GC-MS检测咸鱼中N-亚硝胺的条件优化

Determination and optimization of N-nitrosamines in salted fish by gas chromatography-mass spectrometry

  • 摘要: 利用气相色谱-质谱联用(GC-MS)检测咸鱼中的N-亚硝胺,优化了样品前处理条件,比较了固相微萃取(SPME)和二氯甲烷超声萃取对N-亚硝胺的响应强度的影响,探讨了有机溶剂用量、萃取时间、萃取次数对测定的影响。采用选择离子法定性定量检测咸鱼中N-二甲基亚硝胺(NDMA)、N-二乙基亚硝胺(NDEA)、N-亚硝基吡咯烷(NPYR)和N-二丙基亚硝胺(NDPA)4种N-亚硝胺。结果显示,优化后的线性相关系数分别达到0.999 2、0.999 1、0.999 1和0.999 2;线性范围为0~10 μg·mL-1;该方法重现性好,其相对标准偏差(RSD)均≤2.1%;空白加标回收率可达70%~80%;灵敏度高,检测限分别为0.038 6 μg·kg-1、0.022 7 μg·kg-1、0.031 6 μg·kg-1和0.047 8 μg·kg-1

     

    Abstract: We determined N-nitrosamines in salted fish by gas chromatography-mass spectrometry (GC-MS), optimized the sample preparation conditions, compared the response intensity of N-nitrosamines by SPME and dichloromethane ultrasonic extraction as well as explored the impact of organic solvent, extraction time and times on the determination. By ion selective electrode method, we determined the contents of N-dimethylnitrosamine, N-diethylnitrosamine, N-nitroso-pyrrolidine and N-nitrosamines. Results show that the linear correlation coefficient is 0.999 2, 0.999 1, 0.999 1 and 0.999 2, respectively, with a linear range of 0~10 μg·mL-1. The method has good reproducibility (RSD≤2.1%, blank spiked recovery is 70%~80%) and high sensitivity (detection limit is 0.038 6 μg·kg-1, 0.022 7 μg·kg-1, 0.031 6 μg·kg-1 and 0.047 8 μg·kg-1, respectively).

     

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