色谱

色谱

• 研究论文 • 上一篇    下一篇

L-羟脯氨酸寡肽混合物的高效液相色谱分离与质谱分析

孙艳亭1,卢奎1,马丽1,曹书霞2,赵玉芬2,3

  

  1. 1.School of Chemistry and Chemical Engineering, Henan University of Technology, Zhengzhou 450052, China;
    2.Key Laboratory for Chemical Biology, Department of Chemistry, Zhengzhou University, Zhengzhou
    450052, China; 3.Department of Chemistry, Xiamen University, Xiamen 361005, China
  • 收稿日期:2007-01-05 修回日期:2007-02-12 出版日期:2007-07-30 发布日期:1985-06-25
  • 通讯作者: 孙艳亭

Isolation and Identification of the Mixture of L-Hydroxyproline
Oligo-Peptides by Reversed-Phase High Performance
Liquid Chromatography and Electrospray
Ionization Tandem Mass Spectrometry

SUN Yanting1, LU Kui1, MA Li1, CAO Shuxia2, ZHAO Yufen2,3   

  1. 1.School of Chemistry and Chemical Engineering, Henan University of Technology, Zhengzhou 450052, China;
    2.Key Laboratory for Chemical Biology, Department of Chemistry, Zhengzhou University, Zhengzhou
    450052, China; 3.Department of Chemistry, Xiamen University, Xiamen 361005, China
  • Received:2007-01-05 Revised:2007-02-12 Online:2007-07-30 Published:1985-06-25

PDF

730

摘要：

研究了三氯氧磷辅助下L-羟脯氨酸的成肽反应,建立了采用反相高效液相色谱-质谱/质谱联用技术分离鉴定羟脯氨酸寡肽混合物的方法,优化了L-羟脯氨酸寡肽混合物的色谱分离条件。实验以YWG C8柱(10 μm,250 mm×10 mm)为分离柱,以乙腈-0.06%三氟乙酸水溶液(体积比为2∶98)为流动相进行等度洗脱,在正离子模式下对洗脱物进行了电喷雾电离串联质谱鉴定。结果显示,分离出的各组分分别为L-羟脯氨酸二肽、L-羟脯氨酸环二肽和L-羟脯氨酸三肽。

关键词: L-羟脯氨酸寡肽混合物 , 电喷雾串联质谱, 反相高效液相色谱

Abstract:

A reversed-phase high performance liquid chromatographic-electrospray ionization tandem mass spectrometric method （RP-HPLC/MS2） was developed for the analysis and identification of a reaction mixture of L-hydroxyproline oligo-peptides. The mixture was separated on a YWG C8 column (10 μm, 250 mm×10 mm) using acetonitrile-water containing 0.06% trifluoroacetic acid (2∶98, v/v) as the mobile phase. The separation conditions were optimized. The mixture was analysed with electrospray ionization mass spectrometry （ESI-MS） and ESI-MS/MS in positive mode. MS and MS2 spectra of individual chromatographic peak were obtained. It indicated that there were hydroxyproline dipeptide, hydroxyproline tripeptide and hydroxyproline cyclo-dipeptide in the mixtures, besides hydroxyproline. The described method can be effectively applied to perform identification of hydroxyproline oligo-peptide mixtures.

Key words: electrospray ionization tandem mass spectrometry （ESI-MS/MS）, L-hydroxyproline oligo-peptide mixture , reversed-phase high performance liquid chromatography （RP-HPLC）