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-ESI MS/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100 μL氘代混合内标后用10 mL 100 mmol/L 醋酸铵水溶液萃取,萃取液过水相滤膜后直接进行LC-ESI MS/MS检测.选用Agilent Zorbax Eclipse XDB-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0.007 μg/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.
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