Analysis of Lipids in Crude Extracts by 13C Nuclear Magnetic Resonance

Phospho- and glycolipids with mono- or polyunsaturated fatty acid chains, free and acylated steroids, carotenes and carotenoids, chlorophylls, and related pheophytins were detected in crude extracts by NMR spectroscopy without any need for prior separation. A broad range of molecules belonging to different lipid classes could be identified in one-dimensional 13C NMR spectra obtained by applying a polarization transfer pulse sequence (DEPT 135°). Directly detected or 1H-detected two-dimensional heterocorrelated NMR experiments were performed to facilitate the assignment of peaks arising from carotenoids, unsaturated fatty acid chains, and chlorophylls. 13C NMR data of crude lipid extracts from the macroalgae Ulva rigida and Fucus virsoides are shown to yield an informative overview of their lipid content. NMR is thus proposed as a simple, nonselective, and nondestructive technique for the first screening of the main lipid classes in complex lipid mixtures.