Phosphorylated metabolites are omnipresent in cells, but their analytical characterization faces several technical hurdles. Here, we detail an improved NMR workflow aimed at assigning the highresolution sub-spectrum of the phospho-metabolites in a complex mixture. Combining a pure absorption J-resolved spectrum (Pell & Keeler, J. Magn. Res. 2007) with alternate on-and offswitching of the 31 P coupling interaction during the t 1 evolution with a Pure-In Phase (PIP-) HSQMBC experiment (Castañar et al., Angew. Chemie 2014) without or with TOCSY transfer during the INEPT transfer gives access to selective identification of the individual subspectra of the phosphorylated metabolites. Returning to the initial J-res spectra, we can extract with optimal resolution the full trace for the individual phospho-metabolites, which then can be transposed on the high-resolution quantitative 1D.