摘要
通过顶空固相微萃取进样器(HS-SPME)对卷烟主流烟气剑桥滤片中的游离烟碱进行萃取,并用气相色谱/质谱(GC/MS)进行外标法定量分析,对溶剂、萃取纤维、预平衡时间、萃取时间、萃取温度、脱附时间等分析条件进行了优化.同时建立了滤片不同含水量对游离烟碱测定影响的校正曲线,根据实际样品主流烟气粒相物水分的含量对游离烟碱的测定值进行校正,实现了对游离烟碱存在环境无干扰的条件下简便、快速、准确测定卷烟主流烟气粒相物中的游离烟碱.以参比卷烟3R4F为实际样品进行测定时,本方法的RSD为8.3%,检测限和定量限分别为0.2μg/支和0.5μg/支.
An improved,rapid method to measure free-base nicotine in mainstream cigarette smoke accurately by commercial headspace solid phase microextraction(HS-SPME) combined with GC/MS was established.The factors which play important roles in the determination of free-base nicotine,such as the solvent used for preparation of standards,SPME fiber,pre-equilibrium time before HS-SPME,extraction temperature and time,desorption time,were optimized carefully.Furthermore,an experimental water correction factor based on the water content of particulate phase was established to correct free-base nicotine in actual samples.The precision of the method was evaluated with smoke samples of reference cigarettes(Kentucky reference 3R4F) and the RSD obtained was 8.3%.The calculated limit of detection(LOD) and limit of quantification(LOQ) were 0.2 and 0.5 μg/cig,respectively.
出处
《湖南大学学报(自然科学版)》
EI
CAS
CSCD
北大核心
2011年第11期70-75,共6页
Journal of Hunan University:Natural Sciences
基金
红云红河集团科技项目(HYHH2010HX12)
关键词
游离烟碱
卷烟主流烟气
卷烟工业
顶空固相微萃取
色谱分析
气相色谱/质谱法
free-base nicotine
mainstream cigarette smoke
cigarette manufacture
headspace solid-phase microextraction(HS-SPME)
chromatographic analysis
GC/MS