Magnetic Resonance in Chemistry published by John Wiley & Sons Ltd. ¹³C single pulse excitation magic angle spinning NMR with broadband ¹H decoupling is introduced for measuring the ligand concentration in compressible chromatography media. Its performance is demonstrated for a butyl ligand in agarose resin. Obtaining volume concentration with an accuracy of ca 2% is demonstrated and the effects of temperature, degree of hydration, and other experimental parameters are discussed.

A method for measuring the ligand concentration in heterogeneous materials like chromatography media is described. In this method, ¹³C single pulse excitation magic angle spinning NMR experiment with broadband ¹H 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.