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Table 6 Nuclear magnetic resonance spectroscopy methods

From: Lipids detection and quantification in oleaginous microorganisms: an overview of the current state of the art

Method Microorganisms Sample preparation Compound detection and/or quantification Correlation with method Outcome Reference
TD-NMR Chlorella protothecoides Whole cells Quantitative Nile Red, lipid extraction/gravimetric Less restriction than Nile Red, which cannot determine lipid content < 38% [132]
1H NMR, 13C NMR, 2D 1H/13C NMR, liquid state Ulva rigida, Gracilaria longa, Fucus virsoides, Codium tomentosum Crude extracted lipids, Solvent extraction by Folch method Mono- and polyunsaturated fatty acids, carotenes and carotenoids, steroids, chlorophylls; Qualitative [120]
13C NMR Solid state Chlamydomonas reinhardtii, Pavlova lutheri, Nannochloropsis oculata Whole cells enriched with NaH13CO3 Lipids, saccharides; Quantitative Could not distinguish cell wall components with mobility [123]
1H LF-NMR C. protothecoides Whole cells, crude extracted lipids Quantitative glyceryl trioleate internal standard GC/MS Extremely sensitive, limits of quantification 1.18 g/L, < 2% RSD, limit of detection 0.32 g/L (algal broth) [130]
1H NMR, 1H HR-MAS, liquid state Chlorella, C. reinhardtii Whole cells TAGs; Quantitative, oleic TAG standard internal standard GC Biomonitoring [125]
1D, 2D 1H/13C solution state NMR C. reinhardtii, Chlorella vulgaris, Synechocystis 13C labeled whole cells Lipids, TAGs, among metabolites; Qualitative Metabolic profiles [124]
Liquid state 13C NMR, 31P NMR Neochloris oleoabundans Whole cells TAGs; Qualitative, glyceryl trioleate standard Interference from MAGs and DAGs, no contribution of phospholipids [122]
ERETIC 1H NMR Thalassiosira weissflogii, Cyclotella cryptica, Nannochloropsis salina Solvent-extracted lipids by Folch method Free fatty acids, TAGs, glycolipids, phospholipids; Quantitative Saturation degree, total lipid content, class distribution, profiling [133]
1H, 13C NMR, 1D, 2D C. vulgaris, Scenedesmus ecornis Extracted lipids Unsaturated and saturated fatty acid esters, TAG, free fatty acids, polar lipids, standard: TGO, soybean, Jatropha oil and Mixoil14; Quantitative GC/MS Lipid profiling and quantification of extracts [121]
1H, 13C NMR C. vulgaris, S. ecornis Solvent-extracted lipids by chloroform:methanol:water Neutral lipids (TAGs, free fatty acids), polar lipids (glyceroglycolipids, phospholipids) and unsaturation degree; Quantitative GC/MS Monitoring cultivations for biodiesel potential [39]
Dunaliella sp., Amphidinium carterae, Phaedodactylum tricorutum, Thalassiosira pseudonana Whole cells Lipids, saturated, unsaturated; Qualitative Profiling of whole cells [128]
1H NMR, 1H HR MAS Thalassiosira pseudonana Extracts and whole cells Important metabolites such as polyunsaturated fatty acids, eicosapentaenoic acid and docosahexaenoic Acid; Qualitative Lipid profiling [134]
1H NMR, 1H HR MAS, 13C-NMR Chaetoceros muelleri Extracted lipids and whole cells Important unsaturated fatty acids such as eicosapentaenoic and docosahexaenoic acids, phospholipids, and glycerols; Qualitative Lipid profiling [129]