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
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北京市教委食品质量安全北京实验室项目(5075227125)。


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
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Beijing Municipal Education Commission Food Quality and Safety Beijing Laboratory Project (5075227125).

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    摘要:

    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。

    Abstract:

    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.

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侯彤瑶,王宗义,潘晓玉,张丽萍,刘珊,吴天俁.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[J].食品科学技术学报,2021,39(3):176-182.

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  • 收稿日期:2020-04-20
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  • 在线发布日期: 2021-06-08
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