色谱

色谱 ›› 2013, Vol. 31 ›› Issue (7): 679-683.DOI: 10.3724/SP.J.1123.2013.05021

• 特别策划:庆祝欧庆瑜先生八十华诞专栏 • 上一篇    下一篇

天然维生素E制品中杂质的分离与鉴定

谢云峰1,2, 杨悠悠1,2, 刘佳佳1,2, 武文华3, 杨永坛1,2   

  1. 1. 中粮营养健康研究院, 北京 100020;
    2. 北京市营养健康与食品安全重点实验室, 北京 100020;
    3. 中粮天科生物工程(天津)有限公司, 天津 300457
  • 收稿日期:2013-05-10 出版日期:2013-07-28 发布日期:2013-07-17
  • 通讯作者: 杨永坛
  • 基金资助:

    中粮集团公司资助项目(2013-C2-F001L).

Isolation and identification of impurities in the natural vitamin E

XIE Yunfeng1,2, YANG Youyou1,2, LIU Jiajia1,2, WU Wenhua3, YANG Yongtan1,2   

  1. 1. COFCO Nutrition and Health Research Institute, Beijing 100020, China;
    2. Beijing Key Laboratory of Nutrition Health and Food Safety, Beijing 100020, China;
    3. COFCO Tech Bioengineering (Tianjin) Co., Ltd., Tianjin 300457, China
  • Received:2013-05-10 Online:2013-07-28 Published:2013-07-17

PDF

284

被引次数

8

摘要：

利用高效液相色谱、气相色谱-质谱联用与高分辨质谱对天然维生素E制品中的杂质进行了分离分析与结构鉴定。采用正相高效液相色谱法分离天然维生素E的4种异构体及2种杂质,并对杂质馏分进行富集纯化。将气相色谱-质谱联用与高分辨质谱检测相结合,用于获得杂质的结构信息。通过比较杂质精确相对分子质量和解析质谱碎片离子,推断杂质为芝麻素及其同分异构体表芝麻素。经与芝麻素对照品保留时间及碎片离子数据比对,确证了对杂质结构的推断。所建立的杂质鉴定方法快捷、有效,可应用于天然维生素E制品的食品安全控制。

关键词: 高分辨质谱, 高效液相色谱, 结构鉴定, 气相色谱-质谱联用, 天然维生素E, 杂质

Abstract:

Two impurities in the natural vitamin E extracted from oil deodorizer distillate were separated and characterized by high-performance liquid chromatography (HPLC), gas chromatography-mass spectrometry (GC-MS) and Fourier transform ion cyclotron resonance mass spectrometry (FTICR-MS). The impurities were purified and collected by normal-phase HPLC. The accurate masses were determined using FTICR-MS and fragmentation behavior was studied by GC-MS. The results showed that the impurities had identical MS spectra and similar electron impact (EI) fragmentation patterns. Based on the spectra, the structures of the two impurities were proposed as the enantiomers of sesamin. The presented method is rapid and effective, and can be applied for the food safety to the vitamin E manufacturing industry.

Key words: gas chromatography-mass spectrometry (GC-MS), high performance liquid chromatography (HPLC), high resolution mass spectrometry, impurity, structure identification, vitamin E

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