磁固相萃取技术应用于主流烟气中烟草特有N-亚硝胺的测定

摘要

A magnetic solid phase extraction(MSPE) technique was developed by polymerizing methyl acrylic acid (MAA) on the surface of silica modified Fe3 O4 magnetic nanoparticles (Fe3 O4@SiO2@MAA MNPs),which was combined with HPLC-MS/MS method to analyze the tobacco-specific Nnitrosamines(TSNAs) in mainstream cigarette smoke.In this method,TSNAs were enriched by adding magnetic nano-particles to the extract.The separation was fast under the effect of magnetic materials.The eluent was detected by HPLC-MS/MS under multiple reaction monitoring mode,which could meet the requirements for detection of trace TSNAs in low tar and new tobacco products.The results showed that Fe3 O4@SiO2@MAA MNPs had the uniform size,good monodispersity and super paramagnetism,on which surfaces the carboxyl functional groups could adsorb TSNAs in the solution for separation and enrichment.The pre-treatment method was rapid and simple,and was suitable for analysis on samples of large quantities.The average recoveries for 4 TSNAs ranged from 88.3％ to 112.8％ with the limits of quantitation(LOQs) of 0.10-0.48 μg/L.The method was suitable for the detection of TSNAs with low contents under the complex background.%合成了甲基丙烯酸改性的Fe3O4磁性纳米颗粒(Fe3O4@SiO2@MAA),建立了磁固相萃取技术与高效液相色谱-串联质谱联用检测主流烟气中烟草特有N-亚硝胺(TSNAs)的方法.该方法通过加入磁性纳米颗粒对萃取液中TSNAs进行富集,洗脱液在HPLC-MS/MS多反应监测模式下进行检测,可满足低焦油和新型烟草制品等低含量TSNAs的检测要求.结果表明:Fe3O4@SiO2@MAA纳米颗粒粒径均一,分散性好,具有超顺磁性,其表面的羧基可吸附溶液中的TSNAs,实现分离富集;该前处理方法操作快速简便,适用于大批量样品分析;4种烟草特有N-亚硝胺的定量下限为0.10～0.48 μg/L,加标回收率为88.3％ ～ 112.8％,该方法满足复杂烟气背景下痕量TSNAs的检测要求.