色谱

色谱 ›› 2012, Vol. 30 ›› Issue (06): 590-595.DOI: 10.3724/SP.J.1123.2012.01007

• 研究论文 • 上一篇    下一篇

卷烟主流烟气中碳中心自由基的自旋标记荧光表征

边照阳*, 唐纲岭, 杨飞, 庞永强, 张洪非, 胡清源   

  1. 国家烟草质量监督检验中心, 河南 郑州 450001
  • 收稿日期:2012-01-06 修回日期:2012-03-29 出版日期:2012-06-28 发布日期:2012-06-20
  • 通讯作者: 边照阳,硕士,工程师,主要从事烟草化学、烟草质量检验研究. Tel: (0371)67672728, E-mail: zybian@126.com.
  • 基金资助:

    中国烟草总公司郑州烟草研究院院长基金项目(No. 502009CA0340).

Determination of carbon-centred radicals in mainstream cigarette smoke using spin-labelled fluorophore

BIAN Zhaoyang*, TANG Gangling, YANG Fei, PANG Yongqiang, ZHANG Hongfei, HU Qingyuan   

  1. China National Tobacco Quality Supervision & Test Center, Zhengzhou 450001, China
  • Received:2012-01-06 Revised:2012-03-29 Online:2012-06-28 Published:2012-06-20
  • Contact: Zhao-Yang BIAN

PDF

348

被引次数

4

摘要： 以自旋标记荧光探针4-((9-acridinecarbonyl)amino)-2,2,6,6-tetramethylpiperidin-1-oxyl(TEMPO-9-AC)研究了卷烟主流烟气中的碳中心自由基。以吸烟机抽吸卷烟,以弱荧光的TEMPO-9-AC作为捕集剂捕集卷烟主流烟气中的碳中心自由基,生成稳定的强荧光的碳中心自由基捕集加合物,以高效液相色谱-三重四极杆串联质谱联用仪(HPLC-MS/MS)对其结构进行了确认,并建立了高效液相色谱-荧光检测(HPLC-FLD)的定量方法。结果表明,方法的检出限为0.318 nmol/cig,相对标准偏差(RSD)为3.5%～9.7%;利用TEMPO-9-AC捕集体系鉴别出了10种碳中心自由基;对5种代表性卷烟烟气中的碳中心自由基进行了定量计算,获得了它们在主流烟气中碳中心自由基的含量数据,并发现碳中心自由基总量与焦油释放量之间具有高度的相关性。本法检出限低,重复性好,适用于卷烟主流烟气中碳中心自由基的结构验证及释放量的检测分析。

关键词: 高效液相色谱-三重四极杆串联质谱, 高效液相色谱-荧光检测, 卷烟主流烟气, 碳中心自由基, 自旋标记荧光探针

Abstract: 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.

Key words: carbon-centred radicals, high performance liquid chromatography-fluorescence detection (HPLC-FLD), high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), mainstream cigarette smoke, spin-labelled fluorophore probe