title: ¹³C SPE MAS measurement of ligand concentration in compressible chromatographic beads.
abstract: 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.
authors.affiliation: KTH Royal Institute of Technology, Division of Applied Physical Chemistry, Teknikringen 36, SE-10044, Stockholm, Sweden.|GE Healthcare Bio-Sciences AB, Björkgatan 31, SE-75184, Uppsala, Sweden.
authors.forename: Fredrik
authors.initials: F
authors.lastname: Elwinger
authors.affiliation: KTH Royal Institute of Technology, Division of Applied Physical Chemistry, Teknikringen 36, SE-10044, Stockholm, Sweden.
authors.forename: Sergey V
authors.initials: SV
authors.lastname: Dvinskikh
authors.affiliation: KTH Royal Institute of Technology, Division of Applied Physical Chemistry, Teknikringen 36, SE-10044, Stockholm, Sweden.
authors.forename: István
authors.initials: I
authors.lastname: Furó
mesh_terms: D066241:Carbon-13 Magnetic Resonance Spectroscopy; D008024:Ligands; D015394:Molecular Structure; D009930:Organic Chemicals / Q000032:analysis*; D012685:Sepharose / Q000737:chemistry*
chemical_list: D008024:Ligands; D009930:Organic Chemicals; D012685:Sepharose
keywords: 13C; NMR; agarose; pore; quantitative NMR; solid-state NMR