High resolution 1 H nuclear magnetic resonance (NMR) spectra using spinning at the magic angle ( 1 H MAS NMR) have been obtained on approximately 80 mg samples of intact human kidney tissue obtained during surgery. This technique produces high resolution 1 H NMR spectra in which effects of dipolar couplings, chemical shift anisotropy and magnetic susceptibility differences are minimised, giving resolution comparable to solution state NMR spectroscopy. The combined use of one-dimensional single pulse and spin-echo spectra, and two-dimensional J-resolved and total correlation (TOCSY) spectra, allowed the assignment of a number of resonances of endogenous substances from both cytosolic and membrane compartments. These are the first reported results on human tissues using this technique and the approach offers potential for the identification and rapid quantitation of tissue components and determination of changes in disease states, thereby providing scope for diagnosis and therapy evaluation.