Technology Center, Shanghai Tobacco Group, 200082, Shanghai, PR China.
J Sep Sci. 2013 Aug;36(16):2615-20. doi: 10.1002/jssc.201300030.
A rapid method for the selective determination of four kinds of tobacco-specific nitrosamines, N-nitrosonornicotine, N-nitrosoanatabine, N-nitrosoanabasine and 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone, in mainstream cigarette smoke was developed by GC coupled to positive chemical ionization triple-quadrupole MS. After mainstream cigarette smoke was collected on a cambridge filter pad, the particulate matter was extracted with 0.1 M HCL aqueous solution, cleaned by positive cation-exchange solid extraction, and finally injected into GC-MS/MS using isotopically labeled analogues as internal standards. Excellent linearity was obtained over the concentration range of 0.5-200.0 ng mL(-1) for all tobacco-specific nitrosamines with values for correlation coefficient between 0.9996-0.9999. Limits of detection of each tobacco specific nitrosamine varied from 0.023-0.028 ng cig(-1), and lower limits of quantification varied from 0.077-0.093 ng cig(-1). The recovery of each tobacco specific nitrosamine was from 90.0-109.0%. The relative standard deviations of the intra-day and inter-day precisions were 3.1-5.8 and 3.9-6.6, respectively. This method was applied to reference and domestic cigarettes. The result showed that the method was consistent with traditional methods and can be used as an effective approach for the routine analysis of tobacco-specific nitrosamines.
建立了一种气相色谱-正化学电离串联三重四极杆质谱联用(GC-PCI-MS/MS)快速测定主流烟气中 4 种烟草特有亚硝胺(NNN、NAT、NAB 和 4-(甲基亚硝氨基)-1-(3-吡啶基)-1-丁酮)的方法。采用剑桥滤片捕集主流烟气,用 0.1mol/L HCl 水溶液提取,正相阳离子交换固相萃取净化,以同位素内标法定量。4 种烟草特有亚硝胺在 0.5-200.0ng/mL 范围内线性关系良好,相关系数均大于 0.9996-0.9999。方法检出限为 0.023-0.028ng/cig,定量下限为 0.077-0.093ng/cig。加标回收率为 90.0%-109.0%,日内和日间精密度的相对标准偏差分别为 3.1%-5.8%和 3.9%-6.6%。该方法用于参考和国产卷烟的分析,结果与传统方法一致,可作为烟草特有亚硝胺的常规分析方法。