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. Multidimensional, heteronuclear NMR relaxation methodsare used extensively to characterize the dynamics of biologicalmacromolecules. Acquisition of relaxation datasets on proteins typicallyrequires significant measurement time, often several days. Accordionspectroscopy offers a powerful means to shorten relaxation rate measurementsby encoding the “relaxation dimension” into the indirect evolution period inmultidimensional experiments. Time savings can also be achieved bynon-uniform sampling (NUS) of multidimensional NMR data, which is usedincreasingly to improve spectral resolution or increase sensitivity per unittime. However, NUS is not commonly implemented in relaxation experiments,because most reconstruction algorithms are inherently nonlinear, leading toproblems when estimating signal intensities, relaxation rate constants andtheir error bounds. We have previously shown how to avoid these shortcomingsby combining accordion spectroscopy with NUS, followed by datareconstruction using sparse exponential mode analysis, thereby achieving adramatic decrease in the total length of longitudinal relaxationexperiments. Here, we present the corresponding transverse relaxationexperiment, taking into account the special considerations required for itssuccessful implementation in the framework of the accordion-NUS approach.We attain the highest possible precision in the relaxation rate constants byoptimizing the NUS scheme with respect to the Cramér–Rao lower bound ofthe variance of the estimated parameter, given the total number of samplingpoints and the spectrum-specific signal characteristics. The resultingaccordion-NUS R1ρ relaxation experiment achieves comparableprecision in the parameter estimates compared to conventional CPMG (Carr–Purcell–Meiboom–Gill)R2 or spin-lock R1ρ experiments while saving an order ofmagnitude in experiment time.

magnetic resonance

Rapid measurement of heteronuclear transverse relaxation rates using non-uniformly sampled &amp;lt;i&amp;gt;R&amp;lt;/i&amp;gt;&amp;lt;sub&amp;gt;1&amp;lt;i&amp;gt;ρ&amp;lt;/i&amp;gt;&amp;lt;/sub&amp;gt; accordion experiments