食品科学 ›› 2020, Vol. 41 ›› Issue (8): 262-269.doi: 10.7506/spkx1002-6630-20190415-192

• 工艺技术 • 上一篇    下一篇

乙醇钾催化红花籽油乙酯制备共轭亚油酸乙酯及其产品结构表征

毕艳兰,张飞鸿,徐广维,刘伟,杨国龙   

  1. (河南工业大学粮油食品学院,河南 郑州 450001)
  • 出版日期:2020-04-25 发布日期:2020-04-20
  • 基金资助:
    国家自然科学基金面上项目(31671818)

Potassium Ethanolate-Catalyzed Preparation of Conjugated Linoleic Acid Ethyl Ester from Safflower Seed Oil Ethyl Ester and Its Structural Characterization

BI Yanlan, ZHANG Feihong, XU Guangwei, LIU Wei, YANG Guolong   

  1. (College of Food Science and Engineering, Henan University of Technology, Zhengzhou 450001, China)
  • Online:2020-04-25 Published:2020-04-20

摘要: 研究反应温度、反应时间以及乙醇钾添加量对乙醇钾催化红花籽油乙酯制备活性共轭亚油酸乙酯(conjugated linoleic acid ethyl ester,CLAEE)产品的纯度及得率的影响,并对CLAEE产品进行主要理化指标检测、脂肪酸组成分析以及结构表征。最终优化工艺条件为真空度-0.1 MPa、转速60 r/min、反应温度110 ℃、乙醇钾添加量5%(m/m)、反应时间3 h,在此工艺条件下可以制备出符合市场需要的CLAEE产品,其中活性CLAEE的相对含量为(75.44±1.18)%,双反式CLAEE的相对含量为(0.24±0.09)%,产品得率为(69.50±3.09)%,包括共轭亚油酸产品在内的总得率为90%。通过红外光谱、紫外光谱、气相色谱-质谱联用以及核磁共振对CLAEE产品的结构进行表征,验证其含有4 种同分异构体,分别为c9,t11-CLAEE、t10,c12-CLAEE、t9,t11-CLAEE和t10,t12-CLAEE,其中主要成分为活性CLAEE,即c9,t11-CLAEE及t10,c12-CLAEE。

关键词: 共轭亚油酸乙酯, 红花籽油乙酯, 乙醇钾, 结构表征

Abstract: In this paper, the effects of reaction temperature, reaction time and the amount of potassium ethanolate as catalyst on the purity and yield of conjugated linoleic acid ethyl ester (CLAEE) prepared from safflower seed oil ethyl ester were investigated. The main physicochemical indicators, fatty acid composition, and structure of CLAEE were determined. CLAEE meeting the market requirements was prepared under the following optimized conditions: reaction temperature 110 ℃, catalyst amount 5% (m/m), reaction time 3 h, vacuum degree ?0.1 MPa, and rotation speed 60 r/min. The content of active conjugated linoleic acid ethyl ester in the product was (75.44 ± 1.18)%, and the content of double trans conjugated linoleic acid ethyl ester was (0.24 ± 0.09)%. The yield of the product was (69.50 ± 3.09)%. The total yield of CLAEE and conjugated linoleic acid was 90%. The structure of the CLAEE product was characterized by infrared spectroscopy (IR), UV absorption spectroscopy, gas chromatography-mass spectrometry (GC-MS) and nuclear magnetic resonance (NMR). It was verified to contain four isomers, namely c9,t11-CLAEE, t10,c12-CLAEE, t9,t11-CLAEE and t10,t12-CLAEE, the main ones being active conjugated ethyl linoleate, namely c9,t11-CLAEE and t10,c12-CLAEE.

Key words: conjugated linoleic acid ethyl ester, safflower seed oil ethyl ester, potassium ethoxide, structural characterization

中图分类号: