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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Use of autoclave extraction-supercritical fluid chromatography/tandem mass spectrometry to analyze 4-(methylintrosamino)-1-(3-pyridyl)-1-butanone and N '-nitrosonornicotine in tobacco
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Use of autoclave extraction-supercritical fluid chromatography/tandem mass spectrometry to analyze 4-(methylintrosamino)-1-(3-pyridyl)-1-butanone and N '-nitrosonornicotine in tobacco

机译：使用高压釜提取超临界流体色谱/串联质谱法分析烟草中的4-（甲基氨氨基）-1-（3-吡啶基）-1-丁酮和N'-initrosonornicotine

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4-(methylintrosamino)-1-(3-pyridyl)-1-butanone (NNK) and N'-nitrosonornicotine (NNN) are the most prevalent and toxic tobacco specific nitrosamines (TSNAs). Due to their carcinogenicity, knowledge of the composition of NNK and NNN in tobacco is necessary. Herein, a sensitive and rapid method, which employs autoclave extraction-supercritical fluid chromatography/tandem mass spectrometry (SFC-MS/MS), has been developed for the analysis of NNK and NNN in tobacco. Both water-soluble and matrix-bound NNK and NNN were extracted with 100 mM ammonium acetate in an autoclave (130 degrees C, 4 h), and the aqueous extract was subjected to solvent replacement prior to SFC-MS/MS analysis. NNK and NNN were effectively separated within 5 min by using supercritical CO2 as the main mobile phase coupled with a co-solvent of methanol. Excellent linearity was obtained with coefficients of determination (R-2) greater than 0.9997 in the range of 1-160 ng/mL and 5-800 ng/mL for NNK and NNN, respectively. The recoveries were in the range of 92.5-110.0% at different spiked levels of real samples. 12 tobacco samples which include 3 typical tobacco varieties of burley, flue-cured, and oriental tobaccos had been analyzed, and the fraction of matrix-bound NNK was determined as well. In addition, a comparison between the proposed SFC-MS/MS method and a validated liquid chromatography tandem mass spectrometry (LC-MS/MS) internal standard method was conducted. Both techniques exhibit comparable analysis results, but peak splitting of NNN was observed by LC-MSMS due to the existence of E/Z isomers, while SFC-MS/MS offers great improvement through elution condition optimization, demonstrating the applicability of SFC-MS/MS as an alternative tool for NNK and NNN analysis. (C) 2019 Elsevier B.V. All rights reserved.
机译：4-（甲基氨氨基氨基）-1-（3-吡啶基）-1-丁酮（NNK）和N'-硝化萘豆（NNN）是最普遍的烟草特异性亚硝胺（TSNA）。由于它们的致癌性，需要了解烟草中NNK和NNN的组成。这里，已经开发了一种利用高压灭菌萃取超临界流体色谱/串联质谱（SFC-MS / MS）的敏感和快速方法，用于分析烟草中的NNK和NNN。在高压釜中用100mM乙酸铵（130℃，4小时）萃取水溶性和基质结合的NNK和NNN，在SFC-MS / MS分析之前，将含水提取物进行溶剂置换。通过使用超临界CO2在5分钟内有效地分离NNK和NNN作为与甲醇的共溶剂偶联的主流动相的主流流动相。通过测定系数（R-2）的系数在1-160ng / ml和5-800ng / ml的NNK和NNN的范围内获得优异的线性度。在不同掺入水平的真实样品水平下，回收率在92.5-110.0％的范围内。 12个烟草样品，包括3个典型的烟草品种的伯利，烤烟和东方烟草和东方烟草，也确定了基质结合的NNK的一部分。另外，进行了所提出的SFC-MS / MS方法与验证的液相色谱串联质谱（LC-MS / MS）内标方法的比较。两种技术都表现出可比的分析结果，但由于E / Z异构体的存在，LC-MSMS观察到NNN的峰分裂，而SFC-MS / MS通过洗脱条件优化提供了很大的改进，展示了SFC-MS的适用性/ MS作为NNK和NNN分析的替代工具。 （c）2019 Elsevier B.v.保留所有权利。

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