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.
引用
收藏
页码:572 / 577
页数:6
相关论文
共 50 条
  • [31] Recognition of Membrane Sterols by Polyene Antifungals Amphotericin B and Natamycin, A 13C MAS NMR Study
    Ciesielski, Filip
    Griffin, David C.
    Loraine, Jessica
    Rittig, Michael
    Delves-Broughton, Joss
    Bonev, Boyan B.
    FRONTIERS IN CELL AND DEVELOPMENTAL BIOLOGY, 2016, 4
  • [32] 13C CP/MAS NMR studies of vitamin E model compounds
    Witkowski, S
    Paradowska, K
    Wawer, L
    MAGNETIC RESONANCE IN CHEMISTRY, 2004, 42 (10) : 863 - 869
  • [33] Cumene transformations over mordenite catalysts:: a 13C MAS NMR study
    Ivanova, II
    Montouillout, V
    Fernandez, C
    Marie, O
    Gilson, JP
    MICROPOROUS AND MESOPOROUS MATERIALS, 2003, 57 (03) : 297 - 308
  • [34] Jump in the structure of Type I kerogen revealed from pyrolysis and 13C DP MAS NMR
    Gao, Yuan
    Zou, Yan-Rong
    Liang, Tian
    Peng, Ping'an
    ORGANIC GEOCHEMISTRY, 2017, 112 : 105 - 118
  • [35] 13C CP MAS NMR of halogenated (Cl, Br, I) pharmaceuticals at ultrahigh magnetic fields
    Terskikh, Victor V.
    Lang, Stephen J.
    Gordon, Peter G.
    Enright, Gary D.
    Ripmeester, John A.
    MAGNETIC RESONANCE IN CHEMISTRY, 2009, 47 (05) : 398 - 406
  • [36] Polymorphic Characterization of Pharmaceutical Solids, Donepezil Hydrochloride, by 13C CP/MAS Solid-State Nuclear Magnetic Resonance Spectroscopy
    Park, Tae-Joon
    Ko, Dong-Hyun
    Kim, Young Ju
    Kim, Yongae
    BULLETIN OF THE KOREAN CHEMICAL SOCIETY, 2009, 30 (09): : 2007 - 2010
  • [37] CP MAS 13C NMR Spectroscopy in Determination of Species-Specific Differences in Wood Composition
    Kostryukov, S. G.
    Petrov, P. S.
    Masterova, Yu. Yu.
    Idris, T. D.
    Hamdamov, S. S.
    Yunusov, I. A.
    Kostryukov, N. S.
    RUSSIAN JOURNAL OF BIOORGANIC CHEMISTRY, 2022, 48 (07) : 1441 - 1447
  • [38] Application of Relaxation Dispersion of Hyperpolarized 13C Spins to Protein-Ligand Binding
    Qi, Chang
    Wang, Yunyi
    Hilty, Christian
    ANGEWANDTE CHEMIE-INTERNATIONAL EDITION, 2021, 60 (45) : 24018 - 24021
  • [39] Out-and-back 13C–13C scalar transfers in protein resonance assignment by proton-detected solid-state NMR under ultra-fast MAS
    Emeline Barbet-Massin
    Andrew J. Pell
    Kristaps Jaudzems
    W. Trent Franks
    Joren S. Retel
    Svetlana Kotelovica
    Inara Akopjana
    Kaspars Tars
    Lyndon Emsley
    Hartmut Oschkinat
    Anne Lesage
    Guido Pintacuda
    Journal of Biomolecular NMR, 2013, 56 : 379 - 386
  • [40] 1H, 13C and 31P MAS NMR studies of lyophilized brain tumors
    Marszalek, R.
    Pisklak, M.
    Horsztynski, D.
    Wawer, I.
    SOLID STATE NUCLEAR MAGNETIC RESONANCE, 2010, 37 (1-2) : 21 - 27