An analytical method using laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) was developed and applied to assess enrichment of B-containing p-boronophenylalanine-fructose (BPA-f) and its pharmacokinetic distribution in human tissues after application for boron neutron capture therapy (BNCT). High spatial resolution (50 μm) and limits of detection in the low parts-per-billion range were achieved using a Nd:YAG laser of 213 nm wavelength. External calibration by means of B-enriched standards based on whole blood proved to yield precise quantification results. Using this calibration method, quantification of B in cancerous and healthy tissue was carried out. Additionally, the distribution of B was investigated, providing B enrichment in the investigated tissues. Quantitative imaging of B by means of LA-ICP-MS was demonstrated as a new option to characterise the efficacy of boron compounds for BNCT.