机构地区: 中国水产科学研究院南海水产研究所
出 处: 《南方水产科学》 2012年第4期16-22,共7页
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0~10μg.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 6μg.kg-1、0.022 7μg.kg-1、0.031 6μg.kg-1和0.047 8μg.kg-1。 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).