烟用三乙酸甘油酯含量测定标准方法的改进-烟草科技.PDF

烟草科技/ Tobacco Science Technology 烟草化学/ Tobacco Chemistry 2014 年第 12 期（总第329 期） 烟用三乙酸甘油酯含量测定标准方法的改进 边照阳，刘珊珊，范子彦，杨 飞，张洪非，李中皓，唐纲岭* 国家烟草质量监督检验中心，郑州高新技术产业开发区枫杨街2 号 450001 摘要：为提高烟用三乙酸甘油酯含量检测结果的稳定性，对标准YC 144—2008 中三乙酸甘油酯含量的气 相色谱（GC ）测定方法进行了改进，通过考察稀释溶剂、样品量、所用容器等因素的影响，建立了一种新的 三乙酸甘油酯含量测定的GC 方法，并采用该方法测定了61 个国内外烟用三乙酸甘油酯样品的纯度。结 果表明：①优化确定的实验条件为：10 μL 三乙酸甘油酯样品于2 mL 色谱瓶中，加入1 mL 丙酮，混合均匀 后进行GC 检测，峰面积归一化法定量。②方法的相对标准偏差（RSD ）小于0.009% ，且在48 h 内测定结果 无明显变化。③所测样品中三乙酸甘油酯的含量均≥99.0% ，有55 个样品的含量结果≥99.5% 。该方法 操作简便、有机溶剂用量少、结果稳定，适合于烟用三乙酸甘油酯样品的含量测定。 关键词：烟用三乙酸甘油酯；含量；气相色谱法 中图分类号：TS426 文献标识码：B 文章编号：1002-0861 （2014 ）12-0043-05 Improvement of Standard Method for Determining Purity of Triacetin for Cigarette BIAN Zhaoyang ，LIU Shanshan ，FAN Ziyan ，YANG Fei ，ZHANG Hongfei ，LI Zhonghao ，and TANG Gangling* China National Tobacco Quality Supervision Test Center, Zhengzhou 450001, China Abstract: To ensure the consistency of test result, the gas spectrometry (GC) method for determining the purity of triacetin for cigarette described in standard YC 144—2008 was revised. By investigating the effects of related factors, including dilution solvent, sample volume and container, on test results, a new method was developed, and the purity of 61 samples of domestic and imported triacetin for cigarette was determined with the developed method. The results showed that: 1) The optimized experimental procedure was that 10 μL triacetin was pipetted and transferred into a 2 mL sample vial before adding 1 mL acetone, the solution was thoroughly mixed and then determined by GC. The triacetin was quantified by peak area normalization method. 2) The relative standard deviations (RSD) of the method were less than 0.009%, and the test results did not obviously change within 48 hours. 3) The purity of all the samples wa