碱处理结合盐辅助分散液液微萃取GC-MS/MS检测即食鱼制品中7种N-亚硝胺

Determination of Seven N-Nitrosamines in Ready-to-Eat Fish Products by GC-MS/MS with Alkali-Treatment Coupled Salt-Assisted Dispersive Liquid-Liquid Microextraction

为提高N-亚硝胺的相关检测效率,建立了碱处理结合盐辅助分散液液微萃取(SADLLME)气相色谱-串联质谱法(GC-MS/MS)检测即食鱼制品中7种N-亚硝胺的新方法。样品经氢氧化钡溶液热处理,转移目标物至水溶液中,在辅助盐硫酸钠近饱和条件下,以二氯甲烷为萃取剂进行SADLLME,应用GC-MS/MS进行检测。方法检出限为0.10~0.19μg/kg,定量限为0.28~0.56μg/kg;加标水平为1、5、10μg/kg时,加标回收率为79.19%~117.40%,相对标准偏差为1.06%~10.30%。结果表明:此方法灵敏、可靠,选择性好,样品前处理简单,能够满足相关食品中N-亚硝胺检测的需要。

To improve the detection efficiency,a new method for the determination of 7 N-nitrosamines in ready-to-eat fish products was developed by GC-MS/MS with alkali treatment coupled salt-assisted dispersive liquid-liquid microextraction(SADLLME).The sample was heated with barium hydroxide solution to transfer N-nitrosamines into the water based solution.Then SADLLME was carried out with dichloromethane as extractant and nearly saturated sodium sulfate as assisted salt,and the analytes extracted were determination by GC-MS/MS.The limits of detection and limits of quantitation were 0.10-0.19μg/kg and 0.28-0.56μg/kg,respectively.The recoveries were 79.19%-117.40%with relative standard deviations of 1.06%-10.30%at 1,5 and 10μg/kg spiking levels.The results showed that the method was sensitive,reliable and good selective with simple sample pretreatment and it could meet the needs of monitoring of N-nitrosamines in related foods.