Bian Zhaoyang, Tang Gangling, Yang Fei, Pang Yongqiang, Zhang Hongfei, Hu Qingyuan
China National Tobacco Quality Supervision &Test Center, Zhengzhou 450001, China.
Se Pu. 2012 Jun;30(6):590-5. doi: 10.3724/sp.j.1123.2012.01007.
A method of the determination of the carbon-centred radicals in mainstream cigarette smoke using a spin-labelled fluorophore, 4-((9-acridinecarbonyl) amino)-2,2,6,6-tetramethylpiperidin-1-oxyl (TEMPO-9-AC), as a fluorescent probe is presented. After being producted by smoking in International Organization for Standardization (ISO) mode, the carbon-centred radicals in mainstream cigarette smoke were trapped by TEMPO-9-AC, a carbon-centred radical probe with a low fluorescence intensity. Then the latter was transformed to a stable diamagnetic o-alkoxyamine, a high-fluorescence compound. Finally, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was used to demonstrate the structures of the carbon-centred radicals, and high performance liquid chromatography with a fluorescence detector (HPLC-FLD) was used to determine the concentration of the carbon-centred radicals. The results showed that the 10 carbon-centred radicals were detected in the mainstream cigarette smoke, and the total carbon-centred radicals concentrations for 1R5F, 3R4F, CM6, and two Virginia type cigarettes, were 52.5 nmol/cig, 214.6 nmol/cig, 424.1 nmol/cig, 68.6 nmol/cig, and 334.2 nmol/cig, respectively; and there was positive relation between the concentrations of the total amount of carbon-centred radicals and the tar amounts in the mainstream cigarette smoke. The detection limit was 0.318 nmol/cig, and the relative standard deviations (RSDs) ranged from 3.5% to 9.7%. This method is suitable for the determination of the carbon-centred radicals in the mainstream cigarette smoke.
介绍了一种使用自旋标记荧光团4-((9-吖啶羰基)氨基)-2,2,6,6-四甲基哌啶-1-氧基(TEMPO-9-AC)作为荧光探针测定主流卷烟烟气中碳中心自由基的方法。在按照国际标准化组织(ISO)模式吸烟产生主流卷烟烟气后，烟气中的碳中心自由基被荧光强度较低的碳中心自由基探针TEMPO-9-AC捕获。然后后者转化为稳定的抗磁性邻烷氧基胺，一种高荧光化合物。最后，采用高效液相色谱-串联质谱(HPLC-MS/MS)表征碳中心自由基的结构，采用带荧光检测器的高效液相色谱(HPLC-FLD)测定碳中心自由基的浓度。结果表明，在主流卷烟烟气中检测到10种碳中心自由基，1R5F、3R4F、CM6和两种弗吉尼亚型卷烟的碳中心自由基总浓度分别为52.5 nmol/支、214.6 nmol/支、424.1 nmol/支、68.6 nmol/支和334.2 nmol/支；主流卷烟烟气中碳中心自由基总量浓度与焦油含量之间存在正相关关系。检测限为0.318 nmol/支，相对标准偏差(RSDs)为3.5%至9.7%。该方法适用于测定主流卷烟烟气中的碳中心自由基。
