UPLC-MS/MS对卷烟烟气中4种烟草特有亚硝胺的快速测定

Rapid Determination of 4 Tobacco-specific Nitrosamines in Mainstream Cigarette Smoke by Ultra-performance Liquid Chromatography Tandem Mass Spectrometry

建立了卷烟主流烟气中烟草特有亚硝胺的超高效液相色谱-电喷雾串联质谱（UPLC-MS/MS）测定方法。在标准吸烟条件下,采用剑桥滤片收集卷烟烟气粒相物,用醋酸铵缓冲液提取粒相物,经固相萃取净化后,以电喷雾正离子多反应监测方式,实现了烟气中N-亚硝基降烟碱、4-甲基亚硝基吡啶基丁酮、N-亚硝基新烟草碱和N-亚硝基假木贼碱的基线分离和快速测定。4种烟草特有亚硝胺在0~400μg/L范围内具有良好线性,相关系数大于0.998,定量下限为0.08~0.15μg/L,加标回收率为72%~104%,相对标准偏差为3.8%~9.7%。该方法灵敏、快速、准确,适用于卷烟烟气中烟草特有亚硝胺的测定。

A specific and sensitive method had been developed to rapidly separate and determine 4 tobacco-specific nitrosamines（TSNAs）,including N＇-nitrosonornicotine（NNN）,4-（N-methylnitrosamino）-1-（3-pyridyl）-1-butanone（NNK）,N＇-nitrosoanatabine（NAT） and N＇-nitrosoanabasine（NAB）,in mainstream cigarettes smoke by employing ultra-performance liquid chromatography tandem mass spectrometry（UPLC-MS/MS）.Total particulate matters in mainstream smoke were trapped by cambridge filter pad under standard smoking condition,extracted by using ammonium acetate buffer as solvent,cleaned up on solid phase extraction（SPE）,and then analyzed by UPLC-MS/MS with positive electrospray ionization（ESI） under multiple reaction monitoring（MRM） mode.The supersonic extraction time,experimental conditions of UPLC and MS were also optimized.Under the optimal conditions,the calibration curves showed good linearity for 4 TSNAs in the concentration ranges of 0-400 μg/L with correlation coefficients above 0.998.The limits of quantitation（LOQ） were between 0.08 and 0.15 μg/L（S/N=10）,and average recoveries ranged from 72% to 104% with RSDs of 3.8%-9.7%.The method was sensitive,rapid and accurate,and was suitable for the determination of TSNAs in mainstream cigarette smoke.