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13C SPE MAS measurement of ligand concentration in compressible chromatographic beads
被引:3
作者:
Elwinger, Fredrik
[1
,2
]
Dvinskikh, Sergey V.
[1
]
Furo, Istvan
[1
]
机构:
[1] KTH Royal Inst Technol, Div Appl Phys Chem, SE-10044 Stockholm, Sweden
[2] GE Healthcare Biosci AB, SE-75184 Uppsala, Sweden
基金:
瑞典研究理事会;
关键词:
NMR;
C-13;
solid-state NMR;
quantitative NMR;
agarose;
pore;
SOLID-STATE NMR;
NUCLEAR-MAGNETIC-RESONANCE;
ANGLE-SPINNING NMR;
HYDROPHOBIC INTERACTION CHROMATOGRAPHY;
SUPERCRITICAL CARBON-DIOXIDE;
MODEL ORGANIC-COMPOUNDS;
STATIONARY PHASES;
QUANTITATIVE-DETERMINATION;
CROSS-POLARIZATION;
LIQUID-CHROMATOGRAPHY;
D O I:
10.1002/mrc.4257
中图分类号:
O6 [化学];
学科分类号:
0703 ;
摘要:
A method for measuring the ligand concentration in heterogeneous materials like chromatography media is described. In this method, C-13 single pulse excitation magic angle spinning NMR experiment with broadband H-1 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. Copyright (C) 2015 The Authors. Magnetic Resonance in Chemistry published by John Wiley & Sons Ltd.
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页码:572 / 577
页数:6
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