超高效液相色谱法测定卷烟烟气中游离态和质子化尼古丁含量

采用超高效液相色谱法(UPLC)建立了一种快速测定卷烟烟气中游离态和质子化尼古丁含量的反相离子对液相色谱法.首先对游离态和质子化的尼古丁的样品提取分离条件进行了研究,该方法的流动相为含有4mmol/L的庚烷磺酸钠盐作为离子对试剂的三氟乙酸缓冲水溶液(pH=3)与乙腈混合(体积比86∶14).线性范围为0.06～129μg/mL,相关系数是0.9999,回收率为87%～99.5%.检测下限为60ng/mL.采用该方法测定了26种商品卷烟的游离尼古丁和质子化尼古丁的含量.最后,根据所测样品卷烟中游离态烟碱的数据,并结合卷烟的实际评吸结果数据进行了方差分析和相关性分析.结果表明,游离态烟碱的含量与评吸的劲头指标具有特别显著的正相关性,与喉部刺激、鼻腔刺激、口腔刺激和干躁感4个评吸指标具有一定的负相关性,而与余味评吸指标没有相关性.

Fast determination of nicotine in both free-and protonated form in mainstream tobacco smoke by UPLC

A reversed phase ion-pair liquid chromatographic method was developed to determine nicotine which are in free-base form and protonated form in commercial cigarettes.The extraction conditions of free nicotine and protonated nicotine in trapped mainstream cigarette smoke were studied by using water and chloroform.Mobile phase was consisted of trifluoroacetic acid buffer (pH=3) and acetonitrile (86:14(V/V)) containing 0.004mol/Lsodium heptanesulfonate as an ion pair agent.The linearity was obtained in the range of 0.06—129μg/mL concentrations of nicotine.The correlation coefficient was 0.9999.The recoveries of nicotine were ranged from 87%—99.5%.The limit of detection was 60 ng/mL.The method was applied to some actual commercial cigarettes.Based on both the concentrations of nicotine in free-base form in the samples measured in this work and the smoking quality indicators of the samples, correlation analysis was discussed.