糯米香净油的制备及其热裂解产物  

Preparation of absolute oil from Strobilanthes tonkinensis Lindau and its pyrolysis products

作　　者：徐秀娟[1] 薛云[2] 胡军[1] 白家峰[2] 马骥[1] 孙建生[2] 杨春强[1] 吴彦[2] XU Xiujuan;XUE Yun;HU Jun;BAI Jiafeng;MA Ji;SUN Jiansheng;YANG Chunqiang;WU Yan(Zhengzhou Tobacco Research Institute of CNTC,Zhengzhou 450001,China;Technology Center,China Tobacco Guangxi Industrial Co.,Ltd.,Nanning 530001,China)

机构地区：[1]中国烟草总公司郑州烟草研究院,郑州450001 [2]广西中烟工业有限责任公司技术中心,南宁市530001

出　　处：《烟草科技》2023年第10期70-81,共12页Tobacco Science & Technology

基　　金：国家烟草专卖局创新平台科研活动稳定支持专项“烟草类黑精分离评价及在不同烟草制品中的应用研究”(402021AWRC02);广西中烟工业有限责任公司对外合作项目“特色香料风格特征强化技术研究及应用”(2021450000340049)。

摘　　要：为研究糯米香净油的热裂解行为,采用超临界萃取-分子蒸馏技术制备了糯米香净油,通过GC-MS分析方法明确了不同蒸馏温度下各净油的化学组成,并利用热裂解-气相色谱-质谱联用仪对比分析糯米香净油不同裂解温度下裂解产物的差异。结果表明:①当蒸馏温度为100℃时,糯米香净油挥发性成分的总质量分数高达297.1 mg/g,是分离前的2.1倍。②亚油酸、十六酸、油酸、植醇、角鲨烯、1,2-二甲基-5-氧代-2-吡咯烷甲酸甲酯、2-哌啶甲酸乙酯、麦芽酚和芳樟醇等是糯米香净油的主要成分,而2-乙酰基-1,4,5,6-四氢吡啶和2,6-二乙基吡嗪等氮杂环化合物的质量分数较低,但香气活力值(OAV)值高达286.67(2,6-二乙基吡嗪,4#净油样品),对糯米香净油风味的贡献较大。③糯米香净油300℃的裂解产物以棕榈酸、亚油酸和亚麻酸等酸类成分为主,相对百分含量高达84.02%(5#净油样品);随裂解温度的升高,酸类成分相对百分含量逐渐降低至0,而苯系物和烯烃类化合物的相对百分含量逐渐升高。④2#净油样品的热裂解产物组成与其他样品差异较大,以醇类、氮杂环为主。900℃时,醇类、酮类和氮杂环类化合物的相对百分含量分别为17.05%、6.75%和22.79%,远高于其他样品,主要的裂解产物有芳樟醇、苯乙醇、2,4,4-三甲基-2-环己烯-1-醇、麦芽酚、紫罗兰酮、植酮和2-哌啶酮等。To study the pyrolysis behavior of absolute oil of Strobilanthes tonkinensis Lindau,the absolute oils were prepared by supercritical fluid extraction and molecular distillation methods.The chemical components in the absolute oils prepared at different distillation temperatures were determined by GC-MS analysis,and the differences in the pyrolysis products among the absolute oils of Strobilanthes tonkinensis Lindau prepared at different pyrolysis temperatures were compared and analyzed by pyrolysis-GC/MS.The results showed that:1)At 100℃,the total mass fraction of volatile components in the prepared absolute oil was as high as 297.1 mg/g,which was 2.1 times higher than that before separation.2)Linoleic acid,n-hexadecanoic acid,oleic acid,phytol,squalene,methyl 1,2-dimethyl-5-oxo-2-pyrrolidinecarboxylate,ethyl 2-piperidinecarboxylate,maltol and linalool were the main components in the absolute oil.The mass fractions of N-containing heterocyclic compounds were low,such as 2-acetyl-1,4,5,6-tetrahydropyridine and 2,6-diethylpyrazine,but their OAV values were as high as 286.67(for 2,6-diethylpyrazine in sample No.4#),so their contributions to the flavor of the absolute oil were greater.3)At 300℃,the pyrolysis products were mainly organic acids such as palmitic acid,linoleic acid and linolenic acid,and the total relative percentage was as high as 84.02%for sample No.5#.The content of organic acid gradually decreased to 0 with the increase of pyrolysis temperature,while the relative percentages of benzene homologues and olefins gradually increased.4)The pyrolysis products of sample No.2#were mainly alcohols and N-containing heterocycles,which were quite different from the other samples.At 900℃,the relative percentages of alcohols,ketones,and N-containing heterocyclic compounds were 17.05%,6.75%and 22.79%,respectively,which were much higher than those of the other samples.The main pyrolysis products were linalool,phenylethanol,2,4,4-trimethyl-2-cyclohexene-1-ol,maltol,ionone,phytoketone,2-piperidone,etc.

关 键 词：糯米香 净油 超临界萃取 分子蒸馏 致香成分 热裂解 

分 类 号：TQ657.4[化学工程—精细化工]