UPLC-MS/MS法同时测定烟叶中的TSNAs

Simultaneous determination of four tobacco-specific N-nitrosamines by liquid chromatography-tandem mass spectrometry

摘要: 为快速准确测定烟叶中的烟草特有亚硝胺(TSNAs),优化改进了LC-MS/MS法中样品的前处理条件,建立了测定烟叶中TSNAs的超高效液相色谱-串联质谱(UPLC-MS/MS)方法。结果表明:①用乙酸乙酯萃取代替固相萃取对TSNAs进行纯化,操作快速准确,更适合大批量样品的分析;②N-亚硝基降烟碱(NNN)、4-(N-甲基-N-亚硝基氨基)-1-(3-吡啶基)-1-丁酮(NNK)、N-亚硝基新烟草碱(NAT)、N-亚硝基假木贼碱(NAB)的定量限分别为4.22、2.38、1.29和0.72 ng/g,加标回收率在87.7%~107.0%之间。

Abstract: An improved method was developed to rapidly determine four tobacco-specific N-nitrosamines (TSNAs) by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The new method offered reduced sample preparation and analysis time as compared to traditional methods. The results showed that:1) ethyl acetate could replace solid phase extraction to purify TSNAs from tobacco leaves; the operation was fast and more suitable for analysing samples of large quantities; 2) the limits of detection (LODs) of N-nitrosonornicotine (NNN), 4-(N-methyl-N-nitrosamino)-1-(3-pyridyl)-1-butanone (NNK), N-nitrosoanatabine (NAT) and N-nitrosoanabasine (NAB) were 4.22, 2.38, 1.29 and 0.72 ng/g, respectively, while the recoveries of the method ranged from 87.7% to 107.0%.