Since the beginning of high-resolution magic-angle spinning (HR-MAS) NMR spectroscopy in 1990s, we have witnessed tremendous instrumentation and methodological advancements in the HR-MAS NMR technique for semisolids. With HR-MAS, it is now possible to acquire reliable high-quality spectra in a routine and high-throughput fashion, and it has become a well-integrated metabolic screening tool for ex vivo biospecimens such as tissue biopsies, cells and organisms for NMR-based metabolomics research. This chapter provides the basic principles of HR-MAS and describes a few recent noteworthy developments that could strengthen the role of HR-MAS as a frontline NMR technique for metabolomics.