低共熔溶剂-超高效液相色谱-大气压化学离子化-串联质谱法测定火腿肠中9种N-亚硝胺

Determination of 9 kinds of N-nitrosamines in ham sausage by deep eutectic solvents-ultra performance liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry

中文关键词:  低共熔溶剂  N-亚硝胺  绿色提取  超高效液相色谱-大气压化学离子化-串联质谱法  火腿肠

英文关键词:deep eutectic solvent  N-nitrosamines  green extraction  ultra performance liquid chromatography -atmospheric pressure chemical ionization-tandem mass spectrometry  ham sausage

中文摘要:

      目的 建立低共熔溶剂(deep eutectic solvent, DES)-超高效液相色谱-大气压化学离子化-串联质谱法快速测定火腿肠中9种N-亚硝胺污染物的分析方法。方法 样品经水稀释, 微量DES分散萃取, 50%甲醇水复溶, Agilent Infinitylab Poroshell 120 EC-C18 (2.1 mm×150 mm, 2.7 μm)色谱柱分离, 大气压化学电离源电离, 多反应监测模式检测, 内标法定量分析。结果 9种N-亚硝胺在5.0~60.0 ng/mL范围内线性关系良好, 线性相关系数(r)均大于0.999。方法检出限为0.1~0.3 μg/kg, 定量限为0.3~1.0 μg/kg, 回收率为72.1%~111.6%, 相对标准偏差为0.9%~8.4%。结论 低共熔溶剂对N-亚硝胺的萃取效果佳, 可以解决传统操作步骤烦琐的问题。本方法有机试剂用量少、绿色环保, 适用于火腿肠中9种N-亚硝胺的快速、精准检测。

英文摘要:

      Objective To establish a rapid method for determination of 9 kinds of N-nitrosamines in ham sausage by ultra performance liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry with deep euectic solvent (DES). Methods The samples were initially dissolved in water, then extracted using microscale DES, subsequently re-dissolved in 50% methanol-water before separation by Agilent Infinitylab Poroshell 120 EC-C18 (2.1 mm×150 mm, 2.7 μm) column, and atmospheric pressure chemical ionization source ionization-multiple reaction monitoring -positive ion mode detection. Internal standard method was used for quantitative analysis. Results The linear relationships of 9 kinds of N-nitrosamines of 5.0–60.0 ng/mL were good. The correlation coefficients (r) of the 9 kinds of N-nitrosamines above 0.999, the limits of detection were 0.1?0.3 μg/kg, and the limits of quantification were 0.3?1.0 μg/kg. The recovery rates were 72.1%?111.6% and relative standard deviations of 0.9%?8.4%. Conclusion DES has a good extraction effect of N-nitrosamines, which can solve the problem of complicated tradittional operation steps. The method is environmentally friendly and requires a small amount of organic reagents. It is suitable for the rapid and accurate detection of 9 N-nitrosamines in ham sausage.