Quantitative Fluorine NMR To Determine Carbohydrate Density on Glyconanomaterials Synthesized from Perfluorophenyl Azide-Functionalized Silica Nanoparticles by Click Reaction

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• 作者：Na Kong ; Juan Zhou ; JaeHyeung Park ; Sheng Xie ; Olof Ramstr枚m ; Mingdi Yan
• 刊名：Analytical Chemistry
• 出版年：2015
• 出版时间：September 15, 2015
• 年：2015
• 卷：87
• 期：18
• 页码：9451-9458
• 全文大小：452K
• ISSN：1520-6882

文摘

A quantitative fluorine NMR (¹⁹F qNMR) method was developed to determine the carbohydrate density on glyconanomaterials. Mannose (Man)- and galactose (Gal)-conjugated silica nanoparticles (SNPs) were synthesized from perfluorophenyl azide (PFPA)-functionalized SNPs and propargylated Man or Gal by copper-catalyzed azide鈥揳lkyne cycloaddition (click reaction). After treating PFPA-SNPs or Man-SNPs with hydrofluoric acid followed by lyophilization, the remaining residues were directly subjected to ¹⁹F NMR analysis. The density of PFPA on PFPA-SNP was determined to be 7.7 卤 0.2 脳 10^鈥?6 nmol/nm² and Man on Man-SNP to be 6.4 卤 0.2 脳 10^鈥?6 nmol/nm² giving a yield of 鈭?3% for the click coupling reaction. The apparent dissociation constant (K_d) of Man-SNPs with fluorescein isothiocyanate (FITC)-concanavalin A (Con A) was determined using a fluorescence competition assay to be 0.289 卤 0.003 渭M, which represents more than 3 orders of magnitude affinity increase compared to free Man with Con A.