Determination of N-Nitrosamine Compounds in Meat Products and Aquatic Products by Gas Chromatography-Tandem Mass Spectrometry
摘 要
样品5.000 0 g经乙酸乙酯(20 mL+10 mL)提取,合并的提取液经C18和乙二胺-N-丙基硅烷(PSA)粉末0.2 g净化,离心提取有机层,氮气吹至1 mL。所得溶液采用极性毛细管色谱柱DB-624UI进行气相色谱分离,多模式进样口(MMI)程序升温(PTV)大体积进样,多反应监测(MRM)模式下进行质谱分析。3种N-亚硝胺类化合物(N-二甲基亚硝胺、N-亚硝基吗啉、N-二丙基亚硝胺)的质量浓度在1.0~40.0 μg·L-1范围内与其峰面积呈线性关系,测定下限(10S/N)分别为0.75,0.39,0.28 μg·kg-1。按标准加入法在具有代表性的肉制品(火腿肠)和水产制品(烤鱼片)中分别进行回收试验,回收率在87.8%~103%之间,测定值的相对标准偏差(n=10)均小于8.0%。
Abstract
The sample (5.000 0 g) was extracted with ethyl acetate (20 mL+10 mL), and the combined extract was purified with 0.2 g of C18 and PSA. After centrifugation, the organic layer was concentrated to 1 mL by N2-blowing. The obtained solution was separated by GC using the polar capillary chromatographic column DB-624 UI and program temperature vent (PTV) large-volume sample-introduction at multimode inlet (MMI). Multiple reaction monitoring (MRM) mode was adopted in MS analysis. Linear relationships between values of peak area and mass concentration of N-nitrosamine compounds (N-nitrosodimethylamine, N-nitroso morpholine and N-nitrosodipropylamine) were found in the range of 1.0-40.0 μg·L-1, with lower limits of determination (10S/N) of 0.75,0.39,0.28 μg·kg-1, respectively. Tests for recovery were made by standard addition method for the representative meat product (ham sausage) and aquatic product (grilled fish), giving results in the range of 87.8%-103% and RSDs (n=10) all less than 8.0%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201801011
所属栏目 工作简报
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收稿日期 2017/1/4
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备注蒋万枫(1976-),男,山东青岛人,高级工程师,研究方向为食品检验,jwfvip@126.com
引用该论文: JIANG Wanfeng,YANG Zhao,ZHANG Fengyan,DONG Shizhu. Determination of N-Nitrosamine Compounds in Meat Products and Aquatic Products by Gas Chromatography-Tandem Mass Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(1): 55~58
蒋万枫,杨钊,张凤艳,董诗竹. 气相色谱-串联质谱法测定肉制品和水产制品中N-亚硝胺类化合物[J]. 理化检验-化学分册, 2018, 54(1): 55~58
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【4】许伟,郇延军,孙冬梅,等.原料猪肉的新鲜度对发酵香肠中亚硝酸盐和亚硝胺变化的影响[J].食品工业科技, 2012,33(10):180-184.
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