title: Monosaccharide compositional analysis of marine polysaccharides by hydrophilic interaction liquid chromatography-tandem mass spectrometry.
abstract: A simple and sensitive method was developed using hydrophilic interaction liquid chromatography coupled to tandem mass spectrometry for determination of monosaccharides liberated from marine polysaccharides by acidic hydrolysis. Optimal separation of diastereomeric monosaccharides including hexoses, pentoses, and deoxyhexoses was achieved using an aminopropyl bonded column with mobile phase containing ternary solvents (acetonitrile/methanol/water) in conjunction with MS/MS in SRM mode. Mechanisms for fragmentation of deprotonated monosaccharides with regard to cross-ring cleavage were proposed. Matrix effects from coeluting interferences were observed and isotopic-labeled internal standard was used to compensate for the signal suppression. The method demonstrated excellent instrumental limits of detection (LOD), ranging from 0.7 to 4.2 pg. Method LODs range from 0.9 to 5.1 nM. The proposed method was applied to the analysis of polysaccharides in seawater collected from the open leads of the central Arctic Ocean in the summer of 2008.
authors.affiliation: Department of Meteorology, Stockholm University, Sweden. gao@misu.su.se
authors.forename: Qiuju
authors.initials: Q
authors.lastname: Gao
authors.forename: Ulrika
authors.initials: U
authors.lastname: Nilsson
authors.forename: Leopold L
authors.initials: LL
authors.lastname: Ilag
authors.forename: Caroline
authors.initials: C
authors.lastname: Leck
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D006868:Hydrolysis; D057927:Hydrophobic and Hydrophilic Interactions; D015394:Molecular Structure; D009005:Monosaccharides / Q000032:analysis*; D011134:Polysaccharides / Q000737:chemistry*; D012623:Seawater / Q000032:analysis; D052616:Solid Phase Extraction; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D009005:Monosaccharides; D011134:Polysaccharides