Deng Huimin, Yang Fei, Li Zhonghao, Bian Zhaoyang, Fan Ziyan, Wang Ying, Liu Shanshan, Tang Gangling
China National Tobacco Quality Supervision and Test Center, No. 2 Fengyang Street, High and New Technology Industries Development Zone, Zhengzhou 450001, China.
China National Tobacco Quality Supervision and Test Center, No. 2 Fengyang Street, High and New Technology Industries Development Zone, Zhengzhou 450001, China.
J Chromatogr A. 2017 Jul 21;1507:37-44. doi: 10.1016/j.chroma.2017.05.056. Epub 2017 May 27.
Aromatic amines in mainstream cigarette smoke have long been monitored due to their carcinogenic toxicity. In this work, a reliable and rapid method was developed for the simultaneous determination of 9 aromatic amines in mainstream cigarette smoke by modified dispersive liquid liquid microextraction (DLLME) and ultraperformance convergence chromatography tandem mass spectrometry (UPC-MS/MS). Briefly, the particulate phase of the cigarette smoke was captured by a Cambridge filter pad, and diluted hydrogen chloride aqueous solution is employed to extract the aromatic amines under mechanical shaking. After alkalization with sodium hydroxide solution, small amount of toluene was introduced to further extract and enrich aromatic amines by modified DLLME under vortexing. After centrifugation, toluene phase was purified by a universal QuEChERS cleanup kit and was finally analyzed by UPC-MS/MS. Attributing to the superior performance of UPC-MS/MS, this novel approach allowed the separation and determination of 9 aromatic amines within 5.0min with satisfactory resolution and sensitivity. The proposed method was finally validated using Kentucky reference cigarette 3R4F, and emission levels of targeted aromatic amines determined were comparable to previously reported methods At three different spiked levels, the recoveries of most analytes were ranged from 74.01% to 120.50% with relative standard deviation (RSD) less than 12%, except that the recovery of p-toluidine at low spiked level and 3-aminobiphenyl at medium spiked level was 62.77% and 69.37% respectively. Thus, this work provides a novel alternative method for the simultaneous analysis of 9 aromatic amines in mainstream cigarette smoke.
由于其致癌毒性,主流香烟烟雾中的芳香胺长期以来一直受到监测。在这项工作中,开发了一种可靠且快速的方法,通过改进的分散液液微萃取(DLLME)和超高效合相色谱串联质谱(UPC-MS/MS)同时测定主流香烟烟雾中的9种芳香胺。简而言之,香烟烟雾的颗粒相通过剑桥滤片捕获,并用稀释的盐酸水溶液在机械振荡下萃取芳香胺。用氢氧化钠溶液碱化后,引入少量甲苯,通过改进的DLLME在涡旋下进一步萃取和富集芳香胺。离心后,甲苯相通过通用的QuEChERS净化试剂盒进行净化,最后通过UPC-MS/MS进行分析。由于UPC-MS/MS的卓越性能,这种新方法能够在5.0分钟内分离并测定9种芳香胺,分辨率和灵敏度令人满意。该方法最终使用肯塔基参考香烟3R4F进行了验证,所测定的目标芳香胺的排放水平与先前报道的方法相当。在三个不同的加标水平下,大多数分析物的回收率在74.01%至120.50%之间,相对标准偏差(RSD)小于12%,除了低加标水平下对甲苯胺的回收率为62.77%,中等加标水平下3-氨基联苯的回收率为69.37%。因此,这项工作为同时分析主流香烟烟雾中的9种芳香胺提供了一种新的替代方法。