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投稿时间:2016-06-13
投稿时间:2016-06-13
中文摘要: 建立分散固相萃取/超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定食品塑料包装材料中6种烷基胺类物质(4,4'-亚基双环己胺、青霉胺、N,N-二甲基-1,3-丙二胺、N,N-二乙基-1,3-丙二胺、1,6-己二胺和 5-氨基-1,3,3-三甲基环己甲胺)的分析方法。塑料样品用丙酮超声提取,C18和PSA混合净化后经Eclipse Plus C18色谱柱和0.1%甲酸水溶液(体积分数)-乙腈进行梯度洗脱分离,以串联质谱的多反应监测模式检测。6种烷基胺类物质在0.50 μg/L~100μg/L 浓度范围内线性关系良好,相关系数 0.9958~0.9993;方法检出限(S/N=3)为 0.23 μg/kg~0.56 μg/kg,平均回收率为83.6%~103%,精密度(n=6)为2.3%~6.1%。
中文关键词: 烷基胺 分散固相萃取净化 食品塑料包装材料 超高效相色谱-串联质谱法
Abstract:A simple and rapid method for determination of six alkylamines in food contact plastic package materials by ultra-high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS)coupled with dispersive solid phase extraction(d-SPE)was established.The plastic sample was extracted with acetone under ultrasonication,and purified by a simple d-SPE employing PSA and C18 powder.Then the extract was separated on Eclipse Plus C18 UPLC column with acetonitrile and 0.1%formic acid solution (volumn ratio)as mobile phase under gradient elution mode,then detected by tandem mass spectrometry under ESI at positive and multiple reaction monitoring(MRM)mode.The result indicated that the target analytes were in the range of 0.50 μg/L-100 μg/L with correlation coefficient(r)ranging from 0.995 8 to 0.999 3,the method detection limit(LOD,S/N=3)of the analytes were ranged from 0.23 μg/kg-0.56 μg/kg.The mean recoveries were in the range of 83.6%to 103%,with the precision ranging from 2.3%to 6.1%(n=6).
keywords: alkylaminescompounds dispersive solid phase extraction food contact plastic package materials ultra-high performance liquid chromatography-tandem mass spectrometry
文章编号:201614027 中图分类号: 文献标志码:
基金项目:国家质量监督检验检疫总局科技计划项目(2015QK162)
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