分散固相萃取-气相色谱-串联质谱法测定动物源性食品中9种N-亚硝胺类化合物

Determination of nine N-niitrosamines in animal derived foods by dispersive solid-phase extraction-gas chromatography-tandem mass spectrometry

建立了分散固相萃取-同位素稀释-气相色谱-串联质谱同时测定动物源性食品中9种况-亚硝胺的方法.样品用乙腈提取,上清液经分散固相萃取（dSPE）净化后浓缩.选用DB-WAX极性毛细管色谱柱对待测物进行分离,经EI源电离后以多反应监测（MRM）模式采集数据并做定性筛查和定量分析.9种况-亚硝胺在相应的浓度范围内线性关系良好,相关系数均大于0.99,对4类典型的动物源性食品进行3个不同浓度的加标试验,平均回收率为62.5%-118%,只80为2.11%-25.6%,检出限（[00,5/况=3）为0.02-0.31μg/kg.该方法成本低廉、灵敏可靠,适用于同时对动物源性食品中9种况-亚硝胺进行定性和定量测定.

A method has been developed and validated for the determination of nine N-nitrosamines in animal derived food using dispersive solid-phase extraction （dSPE） coupled with iso-tope dilution-gas chromatography-tandem mass spectrometry （GC-MS/MS）. The samples were extracted by acetonitrile. The extracts were purified using mixed adsorbent by dSPE and then concentrated. The analytes were separated on a DB-WAX polar capillary column,and ionized by EI source. The data were collected by multiple reaction monitoring （MRM） mode,followed by qualitative screening and quantitative analysis. The correlation coefficients of linear calibration curves were over 0. 99 in the corresponding linear ranges. Four kinds of typical animal derived foods were spiked at three levels. The average recoveries of the nine N-nitrosamines ranged from 62. 5% to 118% with RSDs of 2. 11%-25. 6%. The limits of detection （LODs, S/N =3） were 0. 02-0. 31 pg/kg. The method is of low cost, sensitive, reliable,and suitable for the determination of nine N-nitrosamines in animal derived foods.