Dataset Information

Analysis of Synthetic Monodisperse Polysaccharides by Wide Mass Range Ultrahigh-Resolution MALDI Mass Spectrometry.

ABSTRACT: Carbohydrates, such as oligo- and polysaccharides, are highly abundant biopolymers that are involved in numerous processes. The study of their structure and functions is commonly based on a material that is isolated from complex natural sources. However, a more precise analysis requires pure compounds with well-defined structures that can be obtained from chemical or enzymatic syntheses. Novel synthetic strategies have increased the accessibility of larger monodisperse polysaccharides, posing a challenge to the analytical methods used for their molecular characterization. Here, we present wide mass range ultrahigh-resolution matrix-assisted laser desorption/ionization (MALDI) Fourier transform ion cyclotron resonance (FT-ICR) mass spectrometry (MS) as a powerful platform for the analysis of synthetic oligo- and polysaccharides. Synthetic carbohydrates 16-, 64-, 100-, and 151-mers were mass analyzed and characterized by MALDI in-source decay FT-ICR MS. Detection of fragment ions generated from glycosidic bond cleavage (or cross-ring cleavage) provided information of the monosaccharide content and the linkage type, allowing for the corroboration of the carbohydrate compositions and structures.

SUBMITTER: Nicolardi S

PROVIDER: S-EPMC8034773 | biostudies-literature | 2021 Mar

REPOSITORIES: biostudies-literature

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Publications

Analysis of Synthetic Monodisperse Polysaccharides by Wide Mass Range Ultrahigh-Resolution MALDI Mass Spectrometry.

Nicolardi Simone S Joseph A Abragam AA Zhu Qian Q Shen Zhengnan Z Pardo-Vargas Alonso A Chiodo Fabrizio F Molinaro Antonio A Silipo Alba A van der Burgt Yuri E M YEM Yu Biao B Seeberger Peter H PH Wuhrer Manfred M

Analytical chemistry 20210305 10

Carbohydrates, such as oligo- and polysaccharides, are highly abundant biopolymers that are involved in numerous processes. The study of their structure and functions is commonly based on a material that is isolated from complex natural sources. However, a more precise analysis requires pure compounds with well-defined structures that can be obtained from chemical or enzymatic syntheses. Novel synthetic strategies have increased the accessibility of larger monodisperse polysaccharides, posing a ...[more]

PMID: 33667082

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Project description:Biofunctionalized gold nanoparticles (AuNPs) enable innovative translational research and development in biomedicine. Biomolecules such as peptides, proteins, lipids, and carbohydrates can be assembled onto AuNPs to yield nanomaterials with unique properties for applications in imaging, photothermal therapy, vaccination strategies, and drug delivery. The characterization of functionalized AuNPs still remains an analytical challenge that normally requires the combination of multiple techniques. Laser desorption/ionization (LDI) and matrix-assisted LDI (MALDI) have been applied successfully in combination with time-of-flight (TOF) mass spectrometry (MS) for the analysis of the surface chemistry of AuNPs functionalized with synthetic ligands, however only for ligands with a molecular mass limited to 1000 Da. TOF-MS-based approaches in addition exhibit limited performance in terms of mass resolution and MS/MS possibilities. To overcome these limitations, we designed an approach for the analysis of AuNPs based on ultrahigh resolution Fourier transform ion cyclotron resonance (FTICR) MS and a combination of LDI and MALDI. To illustrate the performance of the method, we present a comprehensive characterization of the surface chemistry of AuNPs conjugated via a thiol-ending linker to either the ovalbumin peptide (OVA 323-339), the Lewis X antigen (Galβ1-4[Fucα1-3]GlcNAcβ1) trisaccharide, the tetramannoside Manα1-2Manα1-2Manα1-3Manα1, or a mixture of both carbohydrates. Collision-induced dissociation (CID) was used to characterize the structure of pseudomolecular ions generated by LDI/MALDI in-depth. These included [M + H]+ and [M + Na]+, and importantly also [M + Au]+ and [M + 2Au-H]+ ions. This first observation of gold-containing pseudomolecular ions provides direct evidence for the Au-conjugation of ligands. In addition, we show the applicability of the method to monitor proteolytic cleavage of peptides that are conjugated to the AuNP surface. The presented LDI/MALDI-FTICR-MS and MS/MS approach will be applicable to the characterization of a wide range of functionalized AuNPs.

Dataset Information

Analysis of Synthetic Monodisperse Polysaccharides by Wide Mass Range Ultrahigh-Resolution MALDI Mass Spectrometry.

Publications

Analysis of Synthetic Monodisperse Polysaccharides by Wide Mass Range Ultrahigh-Resolution MALDI Mass Spectrometry.

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