Determination of Nine N-Nitrosamines in Animal Food by Gas Chromatography-Tandem Mass Spectrometry
摘 要
称取样品10.00 g,加入100 μL由N-二甲基亚硝胺-d6和N-亚硝基二丙胺-d14组成的混合内标溶液(1.00 mg·L-1),加入20 mL乙腈,涡旋1 min,于-20℃冷冻20 min,再加入萃取盐(4 g硫酸镁、1 g氯化钠),迅速振荡30 s,以8 000 r·min-1在0℃离心10 min,取上清液加入10 mL乙腈饱和的正己烷,涡旋1 min,以6 000 r·min-1在0℃离心3 min,去除正己烷层,加入净化填料(50 mg N-丙基乙二胺、150 mg封端十六烷基键合硅胶、900 mg Na2SO4),涡旋1 min,以8 000 r·min-1在0℃离心5 min,取上清液用氮吹浓缩(不吹干),用乙腈定容至1.0 mL,采用气相色谱-串联质谱法测定其中的9种N-亚硝胺类化合物。色谱分析中选用VF-WAXms色谱柱(0.25 mm×30 m,0.25 μm),质谱中选择电子轰击离子源和多反应监测模式。9种N-亚硝胺类化合物的质量浓度在5.0~150 μg·L-1内与其峰面积呈线性关系,检出限为0.1 μg·kg-1,测定下限为0.5 μg·kg-1。加标回收率在89.0%~117%之间,测定值的相对标准偏差(n=6)在0.6%~8.0%之间。
Abstract
10.00 g of the sample was taken, then 100 μL of mixed internal standard solution (1.00 mg·L-1, composed of N-nitrosodimethylamine-d6 and N-nitrosodi-n-propylamine-d14) and 20 mL of acetonitrile were added. After vortexing for 1 min, the mixture was freezed at -20℃ for 20 min. Then extract salt (4 g of magnesium sulfate, 1 g of sodium chloride) was added, and the mixture was oscillated rapidly for 30 s, centrifuged at 8 000 r·min-1 for 10 min at 0℃. The supernatant was taken and 10 mL of acetonitrile saturated n-hexane was added, and the mixture was vortexed for 1 min, centrifuged at 6 000 r·min-1 for 3 min at 0℃. The n-hexane layer was removed, and purification packing material (50 mg of N-propyl ethylenediamine, 150 mg of blocked octadecyl boned silica gel, 900 mg of sodium sulfate) was added. After vortexing for 1 min and centrifuging at 8 000 r·min-1 for 5 min at 0℃, the supernatant was concentrated by nitrogen blowing (not dry), and made up to 1.0 mL with acetonitrile. Nine N-nitrosamine compounds were determined by gas chromatography-tandem mass spectrometry. The VF-WAXms column (0.25 mm×30 m, 0.25 μm) was selected for chromatographic analysis. Electron impact ion source and multiple reaction monitoring mode were selected in mass spectrometry. Linear relationships were found between peak area and mass concentration of the nine N-nitrosamine compounds in the range of 5.0-150 μg·L-1. The detection limits were 0.1 μg·kg-1, and the lower limits of determination were 0.5 μg·kg-1. Recovery obtained by standard addition method ranged from 89.0% to 117%, and the relative standard deviations (n=6) of the measured values ranged from 0.6% to 8.0%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201906007
所属栏目 工作简报
基金项目
收稿日期 2018/8/28
修改稿日期
网络出版日期
作者单位点击查看
备注高蕙文,高级工程师,主要从事食品检测工作,13069433@qq.com
引用该论文: GAO Huiwen,LU Lisha,YUAN Hefang. Determination of Nine N-Nitrosamines in Animal Food by Gas Chromatography-Tandem Mass Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(6): 655~660
高蕙文,陆丽莎,袁荷芳. 气相色谱-串联质谱法测定动物性食品中的9种N-亚硝胺类化合物[J]. 理化检验-化学分册, 2019, 55(6): 655~660
共有人对该论文发表了看法,其中:
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】马强,席海为,王超,等.气相色谱-串联质谱法同时测定化妆品中的10种挥发性亚硝胺[J].分析化学, 2011,39(8):1201-1207.
【2】ANDRADE R, REYES F G R, RATH S. A method for the determination of volatile N-nitrosamines in food by HS-SPME-GC-TEA[J]. Food Chemistry, 2005,91(1):173-179.
【3】徐淼,张倩男,杨辉,等.亚硝胺及前体化合物的致癌效应及其食用安全性研究进展[J].癌变·畸变·突变, 2018,30(1):76-79.
