Particle-beam liquid chromatography/mass spectrometry (PB-LC/MS) has been used for the determination of several classes of compounds that are not easily analysed using gas chromatography. The compounds studied were either of low volatility (isocyanate derivatives), thermally unstable (phenylurea herbicides) or highly polar (phenoxyacetic acid herbicides). PB-LC/MS was found to be suitable for the analysis of these compounds and gave library searchable electron impact mass spectra for a range of samples in various matrices (soil, vegetation, filter (air) and concentrate). An advantage of PB-LC/MS, compared with GC/MS, was that the extracts could be run immediately on the LC system (no pre or post work-up derivitization necessary). The post-column addition of alcohols and their effect on PB-LC/MS response was also investigated. An increase in response was found for the series, no additives < methanol < ethanol < propanol = butanol, but pentanol showed a decreased response compared with butanol.