¹³C SPE MAS measurement of ligand concentration in compressible chromatographic beads

A method for measuring the ligand concentration in heterogeneous materials like chromatography media is described. In this method, (13)C single pulse excitation magic angle spinning NMR experiment with broadband (1)H decoupling is used to determine the peak integrals for a butyl ligand in the spectrum of a dried chromatography medium. Within a carefully controlled protocol, those integrals compared with that of the internal reference compound dimethyl sulfone provide the required volume concentration with an accuracy of ca 2%. The effects of temperature, degree of hydration, and other experimental parameters are discussed.