高效液相色谱-串联质谱法测定腌制肉制品中的N,N-二甲基亚硝胺含量

Determination of N,N-dimethylnitrosamine in marinated meat products by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  高效液相色谱-串联质谱法  腌制肉  N,N-二甲基亚硝胺  固相吸附剂

英文关键词:high performance liquid chromatography-tandem mass spectrometry  marinated meat  N,N-dimethylnitrosamine  solid phase adsorbent

中文摘要:

      目的 建立测定腌制肉制品中的N,N-二甲基亚硝胺含量的高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)。方法 样品经乙腈超声提取后,离心, 提取液用增强型基质去除固相吸附剂(enhanced matrix removal, EMR)进行净化, 盐析后得到处理液。在优化的色谱及质谱条件下, 采用ESI 正离子模式电离, 多反应监测(multiple reaction monitoring, MRM)模式扫描测定。结果 N,N-二甲基亚硝胺在2.0~50 μg/L 范围内线性关系良好, 相关系数r 为0.9998, 方法检出限(limit of detection, LOD)和定量限(limit of quantitation, LOQ)分别为0.5 μg/kg 和2.0 μg/kg, 平均回收率为95.6%~102.5%, 相对标准偏差为4.35%~6.76%。结论 该方法操作简便、快速高效、回收率高、灵敏度高、重复性好, 可用于实际测定腌制肉制品中的N,N-二甲基亚硝胺含量。

英文摘要:

      Objective To establish a method for determination of N,N -dimethyl nitrosamine content in salted meat by high performance liquid chromatography-tandem mass spectrometry (HPLC/MS/MS). Methods After ultrasonic extraction of acetonitrile, the sample was centrifuged, the enhanced matrix removal (EMR) was used to remove the enhanced matrix removal, and the treatment solution was obtained. In the optimized chromatography and mass spectrometry conditions, the ESI cation mode was used to ionize. Multiple reaction monitoring (MRM) pattern scanning was used to measured. Results N,N-dimethylnitrosamine had a good linear relationship in the range of 2.0-50 μg/L, and the correlation coefficient was 0.9989. The limits of detection and the limits of quantitation were 0.5μg/kg and 2.0 μg/kg, respectively. The recoveries were 95.6%-102.5%, with the relative standard deviations of 4.35%-6.76%. Conclusion This method is easy, efficient, with high recovery, good sensitivity and high precision,which is suitable for practical determination of N,N-dimethylnitrosamine in marinated meat products.