色谱

色谱

• 研究论文 • 上一篇    下一篇

柱前衍生化-非水毛细管电泳法高效分离饮料中的脂肪醛

白新伟1, 王延宝1,3, 赵怀鑫1, 孙志伟2, 夏莲2, 付艳艳1, 索有瑞2, 李玉林2, 尤进茂1,2*   

  1. 1. 山东省生命有机分析重点实验室, 曲阜师范大学化学科学学院, 山东 曲阜 273165; 2. 中国科学院西北高原生物研究所, 青海 西宁 810001; 3. 济宁学院化学系, 山东 曲阜 273165
  • 收稿日期:2009-05-15 修回日期:2009-07-15 出版日期:2010-01-28 发布日期:1981-09-25
  • 通讯作者: 尤进茂

Separation of derivatized aliphatic aldehydes in beverage by nonaqueous capillary electrophoresis

BAI Xinwei1, WANG Yanbao1,3, ZHAO Huaixin1, SUN Zhiwei2, XIA Lian2, FU Yanyan1, SUO Yourui2, LI Yulin2, YOU Jinmao1,2*   

  1. 1. Key Laboratory of Life-Organic Analysis of Shandong Province, College of Chemistry Science, Qufu Normal University, Qufu 273165, China; 2. Northwest Plateau Institute of Biology, Chinese Academy of Sciences, Xining 810001, China; 3. Department of Chemistry, Jining University, Qufu 273165, China
  • Received:2009-05-15 Revised:2009-07-15 Online:2010-01-28 Published:1981-09-25
  • Contact: 尤进茂

PDF

593

被引次数

6

摘要： 以9,10-菲醌作为柱前衍生试剂,采用非水毛细管电泳模式考察并优化了脂肪醛的分离条件。实验采用毛细管(总长58.5 cm,有效长度50 cm,内径50 μm),应用80 mmol/L NH4Ac、1.4 mol/L HAc缓冲体系,于20 ℃、5 kPa(50 mbar)下压力进样 8 s,在不加入其他添加剂的情况下,实现了7种脂肪醛的高效基线分离,检出限为0.37～0.87 μmol/L,线性范围为0.78～25 μmol/L。应用所建立的方法对实际样品进行了测定,结果令人满意。

关键词: 9,10-菲醌, 非水毛细管电泳, 饮料 , 脂肪醛, 柱前衍生化

Abstract: A simple and mild method for the separation of aliphatic aldehydes based on a condensation reaction with 9,10-phenanthrenequinone as labeling reagent with nonaqueous capillary electrophoresis has been developed. The detection was performed with a diode array detector (DAD). A 58.5 cm (50 cm effective length)×50 μm i. d. untreated fused-silica capillary was used. To optimize the conditions, the background electrolyte concentration, column temperature, voltage and other factors were evaluated. The results indicated that the buffer concentration had a great impact on the separation, but the influences of temperature and added additives on the resolution were not obvious. The optimized conditions were as follows: 80 mmol/L ammonium acetate, 1.4 mol/L acetic acid, voltage of 28 kV, column temperature of 20 ℃ and DAD detection at 254 nm. The samples were introduced atmospherically with the injection at 5 kPa (50 mbar) for 8 s. The results indicate that seven aliphatic aldehyde derivatives and actual samples can be achieved baseline resolution under the proposed conditions.

Key words: 9,10-phenanthrenequinone, aliphatic aldehydes, beverage , pre-column derivatization, nonaqueous capillary electrophoresis