Development and validation of a HILIC-ELSD method for simultaneous analysis of non-substituted and acetylated
Jianghua Pu1, Xia Zhao1, Lin Xiao2
1Key Laboratory of Marine Drugs, Ministry of Education, School of Medicine and Pharmacy, Ocean University of China, Shandong Provincial Key laboratory of Glycoscience and Glycoengineering, Qingdao 266003, China; Laboratory for Marine Drugs and Bioproducts of Qingdao National Laboratory for Marine Science and Technology, Qingdao 266237, China.
Abstract:
A new HILIC-ELSD method was developed for compositional analysis of both xylo-oligosaccharides (XOS) with degree of polymerization (DP) from 2 to 8 and acetylated XOS with DP from 3 to 8. The method was carried out on a zwitterionic HILIC column using ELSD as a detector. The influences of mobile phase composition, column temperature and flow rate on the retention time and resolution of XOS were investigated. An excellent separation result was achieved with a linear gradient elution of 75%-50% acetonitrile in 30min, at a flow rate of 1mL/min and the column temperature at 35°C. In addition, LC-ESI-MS was employed to determine the structural information of X7, X8 and acetylated XOS. The proposed method was simple, reliable, and no derivatization procedure was needed. It is suitable for compositional analysis and quality control of XOS.
