NMR line-fitting quantification of polysaccharide N-acylurea-based modification in glycoconjugates of Salmonella Typhi Vi polysaccharide

Raine Garrido; Jean Pierre Soubal; Leonid Torres; Ubel Ramírez; Vicente Vérez

doi:10.1002/mrc.4579

NMR line-fitting quantification of polysaccharide N-acylurea-based modification in glycoconjugates of Salmonella Typhi Vi polysaccharide

Magn Reson Chem. 2017 Aug;55(8):720-723. doi: 10.1002/mrc.4579. Epub 2017 Feb 5.

Authors

Raine Garrido¹, Jean Pierre Soubal¹, Leonid Torres¹, Ubel Ramírez¹, Vicente Vérez¹

Affiliation

¹ Finlay Institute of Vaccines, Ave 27, No. 19805, La Lisa 17100, Havana, Cuba.

PMID: 28087987
DOI: 10.1002/mrc.4579

Abstract

The polysaccharides modification via carbodiimide reaction is one of the most applied methods for obtaining conjugated vaccines against Salmonella enterica. However, N-acylurea carbodiimide adduct generated in the process is a critical impurity in carbohydrate-based vaccines. A quantitative NMR method was developed for assessing the N-acylurea carbodiimide adduct impurity. The procedure was based on line-fitting facilities for processing the NMR signals on complex spectra. The method showed good linearity, accuracy and precision under inter-operator variation (relative standard deviation <5%). Copyright © 2017 John Wiley & Sons, Ltd.

Keywords: NMR; Salmonella Typhi; line-fitting; quantitative analysis.

MeSH terms

Glycoconjugates / chemistry*
Humans
Magnetic Resonance Spectroscopy
Polysaccharides, Bacterial / chemistry*
Salmonella typhi / chemistry*
Urea / analogs & derivatives*
Urea / chemistry*
Vaccines, Conjugate

Substances

Glycoconjugates
Polysaccharides, Bacterial
Vaccines, Conjugate
Urea