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食品研究与开发:2017,38(6):153-159
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肉制品中N-二甲基亚硝胺测定及不确定度评定
冯秀娟,马桂娟,王紫昕,张文轩,张瑶
(宁夏回族自治区食品检测中心,宁夏 银川 750000)
Uncertainty Evaluation and the Determination of N-dimethyl Nitrosamine in Meat Products
FENG Xiu-juan, MA Gui-juan, WANG Zi-xin, ZHANG Wen-xuan, ZHANG Yao
(Ningxia Hui Autonomous Region Food Testing Center, Yinchuan 750000, Ningxia, China)
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投稿时间:2016-07-11    
中文摘要: 建立气相色谱/三重四级杆质谱法测定肉制品中 N-二甲基亚硝胺的方法, 并对测定过程中可能引入的不确定 度进行分析和评定。试样经 QuEChERS 方法提取后采用 MRM 模式进行定性定量;建立不确定度评定的数学模型,确定 并简化不确定度来源,计算合成不确定度和扩展不确定度。加标回收率范围为 87.8 %~115.3 %,相对标准偏差(RSD)在4.3 %~6.2 %,线性相关系数达 0.999 5,实际分析 15 份样品中检出 5 份阳性样品,含量均低于国家限量值 3.0 μg/kg;测定3.0 μg/kg 时,N-二甲基亚硝胺的含量是(3.0±0.18)μg/kg,相对扩展不确定度为 6.0 %。该试验方法步骤简单、有机溶剂用 量少、灵敏度高,重现性好,满足国家限量检测的要求;本方法适用于 GC-MS/MS 测定肉制品中 N-二甲基亚硝胺的不确 定度评定。
Abstract:Toestablish a method for the determination of N-dimethyl nitrosamine in meat by gas chromatogra- phy/triple level 4 pole mass spectrometry. Meanwhile, analyzing and evaluating the uncertainty which was prop- erly occurred during the method. Samples were extracted by QuEChERS method, which followed by qualitative and quantitative analysis using MRM model. According to set up the mathematical model for the uncertainty e- valuation, it confirmed and simplified the source of uncertainty, as well as calculated the combined uncertainty and the expanded uncertainty. The range of recovery rate with standard solution was 87.8 % to 115.3 % ,relative standard deviation(RSD) was 4.3 % to 6.2 % and the linearly dependent coefficient was 0.999 5. It was showed that there were 5 samples were positive samples(there were 15 samples totally) and the content of those all five samples were lower than the national limited value which was 3.0 μg/kg. The content of N-dimethylnitrosamine was (3.0±0.18)μg/kg and the relative expanded uncertainty was 6.0 % under the condition of detecting 3.0 μg/ kg.Conclusionit could be found that this method was easy, high sensitivity, better repeatability, lower organic solvent consumption and satisfying the requirements of national trace detection. Thus, this method can be used in the uncertainty evaluation during the determination of N-dimethylnitrosamine by GC-MS/MS.
文章编号:201706035     中图分类号:    文献标志码:A
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