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Development of a heart-cutting supercritical fluid chromatography-high-performance liquid chromatography coupled to tandem mass spectrometry for the determination of four tobacco-specific nitrosamines in mainstream smoke

机译:开发一种心脏切削超临界流体色谱 - 高效液相色谱,偶联至串联质谱法测定主流烟雾中的四种烟草特异性亚硝胺

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This paper proposed a newly developed heart-cutting two-dimensional supercritical fluid chromatography-high-performance liquid chromatography system coupled to tandem mass spectrometry (SFC-HPLC-MS/MS) for the determination of four tobacco-specific nitrosamines (TSNAs) in cigarette mainstream smoke. The orthogonality of five SFC columns and two HPLC columns was evaluated. The 1-AA column was applied for the first dimensional (1D) SFC separation to isolate the target compounds from the complex cigarette smoke matrices, and a trapping column in conjunction with an isocratic pump was employed to capture the 1D elutes. Then, the trapped 1D elutes were transferred into the C18 column through a two-position/six-port valve for the second dimensional (2D) analysis. The ion suppression was significantly reduced by the established SFC-HPLC system; meanwhile, the matrix interferences were eliminated as the results demonstrated. A dynamic range between 0.1 and 20ng/mL was achieved with LOQs of 0.72g/cig for N-nitrosonornicotine (NNN), 0.66g/cig for nicotine-derived nitrosamine ketone (NNK), 0.81g/cig for N-nitrosoanatabine (NAT), and 0.39g/cig for N-nitrosoanabasine (NAB). All the results revealed that the presented method exhibited good repeatabilities and recoveries and could be used as a rapid and reliable approach for routine analysis of TSNAs in mainstream smoke.
机译:本文提出了一种新开发的心切割二维超临界流体色谱 - 高性能液相色谱体系,其耦合到串联质谱(SFC-HPLC-MS / MS),用于测定香烟中的四种烟草特异性亚硝胺(TSNA)主流烟雾。评估了五个SFC列和两个HPLC柱的正交性。将1-AA柱施加用于第一尺寸(1D)SFC分离以将来自复杂香烟烟雾基质的靶化合物分离,并且采用与等物泵结合的捕获柱捕获1D次洗脱。然后,将被困的1D洗脱通过用于第二维(2D)分析的双位置/六端口阀转移到C18柱中。已建立的SFC-HPLC系统显着降低离子抑制;同时,随着结果证明的结果,消除了基质干扰。通过0.72g / cig的Loqs为N-Nitrosonornicotine(NNN),0.66g / cig的尼古丁衍生的硝基胺酮(NNK),0.81g / cig的N-Nitrosoanatabine(NAT )和0.39g / cig用于N-硝基壬嗪(NAB)。所有结果表明,呈现的方法表现出良好的重组和回收率,并可作为主流烟雾中TSNA常规分析的快速可靠的方法。

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