首页|QuEChERS-EMR-GC/MS测定鱼肉制品中N-二甲基亚硝胺含量的方法学研究

QuEChERS-EMR-GC/MS测定鱼肉制品中N-二甲基亚硝胺含量的方法学研究

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目的:建立一种QuEChERS-EMR结合气相色谱串联质谱技术快速分析鱼肉制品中N-二甲基亚硝胺的方法.方法:样品加入内标,采用乙腈提取,经QuEChERS-EMR净化,VF-WaxMS(60 m×0.25 mm×0.25 µm)色谱柱分离,在单离子检测(SIM)扫描,内标法定量.结果:N-二甲基亚硝胺在2.0~50.0 ng/mL浓度范围内线性关系良好,相关系数r为0.9994,方法检出限为1.0 µg/kg,方法定量限为3.3 μg/kg,添加浓度水平分别为4.0 μg/kg、20 μg/kg、40 µg/kg时,测定回收率在83.1%~104.3%之间,相对标准偏差在3.3%~6.1%之间.鱼肉基质对N-二甲基亚硝胺的基质效应为7.5%,表现为弱基质效应,可以忽略.结论:该方法操作简便,经济高效,环保,准确度高和重复性好,以及基质效应弱,适用于鱼肉制品中N-二甲基亚硝胺的测定.
Methodological study on the determination of N-dimethyl nitrosamine in fish products by QuEChERS-EMR-GC/MS
In this study we established a method for the rapid analysis of N-dimethyl nitrosamine in fish products by QuEChERS-EMR-GC/MS.The internal standard was added to the sample,which was extracted with acetoni-trile,purified with QuEChERS-EMR,separated by VF-WaxMS column(60 m × 0.25 mm × 0.25 µm),scanned under single ion detection(SIM)mode,and quantified by internal standard method.N-dimethyl nitrosamine had good linear relationship within the concentration range of 2.0 ng/mL to 50.0 ng/mL,and the correlation coefficient was 0.9994.The limit of detection was 1.0 μg/kg,and the limit of quantitation was 3.0 μg/kg.The recoveries were between 83.1%and 104.3%when the spiked levels were 4.0 µg/kg,20 µg/kg and 40 μg/kg.The relative stand-ard deviation was between 3.3%and 6.1%.The matrix effect of fish substrate on N-dimethyl nitrosamine was 7.5%,showing a weak matrix effect and could be ignored.The method is simple,efficient and environmental protec-tive,with high accuracy and good repeatability,which is suitable for the determination of N-dimethyl nitrosamine in fish products.

QuEChERS-EMRN-dimethyl nitrosaminefish productsgas chromatography-mass spectrometry

张洁、董榕贵

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贵州省检测技术研究应用中心,贵州 贵阳 550014

QuEChERS-EMR N-二甲基亚硝胺 鱼肉制品 气相色谱串联质谱

2024

贵州科学
贵州科学院

贵州科学

影响因子:0.395
ISSN:1003-6563
年,卷(期):2024.42(4)
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