The dataset includes raw data and processing files, together with mnova and pdf files of processed spectra for the 1H, 13C, and 31P NMR spectra recorded for the compounds synthesised for a paper on the assessment of mitochondrial lipid peroxidation in cells and zebrafish in vivo using a targeted mass spectrometry probe. The compounds were prepared by Dr Stuart T. Caldwell in the laboratory of Prof. Richard C. Hartley, University of Glasgow.  There are mnova and  pdf files of all processed NMR spectra compiled together. All raw NMR data and processing files are included in folders labelled with the compound names or numbers as they appear in the paper.  The 1H NMR data were acquired on Bruker AVIII 400 and AVIII 500 spectrometers and processed using Bruker Topspin software.