金属络合衍生-高效液相色谱法测定卷烟主流烟气中的氰化氢  

Determination of Hydrogen Cyanide in Cigarette Mainstream Smoke Using Metal-complexing Derivatization and High Performance Liquid Chromatography

作　　者：朱友[1] 蔚亦沛[1] 别振英[1] 陈玉松[1] 任呼博[1] 罗旭[1] 纪立顺[1] 

机构地区：[1]中国烟草总公司山东省公司,济南250098

出　　处：《中国烟草科学》2015年第5期74-78,84,共6页Chinese Tobacco Science

基　　金：中国烟草总公司山东省公司项目"基于GC-MS指纹图谱技术的卷烟感官质量评价方法研究"(KR203)

摘　　要：建立了金属络合衍生和反相高效液相色谱检测主流烟气中氰化氢的方法.该方法以Ni（II）-NH3 为金属络合衍生化试剂,以5 mmol/L 四戊基溴化铵为离子对试剂,分析时间小于10 min.氰化物标准工作曲线在0.1-20 μg/mL 范围内线性关系良好（R2〉0.999）;检出限和定量限分别为0.049 和0.162 μg/支;3 个加标水平回收率在87.41% - 119.47%.该法与连续流动法测定结果较为一致：肯塔基对照卷烟3R4F 检测结果相对偏差为-5.35%,15 种卷烟样品测定结果相对偏差在-0.79%-8.51%.A reverse phase high performance liquid chromatography method was developed for determination of hydrogen cyanide in cigarette mainstream smoke via metal-complexing derivatization. By using Ni(II)-NH3 as derivatizating agent, the proposed method can achieve the analysis within 10 minutes using 5 mmol/L tetraamylammonium bromide as ion-pair reagent. The method enabled good linearity in the range from 0.1 to 20 μg/m L for the standard working solutions with R2 higher than 0.999. The limit of detection and limit of quantization were 0.049 μg/cig and 0.162 μg/cig, respectively. The recoveries for spiked samples at three levels were between 87.41% and 119.47%. The test results of the proposed method were in good agreement with that of continuous flow method with a relative deviation of-5.35% for Kentucky reference cigarette 3R4 F and a relative deviation range from-0.79% to 8.51% for 15 cigarette samples.

关 键 词：金属络合衍生 高效液相色谱法 氰化氢 卷烟主流烟气 

分 类 号：O657.72[理学—分析化学] TS411[理学—化学]