An investigation was conducted on whether the fluorescence spectra of the very similar catecholamines adrenaline and noradrenaline could be separated using chemometric methods. The fluorescence landscapes (several excitation and emission spectra were measured) of two data sets with respectively 16 and 6 samples were measured, the smaller data set with higher resolution and i.e. precision. The samples were artificial urine (pH approximately equal to 3) spiked with the catecholamines in the concentration ranges 40--1200 nmol/L and 5.5--18 micromol/L, respectively. Unfold partial least squares regression (Unfold-PLSR) on the larger data set and parallel factor analysis (PARAFAC) of the six samples of the smaller set showed that there was no difference between the fluorescence landscapes of adrenaline and noradrenaline. It can be concluded that chemometric separation of adrenaline and noradrenaline is not obtainable using this type of fluorescence measurement. Raman scatter, which overlaps the catecholamine spectra, was shown not to have any influence on the models calculated.