微波-同时蒸馏萃取分离肉桂挥发性成分分析  

GC/MS DETERMINATION OF VOLATILE COMPONENTS IN CORTEX CINNAMOMI AFTER SEPARATION BY SIMULTANEOUS DISTILLATION AND EXTRACTION

作　　者：回瑞华[1] 侯冬岩[1] 朱永强[1] 刘晓媛[1] 

机构地区：[1]鞍山师范学院分析测试研究中心,鞍山114005

出　　处：《理化检验（化学分册）》2006年第2期105-108,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：辽宁省教育厅科学技术基金资助课题(20331079)

摘　　要：经粉碎的肉桂干燥树皮置于去离子水中微波加热处理后,用自制的同时蒸馏-萃取装置,以重蒸乙醚为溶剂将试样中的挥发组分萃取分离。用旋转蒸发器除去乙醚后即得到含有试样中挥发组分的透明的黄色液体,收得率为6.5%,应用GC/MS法对黄色液体的组分进行定性和定量分析。借助于联机的计算机和相关软件并用峰面积-归一化计算测得其中共有27个化合物,其中含量最高的是肉桂醛,达94.36%。另取部分上述挥发油(即黄色液体),用加成分解法将其中肉桂醛转化为一种加成产物以沉淀形式析出,即将黄色液体与NaHSO3共置于微波炉中,在不超过10℃的条件下处理直至加成物完全析出。将此加成物分出,并用0.1 mol.L-1盐酸进行水解处理,使加成物恢复成纯度较高的肉桂醛,用IR及MS对其组成及结构作进一步确认。Sample of bark of Cinnamomum cassia presl, was heated with deionized water in microwave oven and its volatile components were distilled and extracted simultaneously with redistilled ether in a special, self-made apparatus. After removing ether in the extract in a rotary evaporator, a transparent, yellow liquid with special fragrance was obtained, which contains the volatile components of the sample. The recovery was about 6.5%. GC/ MS was applied for the identification and quantitative determination of components in the yellow liquid, and by the help of hyphenated computer technique, and by calculation with the peak-area-normalization method 27 compounds were identified, in which the content of cinnamaldehyde amounted to 94. 36%. A separate portion of the volatile oil （i. e. the yellow liquid） was taken for a further separation of cinnamaldehyde by addition decomposition, that is to treat the volalite oil with NaHSO3 in a microwave oven, keeping the temperature not over 10 ℃, until the addition product of cinnamaldehyde was separated. Cinnamaldehyde was then recovered by hydrolysis of the addition product with 0. 1 mol·L^-1 HCl, and its composition and structure were analyzed and verified by IR and MS.

关 键 词：GC-MS 挥发组分 肉桂树皮 同时蒸馏-萃取 加成分解微波处理 肉桂醛 

分 类 号：O658.2[理学—分析化学] TQ244.1[理学—化学]