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液相色谱-串联质谱法测定卷烟主流烟气中的四种致癌物
  • 期刊名称:色谱,2010,V28(08):754-758
  • 时间:0
  • 分类:O658[理学—分析化学;理学—化学]
  • 作者机构:[1]国家烟草质量监督检验中心,河南郑州450001
  • 相关基金:国家自然科学基金项目(No.20701040)
  • 相关项目:新型层状氢氧化物微结构组装体的水相合成、形成机理及应用研究
中文摘要:

N-亚硝基降烟碱(NNN)、4-(亚硝基甲氨基)-1-(3-吡啶基)-1-丁酮(NNK)、N-亚硝基新烟草碱(NAT)和N-亚硝基假木贼碱(NAB)是4种广泛存在于烟草和烟气中的致癌物,准确测定其含量对评估其对人体健康的影响有着重要的作用。采用液相色谱-电喷雾串联质谱(LC-ESIMS/MS)技术建立了卷烟主流烟气中NNN、NNK、NAT和NAB的测定方法,并将其用于中国烤烟和混合型卷烟主流烟气的分析。卷烟主流烟气通过剑桥滤片捕集,捕集烟气后的滤片在加入100μL氘代混合内标后用10mL100mmol/L醋酸铵水溶液萃取,萃取液过水相滤膜后直接进行LC-ESIMS/MS检测。选用AgilentZorbaxEclipseXDB-C18色谱柱,以流动相0.1%(v/v)乙酸水溶液和0.1%(v/v)乙酸甲醇溶液梯度洗脱,质谱检测采用正离子扫描,多反应监测模式。NNN、NNK、NAT和NAB的检出限分别为0.019、0.002、0.008和0.007μg/L,回收率为84.9%~104.5%,相对标准偏差(n=8)为2.96%~6.65%。该方法的检出限低,特异性好,适用于卷烟主流烟气中NNN、NNK、NAT和NAB释放量的检测。

英文摘要:

N-nitrosonornicotine ( NNN) ,4-( methylnitrosamino)-1-( 3-pyridyl)-1-butanone ( NNK) ,N-nitro-soanatabine ( NAT) and N-nitrosoanabasine ( NAB) are the most abundant carcinogens identified in tobacco and tobacco smoke. The accurate quantifications of NNN,NNK,NAT and NAB are necessary to evaluate its impact on the public health. A liquid chromatography-electrospray tandem mass spectrometry ( LC-ESI MS/ MS) method was developed to simultaneously determine NNN,NNK,NAT and NAB in mainstream cigarette smoke. Mainstream smoke was collected in a Cambridge filter pad and then was extracted by 10 mL 100 mmol/L ammonium acetate after 100 μL of mixed deuterated internal standards was added. Then the extract was detected by using positive electrospray ionization on a tandem mass spectrometer in multiple reaction mo-nitoring ( MRM) mode. NNN,NNK,NAT and NAB were separated on a Zorbax Eclipse XDB-C18 column with the gradient elution using mobile phase A ( 0. 1% acetic acid in water) and mobile phase B ( 0. 1% acetic acid in methanol) . The detection limits for NNN,NNK,NAT and NAB were 0. 019,0. 002,0. 008 and 0. 007 μg/L,respectively. The recoveries were varied from 84. 9% to 104. 5% for Chinese Virginia cigarettes and the relative standard deviations ( n =8) ranged from 2. 96% to 6. 65%. This proposed approach,which provides a higher sensitivity and specificity,is suitable for the determination of NNN,NNK,NAT and NAB in mainstream cigarette smoke.

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