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 |
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中文摘要: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010 ~048 μg/L,加标回收率为883%~1128%,该方法满足复杂烟气背景下痕量TSNAs的检测要求。 |
中文关键词:磁固相萃取技术(MSPE) 主流烟气 烟草特有N 亚硝胺 液相色谱-串联质谱 |
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A Magnetic Solid Phase Extraction Technique for Determination of Tobacco specific N Nitrosamines in Mainstream Cigarette Smoke |
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Abstract:A magnetic solid phase extraction(MSPE) technique was developed by polymerizing methyl acrylic acid(MAA) on the surface of silica modified Fe3O4 magnetic nanoparticles(Fe3O4@SiO2@MAA MNPs),which was combined with HPLC-MS/MS method to analyze the tobacco specific N nitrosamines(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 Fe3O4@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 883% to 1128% with the limits of quantitation(LOQs) of 010-048 μg/L.The method was suitable for the detection of TSNAs with low contents under the complex background. |
Key Words:magnetic solid phase extraction technique(MSPE) mainstream cigarette smoke tobacco specific N nitrosamines HPLC-MS/MS |
引用本文:陈嘉彬,孙海峰,游金清,朱钢添,何君,谢涛.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[J].分析测试学报,2018,37(5):588-593. |
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