电子烟烟液中烟碱旋光异构体的手性液相色谱分离及测定  

Separation and determination method of nicotine enantiomers in e-cigarette solution based on chiral HPLC

作　　者：余晶晶[1] 蔡君兰[1] 王冰[1] 秦亚琼[1] 赵晓东[1] 刘克建[1] 薛聪 张晓兵[1] 刘绍锋[1] YU Jing-jing;CAI Jun-lan;WANG Bing;QIN Ya-qiong;ZHAO Xiao-dong;LIU Ke-jian;XUE Cong;ZHANG Xiao-bing;LIU Shao-feng(Key Laboratory of Tobacco Chemistry,Zhengzhou Tabacco Research Institute of CNTC,No.2 Fengyang Street,HighTech Zone,Zhengzhou China 450001)

机构地区：[1]中国烟草总公司郑州烟草研究院,烟草化学重点实验室,河南郑州450001

出　　处：《化学研究与应用》2018年第12期1948-1955,共8页Chemical Research and Application

基　　金：中国烟草总公司标准预研项目(2015QB008)资助.

摘　　要：建立了手性色谱柱-液相色谱-二极管阵列检测器(HPLC-DAD)法测定电子烟烟液中烟碱旋光异构体,即左旋烟碱(S-(-)-烟碱)和右旋烟碱(R-(+)-烟碱),对分析方法进行了优化和表征。结果表明:(1)最优的色谱条件为:采用大赛璐手性柱CHIRALPAK-IC,流动相为正己烷/异丙醇(体积比为95:5,含0. 1%二乙胺),流速1. 0 m L·min-1,等度洗脱。在优选条件下,电子烟烟液中左旋烟碱和右旋烟碱能实现基线分离,分析时间仅需18 min;(2)左旋烟碱和右旋烟碱分别在15～700μg·m L-1、0. 75～30μg·m L-1浓度范围内线性关系良好,二者检出限均为0. 02 mg·g-1。本方法左旋烟碱的日内、日间精密度分别为0. 73%、1. 67%,右旋烟碱的日内、日间精密度分别为4. 50%、8. 60%;二者回收率的结果在95. 50%～104. 5%之间;(3)选取不同口味、不同焦油量的电子烟烟液样品67个,对烟碱旋光异构体分别进行测定,结果表明电子烟烟液中主要为左旋烟碱,右旋烟碱检出率仅为12%,其含量占总烟碱的比例为0. 41%～4. 55%;(4)选取电子烟烟液样品20个,采用所建立的方法测定电子烟烟液和对应的电子烟气溶胶中左旋烟碱和右旋烟碱的含量,结果表明含有右旋烟碱的电子烟烟液所对应的电子烟气溶胶中未检出右旋烟碱。For the separation and analysis of nicotine enantiomers( i.e.S-(-)-nicotine and R-( +)-nicotine) in e-cigarette solution,a normal phase HPLC-DAD method coupled with a chiral column was developed in this work.The optimization and characterization of analytical method were performed.The results were as follow:(1)The optimized condition was as follows: CHIRALPAK-IC chiral column was chosen and the mobile phase was hexane/isopropanol with volume ratio of 95: 5 containing 0. 1%diethylamine,which the flow rate was 1. 0 m L·min-1 under isocratic elution.Under the optimized condition,the baseline separation of S-(-)-nicotine and R-( +)-nicotine was achieved within 18 min;(2)S-(-)-nicotine and R-( +)-nicotine showed linear calibration curves in the range of15 ~ 700 μg·m L-1 and 0. 75 ~ 30 μg·m L-1,respectively,with lower limit of detections( LODs) of 0. 02 mg·g-1.The intra-day and inter-day precisions of S-(-)-nicotine were less than 0. 73%and 1. 67%,respectively,which were less than 4. 50%and 8. 60%for R-( +)-nicotine.The recovery was in the range of 95. 50% ~104. 5%;(3) The contents of S-(-)-nicotine and R-( +)-nicotine for 67 ecigarette solution samples with different taste and tar amount were determined.E-cigarette solution contained mainly S-(-)-nicotine.Only 12%samples contained both S-(-)-nicotine and R-( +)-nicotine,and the ratio of R-( +)-nicotine in total nicotine was 0. 41%~ 4. 55%;(4) 20 e-cigarette solutions were chosen for the determined S-(-)-nicotine and R-( +)-nicotine in e-cigarette solution and corresponding e-cigarette aerosol.However,R-( +)-nicotine was not detected in e-cigarette aerosol,as the corresponding e-cigarette solution contained R-( +)-nicotine.

关 键 词：电子烟烟液 手性色谱柱 正相液相色谱 二极管阵列检测器 左旋烟碱 右旋烟碱 

分 类 号：O657.7[理学—分析化学]