Abstract The 1 H NMR analysis of species containing NMR‐active heteronuclei can be difficult due to signal overlap caused by the combined effects of homonuclear and heteronuclear scalar ( J ) couplings. Here, a general pure shift method is presented for obtaining ultra‐high resolution 1 H NMR spectra where spectral overlap is drastically reduced by suppressing both homonuclear and heteronuclear J ‐couplings, giving one single signal per 1 H chemical environment. Its usefulness is demonstrated in the analysis of fluorine‐ and phosphorus‐containing compounds of pharmaceutical and biochemical interest.