【4】LI L, WANG P, XU X L, et al. Influence of various cooking methods on the concentrations of volatile N-nitrosamines and biogenic amines in dry-cured sausages[J]. Journal of Food Science, 2012,77(5):560-565.
【5】何春红.食品中N-亚硝胺类化合物及其检测方法研究进展[J].安徽农学通报, 2013,19(4):132-134.
【6】李玲,徐幸莲,周光宏.气质联用检测传统中式香肠中的9种挥发性亚硝胺[J].食品科学, 2013,34(14):241-244.
【7】CHARROIS J W A, AREND M W, FROESE K L, et al. Detecting N-nitrosamines in drinking water at nanogram per liter levels using ammonia positive chemical ionization[J]. Environmental Science & Technology, 2004,38(18):4835-4841.
【8】李婷,鲜殷鸣,孙成,等.水中N-亚硝胺类消毒副产物的污染现状及分析技术[J].环境化学, 2012,31(11):1767-1774.
【9】杨宁,陈颖慧,邓莉,等.双填料固相萃取-高效液相色谱/质谱法同时检测腌菜中9种N-亚硝胺[J].分析化学, 2013,41(7):1044-1049.
【10】赵庄,许杨彪,刘向红,等.改进的QuEChERS结合气相色谱-三重四极杆质谱法快速测定酸肉中10种挥发性N-亚硝胺类化合物[J].色谱, 2017,35(10):1086-1093.
【11】刘印平,刘玉欣,云鹏,等.啤酒和腊肠中N,N-二甲基亚硝胺的测定[J].食品安全质量检测学报, 2015,6(10):3834-3838.
【12】赵博,邓美林,杨小珊,等.分散固相萃取-气相色谱-串联质谱法测定动物源性食品中9种N-亚硝胺类化合物[J].色谱, 2016,34(10):998-1004.
【13】樊丽琴,杨贤庆,陈胜军,等.光照及温度对N-二甲基亚硝胺和N-二乙基亚硝胺降解的影响研究[J].南方水产, 2009,5(3):53-58.
【14】蒋万枫,杨钊,张凤艳,等.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.
【2】ANDRADE R, REYES F G R, RATH S. A method for the determination of volatile N-nitrosamines in food by HS-SPME-GC-TEA[J]. Food Chemistry, 2005,91(1):173-179.
【3】徐淼,张倩男,杨辉,等.亚硝胺及前体化合物的致癌效应及其食用安全性研究进展[J].癌变·畸变·突变, 2018,30(1):76-79.
【4】LI L, WANG P, XU X L, et al. Influence of various cooking methods on the concentrations of volatile N-nitrosamines and biogenic amines in dry-cured sausages[J]. Journal of Food Science, 2012,77(5):560-565.
【5】何春红.食品中N-亚硝胺类化合物及其检测方法研究进展[J].安徽农学通报, 2013,19(4):132-134.
【6】李玲,徐幸莲,周光宏.气质联用检测传统中式香肠中的9种挥发性亚硝胺[J].食品科学, 2013,34(14):241-244.
【7】CHARROIS J W A, AREND M W, FROESE K L, et al. Detecting N-nitrosamines in drinking water at nanogram per liter levels using ammonia positive chemical ionization[J]. Environmental Science & Technology, 2004,38(18):4835-4841.
【8】李婷,鲜殷鸣,孙成,等.水中N-亚硝胺类消毒副产物的污染现状及分析技术[J].环境化学, 2012,31(11):1767-1774.
【9】杨宁,陈颖慧,邓莉,等.双填料固相萃取-高效液相色谱/质谱法同时检测腌菜中9种N-亚硝胺[J].分析化学, 2013,41(7):1044-1049.
【10】赵庄,许杨彪,刘向红,等.改进的QuEChERS结合气相色谱-三重四极杆质谱法快速测定酸肉中10种挥发性N-亚硝胺类化合物[J].色谱, 2017,35(10):1086-1093.
【11】刘印平,刘玉欣,云鹏,等.啤酒和腊肠中N,N-二甲基亚硝胺的测定[J].食品安全质量检测学报, 2015,6(10):3834-3838.
【12】赵博,邓美林,杨小珊,等.分散固相萃取-气相色谱-串联质谱法测定动物源性食品中9种N-亚硝胺类化合物[J].色谱, 2016,34(10):998-1004.
【13】樊丽琴,杨贤庆,陈胜军,等.光照及温度对N-二甲基亚硝胺和N-二乙基亚硝胺降解的影响研究[J].南方水产, 2009,5(3):53-58.
【14】蒋万枫,杨钊,张凤艳,等.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.
相关信息