The organic load of bulk water samples, collected from five industrially im
pacted estuaries, was extracted using solid-phase extraction. Where toxicit
y was demonstrated using a Tisbe battagliai bioassay, a toxicity directed f
ractionation scheme was applied to isolate causal compounds. To reduce the
complexity of the extracts toxicity profiles were obtained following solid-
phase fractionation and reverse-phase HPLC. Candidate toxic contaminants we
re identified by GC-MS. All procedures were evaluated with a series of refe
rence compounds of widely differing polarity. The method was successful in
identifying a number of compounds, which traditionally have not been select
ed for inclusion in monitoring programs, as the probable cause of detriment
al environmental effect. The results suggest that chlorinated phenols are a
major contributor to poor water quality in the lower reaches of the river
Tyne and alkylphenol surfactant metabolites in the river Tees. Other compou
nds, as yet unidentified, also contribute to poor water quality. It is sugg
ested that the identified compounds should now be surveyed more widely and
considered for inclusion in future monitoring programs.