气相色谱-串联质谱法测定无烟气烟草中N,N-二甲基亚硝胺
GC-MS/MS Determination of N-Nitrosodimethylamine in Smokeless Tobacco
摘 要
提出了气相色谱-串联质谱法测定无烟气烟草中N，N-二甲基亚硝胺的方法。无烟气烟草样品（0.500 g）用二氯甲烷10 mL超声萃取，上清液用硅固相萃取柱净化。在气相色谱分离中用DB-WAX石英毛细管色谱柱为固定相，在质谱分析中采用多反应监测模式。采用内标法定量。N，N-二甲基亚硝胺的线性范围为0.2~10 μg·L-1，方法的检出限（3s）为0.018 ng·g-1，测定下限（10s）为0.060 ng·g-1。在3，6，10 ng等3个浓度水平进行加标回收试验，回收率为94.7%~101%，测定值的相对标准偏差（n=5）为2.8%~6.8%。
N,N-二甲基亚硝胺
无烟气烟草
GC-MS/MS
N-nitrosodimethylamine
smokeless tobacco
Abstract
A method of GC-MS/MS for the determination of N-nitrosodimethylamine in smokeless tobacco was proposed. The sample of smokeless tobacco (0.500 g) was extracted ultrasonically with 10 mL of dichloromethane and the supernatant was purified with Si solid phase extraction column. The DB-WAX quartz capillary chromatographic column was used for GC separation and the multiple reaction monitoring mode was adopted in MS determination.Internal standard method was used for quantitative. Linearity range of N-nitrosodimethylamine was found between 0.2 μg·L-1 and 10 μg·L-1 with detection limit (3s) of 0.018 ng·g-1 and lower limit of determination (10s) of 0.060 ng·g-1. Tests for recovery were made by standard addition method at the concentration levels of 3, 6, 10 ng, giving values of recovery and RSD's (n=5) in the ranges of 94.7%-101% and 2.8%-6.8% respectively.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201708011
所属栏目 工作简报
基金项目
收稿日期 2016/8/27
修改稿日期
网络出版日期
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备注刘鸿(1986-),男,湖北鄂州人,工程师,主要从事烟草化学研究工作
引用该论文: LIU Hong,ZHANG Yichun,LU Yifeng,SHI Jiaqin,GU Wenbo. GC-MS/MS Determination of N-Nitrosodimethylamine in Smokeless Tobacco[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(8): 917～922
刘鸿,张怡春,陆怡峰,史佳沁,顾文博. 气相色谱-串联质谱法测定无烟气烟草中N,N-二甲基亚硝胺[J]. 理化检验－化学分册, 2017, 53(8): 917～922
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参考文献
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【17】刘津津,廖晓斌,周真明,等.高效液相色谱串联质谱法测定含藻水氯化消毒后7种亚硝胺物质[J].分析化学, 2015,43(4):502-506.
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【20】芮晓东,胡守毅,曹红云,等.匀浆提取-超高效液相色谱-串联质谱法测定烟草中亚硝胺含量[J].理化检验-化学分册, 2013,49(5):593-596.
【21】杨荣静,卫碧文,高欢,等.气相色谱-正化学电离质谱法检测婴儿奶嘴中N-亚硝胺物质的迁移量[J].理化检验-化学分册, 2013,49(12):1423-1427.
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【23】幸苑娜,倪宏刚,王欣,等.气相色谱-正化学源质谱法测定橡胶中N-亚硝胺及其前体物的迁移量[J].分析化学, 2011,39(7):1065-1070.
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【25】顾文博,周宛虹,陆怡峰,等.气相色谱-三重四极杆串联质谱法测定卷烟烟气中的烟草特有亚硝胺[J].烟草科技, 2013(10):43-48.
【26】何淑娟,赵丽敏,李强,等.气相色谱-质谱法测定肉制品中的9种挥发性N-亚硝胺类物质[J].肉类研究, 2015(1):27-30.
【27】冯桂学,刘莉,顿咪娜,等.固相萃取-气相色谱-质谱法测定水中10种嗅味物质的含量[J].理化检验-化学分册, 2017,53(5):502-506.
【2】BABERSCHKE N, STEINBERG C, SAUL N. Low concentrations of dibromoacetic acid and N-nitrosodimethylamine induce several stimulatory effects in the invertebrate model Caenorhabditis elegans[J]. Chemosphere, 2015,124:122-128.
【3】SUN H, YU L H, WEI H L, et al. A novel antihepatitis drug, bicyclol, prevents liver carcinogenesis in diethylnitrosamine-initiated and phenobarbital-promoted mice tumor model[J]. Journal of Biomedicine and Biotechnology, 2012,2012:1-9.
