The content of low-molecular-weight compounds in the red alga Gracilariopsis lemaneiformis [(Bory) Dawson, Acleto, et Foldvik] has been analysed in-situ using high-resolution magic angle spinning (HR-MAS) nuclear magnetic resonance (NMR) spectroscopy. The major heteroside was shown to be floridoside, but digeneaside and isofloridoside were also detected in the alga. Other major components were isethionic acid and the amino acids taurine and citrulline. The results from the HR-MAS NMR analysis were confirmed with high-resolution NMR spectroscopy, high-resolution fast atom bombardment mass spectrometry (FABMS) and GC-MS, on material isolated from the studied alga, but also on authentic samples.