This paper describes certain applications for endocrine-disrupting compounds determination. LC-MS was applied using an electrospray ionization (ESI) technique in positive mode for alcohol polyethoxylates and nonylphenol and octylphenol polyethoxylates (NPEOn and OPEOn), and in negative mode for 4-nonylphenol (4-NP) and 4-octylphenol (4-OP) to determine targeted compounds in wastewater and sludge. GC-MS and GC-MS-MS were used to determine 4-NP, 4-tert.-octylphenol (4-t-OP), bisphenol A, estradiol-17beta, estriol estrone, testosterone, 17alpha-ethynylestradioL cholesterol, coprostan-3-ol, coprostan and coprostan-3-one in both surface water and wastewater after derivatization with N,O-bis(trimethyl-silyl)trifluoroacetamide (BSTFA). Extraction from the water samples was by an SPE technique, using either a copolymeric (Oasis HLB) or C18 silica sorbents, depending on the target contaminants. Extraction from the sludge samples was by a Soxtec system using methanol. Percentage recoveries for most of the selected compounds, using either a copolymeric (Oasis HLB) or C18 silica sorbents, were satisfactory (>60%). Quantification limits for the target compounds were at ppb levels in both water and sludge samples when using LC-ESI-MS in both positive and negative modes. They reached ppt levels in water when using GC-MS (in large volume injection mode) and GC-MS-MS. The results revealed 4-NP, NPEOn and AEOs in sludge samples at a concentration range of 1.3-8.5 microg/g, and NPEOn, OPEOn and other compounds, such as coprostan and bisphenol A, in surface water and/or wastewater samples at concentrations ranging from the ppt to ppb levels.