【4】LIN H L, HOLLENBERG P F. N-nitrosodimethylamine-mediated formation of oxidized and methylated DNA bases in a cytochrome P4502E1 expressing cell line[J]. Chemical Research in Toxicology, 2001,14(5):562-566.
【5】LV C L, LIU Y D, ZHONG R G. Theoretical investigation of N-nitrosodimethylamine formation from dimethylamine nitrosation catalyzed by carbonyl compounds[J]. Journal of Physical Chemistry A, 2009,113(4):713-718.
【6】邓其馨,黄朝章,张建平,等.液相色谱串联质谱法测定烟用香精香料中的亚硝胺[J].现代食品科技, 2014(1):195-199.
【7】费桂琴,陈山丹,白桦,等.高效液相色谱-串联质谱法测定玩具弹性体中13种N-亚硝胺[J].理化检验-化学分册, 2015,51(11):1529-1533.
【8】刘志健,蔡锦安,陈志,等.固相微萃取-气相色谱-质谱法测定橡胶密封圈中8种N-亚硝胺含量[J].理化检验-化学分册, 2016,52(6):643-647.
【9】封棣,易馨如,杨慧敏,等.顶空-固相微萃取-气相色谱-质谱法测定乳胶避孕套中亚硝胺的模拟迁移量[J].理化检验-化学分册, 2014,50(6):670-674.
【10】FDA. Harmful and potentially harmful constituents in tobacco products and tobacco smoke:Established list[J]. Federal Register, 2012,77(64):20027-20034.
【11】BUNCH J E. CORESTA reference products 2010 analysis[J]. Tennessee:American Snuff Company, 2014.
【12】周劼,刘洪伟,彭俊,等.气相色谱-热能分析联用仪测医用橡胶手套中可迁移亚硝胺成分的含量[J].今日药学, 2013(8):480-483.
【13】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.
【14】DALLINGA J W, KRUL C A M, TENFELDE A, et al. Determination of N-nitrosodimethylamine in artificial gastric juice by gas chromatography-mass spectrometry and by gas chromatography-thermal energy analysis[J]. European Journal of Cancer Prevention, 2001,10(3):265-268.
【15】DUTRA C B, ANDRADE R, REYES F G R, et al. Determination of volatile N-nitrosamines in sausages by HS-SPME-GC-TEA[J]. Toxicology Letters, 2006,164(3):274-275.
【16】陈婷,温裕云,欧延,等.固相萃取净化及超高效液相色谱-串联质谱法测定橡胶制品中的13种N-亚硝胺[J].色谱, 2014,32(1):89-94.
【17】刘津津,廖晓斌,周真明,等.高效液相色谱串联质谱法测定含藻水氯化消毒后7种亚硝胺物质[J].分析化学, 2015,43(4):502-506.
【18】朱翔,李伟,刘玉灿,等.超高效液相色谱-三重四极杆质谱联用仪同时检测水中9种亚硝胺[J].分析测试学报, 2014,33(8):866-872.
【19】KOSAKA K, ASAMI M, OHKUBO K, et al. Determination of a N-nitrosodimethylamine precursor in water using ultra-high performance liquid chromatography-tandem mass spectrometry[J]. Analytical Sciences, 2015,31(8):769-772.
【20】芮晓东,胡守毅,曹红云,等.匀浆提取-超高效液相色谱-串联质谱法测定烟草中亚硝胺含量[J].理化检验-化学分册, 2013,49(5):593-596.
【21】杨荣静,卫碧文,高欢,等.气相色谱-正化学电离质谱法检测婴儿奶嘴中N-亚硝胺物质的迁移量[J].理化检验-化学分册, 2013,49(12):1423-1427.
【22】许渝谨.固相萃取-气相色谱-正化学离子源质谱法检测水中9种亚硝胺类消毒副产物[D].青岛:青岛理工大学, 2012.
【23】幸苑娜,倪宏刚,王欣,等.气相色谱-正化学源质谱法测定橡胶中N-亚硝胺及其前体物的迁移量[J].分析化学, 2011,39(7):1065-1070.
【24】U.S. Environmental Protection Agency (EPA) Method 521 Determination of nitrosamines in drinking water by solid phase extraction and capillary column gas chromatography with large volume injection and chemical ionization tandem mass spectrometry (MS/MS)[S].
【25】顾文博,周宛虹,陆怡峰,等.气相色谱-三重四极杆串联质谱法测定卷烟烟气中的烟草特有亚硝胺[J].烟草科技, 2013(10):43-48.
【26】何淑娟,赵丽敏,李强,等.气相色谱-质谱法测定肉制品中的9种挥发性N-亚硝胺类物质[J].肉类研究, 2015(1):27-30.
【27】冯桂学,刘莉,顿咪娜,等.固相萃取-气相色谱-质谱法测定水中10种嗅味物质的含量[J].理化检验-化学分册, 2017,53(5):502-506.
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