建立了同时检测干制水产品中9种N-亚硝胺类化合物的气相色谱-三重四极杆串联质谱（GC-MS/MS）方法。采用QuEChERS（quick，easy，cheap，effective，rugged and safe）的前处理方法，样品经乙腈提取后，使用增强型脂质去除产品（Bond Elut EMR-Lipid）基质分散净化，以聚乙二醇石英毛细管柱HP-INNO-WAX（30 m×0.25 mm×0.25 μm）分离化合物，GC-MS/MS采用多反应监测模式（MRM）检测，外标法定量。结果表明，9种N-亚硝胺类化合物在0.30~50.00 μg/L范围内线性关系良好，相关系数（R2）大于0.999，方法的检出限为0.3 μg/kg，定量限为1.0 μg/kg。对鱿鱼、虾干、蚝干和干贝4种基质分别添加1.00 μg/kg、4.00 μg/kg和10.00 μg/kg 3个质量浓度进行加标回收试验，9种N-亚硝胺化合物的回收率为80.41%~113.73%，相对标准偏差（RSD）为1.34%~11.80%（n=6）。市售干制水产品N-二甲基亚硝胺、N-二乙基亚硝胺、N-二丁基亚硝胺、N-亚硝基吡咯烷和N-二苯基亚硝胺均有不同程度的检出。该方法前处理过程简单，节省成本，灵敏度高，稳定性好，定性准确，可快速同时对水产干制品中9种N-亚硝胺类化合物进行定性和定量分析。

A method for the simultaneous determination of nine N-nitrosamines in dried aquatic products by gas chromatography-tandem mass spectrometry (GC-MS/MS) was established. After quick, easy, cheap, effective, rugged, and safe (QuEChERS) pretreatment, the samples were subjected to acetonitrile extraction, followed by the application of Agilent bond elut enhanced matrix removal-lipid (EMR-Lipid). The compounds of interest were separated by a HP-INNOWAX column (30 m×0.25 mm×0.25 μm). They were subsequently analyzed by GC-MS/MS in the multiple reaction monitoring mode (MRM) and quantified by an external standard method. The experimental results show good linearity for the nine N-nitrosamines in the range from 0.30 to 50.00 μg/L, with linear regression coefficients R2 higher than 0.999. The limits of detection are 0.3 μg/kg, and the limits of quantification are 1.0 μg/kg. The average recovery rates of the nine N-nitrosamines were between 80.41% and 113.73% when 1.00 μg/kg, 4.00 μg/kg, and 10.00 μg/kg of N-nitrosamines were added to dried squids, shrimps, oysters, and scallops. Meanwhile, the relative standard deviations (RSDs) were 1.34% to 11.80% (n=6). Different levels of N-nitrosodimethylamine, N-nitrosodiethylamine, N-nitrosodibutylamine, N-nitrosopyrrolidine, and N-nitrosodiphenylamine were detected in dried aquatic products available in the market. The proposed method enables simple pre-treatment, and it is inexpensive, highly sensitive, reasonably stable, and quantitatively accurate. It can rapidly determine and quantitatively analyze nine N-nitrosamines in dry aquatic products.

广东省科技计划项目（2017B020207009；2017A070701039）