建立了液相色谱串联质谱法(LC-MS/MS)测定烟用香精及料液中N-亚硝基去甲基烟碱(NNN)、N-亚硝基假木贼碱(NAB)、N-亚硝基新烟草碱(NAT)和4-(N-甲基-N-亚硝胺)-1-(3-吡啶基)-丁酮(NNK)4种烟草特有亚硝胺(TSNAs)的方法。样品采用含0.1 mol/L的醋酸铵甲醇水溶液溶解提取，在C18色谱柱上采用梯度洗脱分离目标物和干扰物，电喷雾正离子模式下，多反应检测模式测定。结果表明，4种TSNAs的检测限(S/N=3)和定量限(S/N=10)分别为0.4~1.6 ng/g和1.4~4.8 ng/g，标准工作液在1~50 ng/L的范围内线性良好，相关系数均大于0.9995，高中低三个浓度水平的加标回收率在93.5%~105.9%之间，6次重复实验的RSD范围为1.8%~4.7%，均小于5%。使用该方法分析测定了8个市售烟用香精香料样品，其中3个样品检测到TSNAs。该方法准确、灵敏，适用于烟用香精及料液样品中TSNAs的分析检测。

Four tobacco-specific nitrosamlnes (TSNAs), including (R,S)-N-Nitrosoanabasine (NAB), (R,S)-N-Nitrosoanatabine (NAT), 4-(Methylnitrosoamino)-1-(3-pyridinyl)-1-butanone (NNK), and rac N’-Nitrosonornicotine (NNN) in tobacco essence and flavor were determined by liquid chromatography tandem mass spectrometry (LC-MS/MS). Sample were dissolved and extracted with 0.1 mol/L ammonium acetate methanol-water solution. The compounds were separated by gradient elution on C18 column and detected in positive ion mode using multiple reactions monitoring with a triple-quadruple MS of electrospray ionization. The results showed that the limits of detection (S/N= 3) and limits of quantity (S/N= 10) of four TSNAs were in the range of 0.4~1.6 ng/g and 1.4~4.8 ng/g, respectively. The linear correlation coefficients were above 0.9995 within 1~50 ng/L, and the recovery rates were between 93.5% to 105.9% in high, medium and low spiked levels. The relative standard deviation (RSD) of six repeat tests was below 5% (1.8~4.7%). Eight tobacco essence and flavor samples were evaluated by the method, and three samples were detected TSNAs. The method is of good efficiency, sensitivity and selectivity, and can be successfully applied to determine the TSNAs in varieties of tobacco essence and flavor.

国家烟草专卖局卷烟减害技术重大专项子项目(110200902013)