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https://hdl.handle.net/2440/97734
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Type: | Journal article |
Title: | Butanolysis derivatization: improved sensitivity in LC-MS/MS quantitation of heparan sulfate in urine from mucopolysaccharidosis patients |
Author: | Trim, P. Hopwood, J. Snel, M. |
Citation: | Analytical Chemistry, 2015; 87(18):9243-9250 |
Publisher: | American Chemical Society |
Issue Date: | 2015 |
ISSN: | 0003-2700 1520-6882 |
Statement of Responsibility: | Paul J. Trim, John J. Hopwood, and Marten F. Snel |
Abstract: | Heparan sulfate (HS) is a complex oligosaccharide that is a marker of a number of diseases, most notably several of the mucopolysaccharidoses (MPS). It is a very heterogeneous compound and its quantification at physiological concentrations in patient samples is challenging. Here, we demonstrate novel derivatization chemistry for depolymerization/desulfation and alkylation of HS based on butanolysis. The resultant alkylated disaccharides are quantifiable by LC-MS/MS. This new method is at least 70-fold more sensitive than a previously published methanolysis method. Disaccharide yield over time is compared for methanolysis, ethanolysis, and butanolysis. Maximum disaccharide concentration was observed after 2 h with butanolysis and 18 h with ethanolysis whereas a maximum was not reached over the 24 h of the experiment with methanolysis. The sensitivity of the new technique is illustrated by the quantification of HS in 5 μL urine samples from MPS patients and healthy controls. HS was quantifiable in all samples including controls. Disaccharide reaction products were further characterized using exact mass MS/MS. |
Keywords: | Humans Mucopolysaccharidoses Butanols Methanol Heparitin Sulfate Urinalysis Chromatography, Liquid Adolescent Child Child, Preschool Infant Female Male Tandem Mass Spectrometry Young Adult Limit of Detection |
Rights: | © 2015 American Chemical Society |
DOI: | 10.1021/acs.analchem.5b01743 |
Published version: | http://dx.doi.org/10.1021/acs.analchem.5b01743 |
Appears in Collections: | Aurora harvest 3 Medicine publications |
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