This paper describes so me results obtained in an investigati on of urea-formaldehyde (UF) resins of different de grees of poly merisation by matrix-assisted la ser de sorption/ionisation tim e-of-flight (M ALDI-TOF) mass spectrometry (MS). MALDI-TOF MS prove d to be an ap propriate techniq ue for analy zing these ty pes of p olymers, bearin g in mind th at the result s of t he analysis correspond with prev ious phy sical a nd che mical measurements. This technique en ables a relatively swift deter mination of the degree of poly merrisation throug h the monitoring of key changes in the structu re of a poly mer. Thus, in the analysis of UF re sins, it may be possible to monitor a decrea se in the intensity of the monohydroxymethyl urea (MMU) si gnal, which corresponds t o an in crease of the mass spectra v alues i n the mass ra nge of hi gher homologues, above 1000 g mol -1 . A noticeabl e difference concerns the signal intensities in the higher mass ranges (up to 1400 g mol -1 ), which corresponds to more bra nched and longer ho mologues of th e poly mers. Especially , a sign ificantly more intensive signal of MMU wa s registered. The average molecular weight ( MW) of the exa mined sa mples was between 936 and 1324 g m ol -1 , with a maximal deviation of 20 %, depending on the ratios of the reactants.