液相色谱-电喷雾-四级杆-飞行时间质谱法分析琼胶寡糖

Analysis of Agaro-oligosaccharide by Liquid Chromatography Coupled with Electrospray Ionization-Quadrupole-Time of Flight-Mass Spectrometry

建立超高效液相色谱-电喷雾-四级杆-飞行时间质谱联用技术快速分离鉴定琼胶寡糖的方法。通过分析比较3种色谱柱(BEH Amide、BEH C8及Atlantis T3)对琼胶寡糖的分离结果发现,Amide色谱柱具有最佳优势,在无需样品衍生的状态下,可使聚合度介于3～29的琼胶寡糖得以良好分离,分析迅速,灵敏度高。而衍生后,则是采用Atlantis T3柱分离效果最佳,在紫外吸收色谱图上分离状态良好。色谱通过与电喷雾-四级杆-飞行时间质谱联用,能准确获得每个色谱信号对应的质谱结构信息,谱图清晰、简单,归属容易。

A method was developed to isolate and identify agaro-oligosaccharides by ultra performance liquid chromatography-electrospray ionization-quadrupole-time of flight mass spectrometry（UPLC-ESI-Q-TOF-MS）.In the experiment,three chromatographic columns（BEH Amide,BEH C8 and Atlantis T3） were used to isolate agaro-oligosacchrides.It was found that the BEH Amide had excellent isolation effect.Agarobiose oligomers with degree of polymerization（DP） ranging from 3 to 29 could be isolated rapidly and sensitively,and no derivatization procedure was needed.However,after derived with α-naphthylamine,agarobiose oligomers could be separated better by Atlantis T3 column,and a perfect AU spectrum was obtained.When combined liquid chromatography with ESI-Q-TOF-MS,accurate structure information of each chromatogram peak was obtained,the spectra were clear and the molecular weight of those oligosacchandes could be assigned easily.