在线液相-气相二维色谱高灵敏测定卷烟主流烟气中的4-（N-甲基亚硝胺基）-1-（3-吡啶基）-1-丁酮

建立了在线液相-气相二维色谱测定卷烟主流烟气中4-(N-甲基亚硝胺基)-1-(3-吡啶基)-1-丁酮(NNK)的方法。 NNK 的分析在在线凝胶气质联用仪上进行,采用自行装填的微型碱性氧化铝柱,并把仪器上的凝胶柱换成氧化铝柱,用于 NNK 的分析。捕集有主流烟气总粒相物的剑桥滤片用二氯甲烷提取,以 D4-NNK 为内标,提取液经微型氧化铝柱分离,含 NNK 的部位切割进入气相色谱,排干溶剂后启动气相色谱升温经毛细管柱进行分离,用质谱检测。本方法将烟气国标方法 NNK 测定中的氧化铝柱色谱净化和气相色谱-质谱分析在线连接起来,可不经样品前处理净化直接进样分析；每次进样可达40μL,是常规气相色谱-质谱分析最大进样量(2.0μL)的20倍,显著提高了分析灵敏度。方法线性范围达1.2~120 ng/ mL,相关系数为r=0.9998,回收率为93.9%~96.0%；检出限和定量限分别为0.25 ng/ mL 和0.9 ng/ mL,样品分析结果与中国烟草总公司企业标准方法进行对比,结果相符合。

Online Liquid Chromatography-Gas Chromatography-Mass Spectrometry for Highly Sensitive Determination of 4-(Methylnitrosamino)-1-(3-pyridyl)-1-butanone in Mainstream Cigarette Smoke

A new approach based on online coupled liquid chromatography-gas chromatography-mass spectrometry ( LC-GC / MS ) was developed for the rapid determination of 4-( methylnitrosamino )-1-( 3-pyridyl)-1-butanone (NNK) in mainstream cigarette smoke, in which a switching valve was employed to online switching between two-dimensional chromatography. The online LC-GC / MS system used in this study was built by using online gel permeation chromatography-gas chromatography-mass spectrometry except that the micro gel column was replaced by micro alkaline alumina column which was prepared by ourselves before. The NNK in mainstream cigarette smoke was collected by a Cambridge filter pad, then the pad was extracted with dichloromethane, and the extract was quantitatively analyzed by online LC-GC / MS with D4-NNK as an internal standard. Online LC-GC / MS allowed online pretreatment purification, and the sample was subjected to online LC-GC / MS without any prior purification, which reduced human error in analysis process. The injection volume of the present online LC-GC / MS could reach 40 μL, which was 20 times of that of the conventional GC / MS (2. 0 μL of injection volume), and thus significantly improved the sensitivity. Under the optimum conditions, good linearity ( r = 0. 9998) was obtained over the range of 1. 2 - 120 ng / mL. The recoveries at three spiked levels ranged from 93. 9% to 96. 0% , and the limits of detection for qualitative and quantitative detection were 0. 25 ng / mL and 0. 9 ng / mL, respectively. All the results obtained by the present method are comparable to those of standard method recommend by China National Tobacco Company.