30(12):1377-1381.
建立了液相色谱-离子阱-飞行时间串联质谱(LCMS-IT-TOF)同时测定肉制品中14种杂环胺(HAAs)残留量的分析方法。样品以乙腈提取,经Phenomenex strata-X-C小柱净化,甲醇-氨水(9∶1)洗脱,氮吹至干,经1 mL乙腈-水(1∶9)定容离心后上机测定,基质曲线内标法定量。结果表明,14种杂环胺在5~250 μg/L质量浓度范围内线性良好,相关系数均不低于0.994 0,检出限(S/N=3)为0.59~3.27 μg/kg。14种杂环胺在加标水平为10、50、250 μg/kg时的回收率分别为69%~107%、67%~106%、76%~113%,相对标准偏差(RSD,n=6)分别为1.5%~15.6%、1.3%~11.8%、1.8%~9.7%。结果显示该方法线性范围宽,精密度和准确度较高,分析时间短,净化效果好,可满足肉制品中多种杂环胺残留同时检测的要求。
A rapid analytical method was developed for the determination of 14 heterocyclic aromatic amines(HAAs) in meat products by liquid chromatography-ion trap-time of flight tandem mass spectrometry(LCMS-IT-TOF).The samples were extracted with acetonitrile.The extract was cleaned up with Phenomenex strata-X-C,eluted with methanol-ammonia(9∶1),then evaporated with a stream of nitrogen to near dryness and redissoved with acetonitrile-water(1∶9).The separation of HAAs was performed on a Phenomenex Kinetex 2.6μ C18 100A (2.1 mm i.d.×100 mm,2.6 μm),using 30 mmol/L ammonium formate-acetonitrile as mobile phase by gradient elution.The analytes were detected under positive ion electrospray ionization mode.Results showed that the linear ranges of 14 HAAs were 5-250 μg/L with limits of detection(S/N=3) of 0.59-3.27 μg/kg.The mean recoveries of all the compounds at three spiked levels of 10,50,250 μg/kg were in the range of 69%-107%,67%-106% and 76%-113%,respectively,with the corresponding RSDs(n=6) of 1.5%-15.6%,1.3%-11.8% and 1.8%-9.7%,respectively.The established method showed a wide liner range and a high sensitivity,and could meet the requirements for the simultanous analysis of the HAAs in meat products.
液相色谱-离子阱-飞行时间串联质谱(LCMS-IT-TOF)肉制品杂环胺(HAA)
liquid chromatography-ion trap-time of flight tandem mass spectrometry(LCMS-IT-TOF)meat productsheterocyclic aromatic amines(HAAs)
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