NMR spectroscopy is a powerful tool for metabolomic studies, offering highly reproducible and quantitative analyses. This burgeoning field of NMR metabolomics has been greatly aided by the development of modern spectrometers and software, allowing high-throughput analysis with near real-time feedback. Whilst one-dimensional proton (1D-1H) NMR analysis is best described and remains most widely used, a plethora of alternative NMR techniques are now available that offer additional chemical and structural information and resolve many of the limitations of conventional 1D-1H NMR such as spectral overlay. In this book chapter, we review the principal concepts of practical NMR spectroscopy, from common sample preparation protocols to the benefits and theoretical concepts underpinning the commonly used pulse sequences. Finally, as a case study to highlight the utility of NMR as a method for metabolomic investigation, we have detailed how NMR has been used to gain valuable insight into the metabolism occurring in kidneys prior to transplantation and the potential implications of this.