中国科学技术大学学报 ›› 2016, Vol. 46 ›› Issue (10): 814-820.DOI: 10.3969/j.issn.0253-2778.2016.10.004

• 原创论文 • 上一篇    下一篇

滁菊精油的超临界流体萃取及全二维色谱分析

黄贵凤   

  1. 1.中国科学技术大学化学系,安徽合肥 230026; 2.安徽中烟工业有限责任公司技术中心,安徽省烟草化学重点实验室,安徽合肥 230088
  • 收稿日期:2016-04-11 修回日期:2016-05-17 出版日期:2016-10-31 发布日期:2016-10-31
  • 通讯作者: 杨俊
  • 作者简介:黄贵凤,女,1990年生,硕士. 研究方向:分离科学. E-mail:sa130190@mail.ustc.edu.cn
  • 基金资助:
    中国烟草总公司科技重大专项项目(110201301030CBR-051),安徽省烟草化学重点实验室开放基金(0920140421001)资助.

Analysis of essential oil of Dendranthema morifolium cv. Chuju by GC×GC-TOF/MS with supercritical CO2 extraction

HUANG Guifeng   

  1. 1.Department of Chemistry, University of Science and Technology of China, Hefei 230026, China; Anhui Key Laboratory of Tobacco Chemistry, Technology Center, China Tabacco Anhui Industrial Co., Ltd, Hefei 230088, China
  • Received:2016-04-11 Revised:2016-05-17 Online:2016-10-31 Published:2016-10-31

摘要: 以超临界CO2流体萃取(SFE)结合全二维气相色谱-飞行时间质谱(GC×GC-TOF/MS)分析,提取和鉴定滁菊精油的化学成分.采用正交试验设计考察SFE萃取压力、夹带剂添加量、萃取温度、萃取时间和CO2流量等因素对精油得率的影响.获得最佳萃取条件为萃取压力35 MPa,夹带剂添加量16%,温度55 ℃,时间3 h,CO2流量50 kg/h;得率为640%.通过比对色谱数据库的保留指数和TOF/MS的谱库检索,共鉴定出精油中的92种组分,其主要成分为萜类物质,占已鉴定化合物的6674%.此外,首次在菊属植物中初步检出3,4-二氢-β-紫罗兰酮、5,6-环氧化物-β-紫罗兰酮、3-羟基-5,6-环氧基-β-紫罗兰酮等3种重要的花香类物质.

关键词: 超临界流体萃取, 全二维气相色谱/飞行时间质谱, 滁菊, 精油成分

Abstract: The chemical compounds of essential oil from the flowers of Dendranthema morifolium cv. Chuju were studied by comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC×GC-TOF/MS) combined with supercritical carbon dioxide extraction (SFE). The effects of SFE different parameters including extraction pressure, co-solvent content, extraction time, extraction temperature and CO2 flow rate on the essential oil yield was investigated using orthogonal array design. The results indicate that the optimal extraction conditions are as follow: pressure 35 MPa, co-solvent content 16%, temperature 55 ℃, extraction time 3 h and CO2 flow rate 50 kg/h. Under the optimal extraction conditions, the essential oil yield is 640%. By searching TOF/MS spectral library and comparing the GC×GC retention indices with database values, 92 compounds are identified. The major constituents in the essential oil are terpenoids which make up 6674% of the identified volatile compounds. In addition, three important floral aroma components, 3,4-didehydro-β-ionone, β-Ionon-5,6-epoxide, 3-Hydroxy-5,6-epoxy-β-ionone are rudimentarily found in Dendranthema morifolium.

Key words: supercritical fluid extraction, comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry, Dendranthema morifolium cv. Chuju, essential oil