As the cell membranes are one of the targets of drug treatment in cancer cells, their membrane composition and variations in this composition need to be analyzed. Gradient selected 2D-NMR inverse heteronuclear chemical shift correlations are have described, which offer optimum sensitivity combined with a high reliability for unequivocal signal assignment in proton, carbon and phosphorous spectra, concerning neutral lipids and in particular phospholipids. Additionally, an extraction procedure is presented to extract subsequently the water soluble (PCA extract) and lipophilic metabolites (chloroform/methanol extract) from the same cell batch.