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Journal Article

Accurate quantification of water-macromolecule exchange induced frequency shift: Effects of reference substance

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Leutritz, T., Hilfert, L., Smalla, K.-H., Speck, O., & Zhong, K. (2013). Accurate quantification of water-macromolecule exchange induced frequency shift: Effects of reference substance. Magnetic Resonance in Medicine, 69(1), 263-268. doi:10.1002/mrm.24223.

Cite as: https://hdl.handle.net/11858/00-001M-0000-002B-02D6-D
Water–macromolecule exchange induces a bulk water frequency shift contributing to the contrast in phase imaging. For separating the effects of the water–macromolecule exchange and the macromolecule susceptibility, appropriate internal or external references are needed. In this study, two internal reference compounds, 2,2,3,3-tetradeuterio-3-trimethylsilyl-propionate (TMSP) and 1,4-dioxane, were used to study the macromolecule-dependent water frequency shift in a bovine serum albumin (BSA)–water system in detail. For TMSP, the water–macromolecule exchange shift depended on both the BSA and the reference concentration and stabilized to a value of 0.025 ppm/mM (298 K, TMSP concentrations > 30 mM). For dioxane, the dependency of the water–macromolecule exchange shift on the BSA concentration is independent of dioxane at low concentrations. The resulting shift was smaller (0.009 ppm/mM) when compared with using higher TMSP concentrations as reference. This discrepancy might be due to additional dioxane–water interactions. Measurements with an external chloroform reference in a coaxial geometry showed a shift of −0.013 ppm/mM resulting from the opposing effects of macromolecules in water exchange-induced shift and diamagnetic susceptibility shift. All these effects should be considered in the interpretation of tissue phase contrast. From the experimental data, the equilibrium binding constant between BSA and TMSP has been quantified to be Kd = 1.3 ± 0.4, and the estimated number of interaction sites for BSA is 12.7 ± 2.6.