Experimental design-based isotope-dilution SPME-GC/MS method development for the analysis of smoke flavouring products

For the implementation of Regulation (EC) No 2065/2003 related to smoke flavourings used or intended for use in or on foods a method based on solid-phase micro extraction (SPME) GC/MS was developed for the characterisation of liquid smoke products. A statistically based experimental design (DoE) was used for method optimisation. The best general conditions to quantitatively analyse the liquid smoke compounds were obtained with a polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibre, 60°C extraction temperature, 30 min extraction time, 250°C desorption temperature, 180 s desorption time, 15 s agitation time, and 250 rpm agitation speed. Under the optimised conditions, 119 wood pyrolysis products including furan/pyran derivatives, phenols, guaiacol, syringol, benzenediol, and their derivatives, cyclic ketones, and several other heterocyclic compounds were identified. The proposed method was repeatable (RSD%

为满足与食品中或拟用于食品的烟熏风味剂相关的（欧盟）委员会条例（EC）第2065/2003号的实施要求，本研究开发了一种基于固相微萃取（solid-phase micro extraction, SPME）-气相色谱-质谱联用（GC/MS）的方法，用于液体烟熏制品的表征。研究采用基于统计的实验设计（DoE）对该方法进行优化，最终确定了适用于液体烟熏成分定量分析的最优通用实验条件：采用聚二甲基硅氧烷/二乙烯基苯（PDMS/DVB）萃取纤维，萃取温度60℃，萃取时长30 min，解吸温度250℃，解吸时长180 s，搅拌时长15 s，搅拌转速250 rpm。在优化后的实验条件下，共鉴定出119种木材热解产物，涵盖呋喃/吡喃衍生物、酚类、愈创木酚、丁香酚、苯二酚及其衍生物、环酮类以及多种其他杂环化合物。所建立的方法具有良好的重复性（RSD%