GC-TEA法测定卷烟主流烟气TSNAs前处理方法的改进

Improvement of pretreatment method for determination of TSNAs in mainstream cigarette smoke by GC-TEA

为改进气相色谱-热能分析联用法（GC-TEA）法测定卷烟主流烟气TSNAs的前处理方法,依托改良的索氏提取器将原方法中的提取、浓缩、柱层析净化、再浓缩四步有机结合,然后对卷烟主流烟气中的TSNAs进行测定。结果表明：1在10-4000 ng/m L的浓度范围内,4种TSNAs回归曲线的线性相关系数均大于0.999,该方法检测限在0.12-0.15 ng/cig之间,回收率在92.0%-102.3%之间,日内相对标准偏差在3.06%-5.80%之间,日间相对标准偏差在3.40%-6.93%之间;2将本方法与CORESTA N°63方法进行比较,两者结果无显著性差异。本方法采用改良的索氏提取器进行样品前处理可避免多次转移、浓缩,简化了操作步骤,缩短了前处理时间,有效减少分析误差,且有机溶剂用量大大减少,减少了对环境的污染,结果准确可靠,适用于主流烟气中TSNAs的分析检测。

In order to improve pretreatment method for the determination of TSNAs in mainstream cigarette smoke by GC-TEA,improved soxhlet extractor was used to pre-treat mainstream cigarette smoke samples which combined four steps of extraction, concentration, column chromatography pufi cation and re-concentration traditionally used. Results indicated that： 1） with concentration range of 10-4000 ng/m L, the linear correlation coeffi cients of four TSNAs regression curves were higher than 0.999. The limits of quantifi cation of this method ranged from 0.12 to 0.15 ng/cig, the recoveries were from 92.0% to 102.3%, the intra-day relative standard deviations（RSD） were between 3.06% and 5.80%, and the inter-day RSD were between 3.40% and 6.93%. 2） No signifi cant difference was detected compared with CORESTA N° 63 method. Repeated transferring and concentrating steps could be avoided. Therefore this method was suitable for the determination of TSNAs in mainstream cigarette smoke as it featured more accuracy and better reliability as well as simplifi ed operation steps, shorted pretreatment time, less organic solvents, reduced analysis errors.