Analysis of Oligo-κ-carrageenan by Reversed Phase Ion-pair Ultra-Performance Liquid Chromatography Coupled with Electrospray Ionization-Time of Flight-Mass Spectrometry
- VernacularTitle:κ-卡拉胶寡糖的反相离子对-超高效液相色谱-四极杆-飞行时间质谱研究
- Author:
Yang GAO
;
Haimin CHEN
;
Lilin XU
;
Deying CHEN
;
Xiaojun YAN
- Publication Type:Journal Article
- Keywords:
κ-Carrageenan;
reversed phased ion-pair chromatography;
ultra performance liquid chromatography;
time of flight-mass spectrometry;
polyacrylamide gel electrophoresis
- From:
Chinese Journal of Analytical Chemistry
2009;37(11):1590-1595
- CountryChina
- Language:Chinese
-
Abstract:
A method was developed to elucidate the structures of sulfated oligosaccharides through establishment of an effective reversed phase ion pair ultra-performance liquid chromatography coupled with electrospray ionization time of flight mass spectrometry( RPIP-UPLC-ESI-TOF-MS). Heptylamine (20 mmol/L,pH4) has been selected as the ion-pairing agent.κ-Carrageenan oligosaccharides have been separated on BEH C_(18) column using MeOH/H_2O with 25% heptylammonium formate as eluent in linear gradient mode. Mass spectra were obtained by ESI-Q-TOF-MS in both positive and negative modes. κ-Carrageenan oligosaccharides were well separated up to pentatetrasaccharide,and ESIMS analysis for κ-carrageenan oligosaccharides up to hepta-cosasccharide. The results showed that all acid hydrolyzed κ-carrageenan oligosaccharides were odd sugars,which was further confirmed by polyacrylamide gel electrophoresis ( PAGE). The characteristic fragmentation pattern of ion-pair oligosaccharides in mass spectra can be applied for rapid structure identification.
