QuEChERS-气相色谱-串联质谱法测定香肠和火腿肠制品中13种N-亚硝胺化合物

Determination of 13 kinds of volatile N-nitrosamines in sausage and ham products by gas chromatography tandem mass spectrometry

中文关键词:  快速基质分散净化  香肠和火腿肠制品  肉制品  N-亚硝胺  气相色谱-串联质谱法

英文关键词:This method is simple, accurate, sensitive and reproducible, and suitable for rapid detection of N-nitrosamines in meat products.

中文摘要:

      目的 建立采用快速基质分散净化QuEChERS (quick, easy, cheap, effective, rugged, safety)-气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry, GC-MS/MS)快速测定香肠和火腿肠制品中13种N-亚硝胺类化合物的分析方法。方法 样品加入内标, 经乙腈提取, QuCEhERS萃取盐包和基质分散净化包净化, 采用DB-WAXETR(30 m×0.25 mm, 0.25 μm)色谱柱分离, 在多反应监测模式(mult-reaction monitoring, MRM)下测定, 内标法定量。结果 13种N-亚硝胺化合物在1~100 μg/L范围内线性关系良好, 相关系数(r)均大于0.99, 定量限为0.03~2.84 μg/kg; 添加水平为3~30 μg/kg, 平均回收率为59.1%~119.2%, 相对标准偏差为0.6%~15.1% (n=6)。结论 该方法简单准确、灵敏度高、重复性好, 适用于批量肉制品样品中13种N-亚硝胺类化合物的快速检测。

英文摘要:

      Objective To establish a method for the rapid determination of 13 kinds of N-nitrosamines in sausage and ham by QuEChERS (quick, easy, cheap, effective, rugged, safety) extraction and purification and gas chromatography-tandem mass spectrometry (GC-MS/MS). Methods The samples with internal standard were extracted by acetonitrile, purified by QuEChERS extraction salt pack and matrix dispersion purification pack. Then, the samples were separated by DB-WAXETR (30 m×0.25 mm, 0.25 μm) chromatographic column, determined under multi-reaction monitoring mode (MRM) and quantified by internal standard method. Results The linear relationships of 13 N-nitrosamines were good in the range of 1?100 μg/L. The correlation coefficient (r) was greater than 0.99, and the limit of quantitative was 0.03?2.84 μg/kg. The average recovery was 59.1%?119.2% with the addition level of 3?30 μg/kg, and the relative standard deviation was 0.6%?15.1% (n=6).