QuEChERS技术结合气相色谱-串联质谱法同时测定水产品中10种亚硝胺

Simultaneous determination of 10 kinds of nitrosamines in aquatic products by QuEChERS combined with gas chromatography-tandem mass spectrometry

目的建立QuEChERS技术结合气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)同时测定水产品中10种亚硝胺含量的分析方法。方法样品经过乙腈-水溶液(1:1,V:V)提取后,利用QuEChERS分散吸附剂净化基质,随后采用多反应监测(multiple reaction monitoring,MRM)模式,外标法定量。结果10种亚硝胺的定量限为1.0μg/kg,并在1.0~100.0 ng/mL范围内线性关系良好,相关系数r≥0.9988。在样品基质中分别添加2、5、20μg/kg 3个水平的混合标准溶液进行加标回收实验,10种亚硝胺的加标回收率为87.5%~102.8%,相对标准偏差(relative standard deviations,RSDs)为1.9%~4.4%(n=6)。结论该方法具有前处理过程快速简便、灵敏度高、稳定性好的优点,并能够满足同时对水产品中10种亚硝胺进行分析检测及准确定量。

Objective To establish a method for the simultaneous determination of 10 kinds of nitrosamines in aquatic products by QuEChERS combined with gas chromatography-tandem mass spectrometry.Methods The samples were subject to mixture of acetonitrile-water(1:1,V:V)for extraction,the matrix was purified by QuEChERS dispersion adsorbent.They were subsequently analyzed in the multiple reaction monitoring(MRM)mode and quantified by external standard method.Results The limits of quantification of 10 kinds of nitrosamines were 1.0μg/kg,and the linear relationships were good in the range of 1.0-100.0 ng/mL with the correlation coefficient(r)≥0.9988.Adding 2,5 and 20μg/kg at 3 levels mixed standard solutions to the sample matrix respectively were used for standard addition recovery experiment.The standard addition recoveries of 10 kinds of nitrosamines were 87.5%-102.8%,and the relative standard deviations(RSDs)were 1.9%-4.4%(n=6).Conclusion This method has the advantages of quick and easy pre-processing,processhighly sensitive,reasonably stable,and it can simultaneously,rapidly determine and quantitatively analyze 10 kinds of nitrosamines in aquatic products.