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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。
A liquid chromatographic tandem mass spectrometry (LC-MS / MS) was developed for the determination of N-nitrosonominyl nicotine (NNN), N-nitrosoacrine (NAB) Four tobacco-specific nitrosamines (TSNAs), including N-nitrosotetraline (NAT) and 4- (N- methyl-N-nitrosamino) -1- (3-pyridyl) )Methods. Samples were extracted with 0.1 mol / L ammonium acetate in methanol and separated by gradient elution on a C18 column. The electrospray positive ion mode was used to determine the multi-reaction mode. The results showed that the detection limits (S / N = 3) and the limit of quantification (S / N = 10) of the four TSNAs were 0.4-1.6 ng / g and 1.4-4.8 ng / g, respectively. / L, the correlation coefficient was greater than 0.9995, the recoveries of high, middle and low concentration levels were in the range of 93.5% -105.9%, and the RSD range of 6 replicates was 1.8% -4.7%, both of which were less than 5%. Using this method, 8 commercial samples of tobacco flavors and fragrances were analyzed and analyzed, of which 3 samples detected TSNAs. The method is accurate and sensitive and is suitable for the analysis and detection of TSNAs in tobacco flavor and feed samples.