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Acidic polysaccharides including glycosaminoglycans(GAGs) and non-GAGs containing uronic acid may be involved in biological processes.This study developed a glycomics method to analyze acidic polysaccharides by detecting the disaccharides from acid hydrolysates using HPLC-MS/MS upon 1-phenyl-3-methyl-5-pyrazolone(PMP) derivatization.