Urbanized and industrialized communities have various anthropogenic activities and produce considerable amounts of municipal effluents, which are discharged along with a wide variety of pollutants to coastal waters. Municipal effluents are one of the major sources of pollutants for the estuaries and coastal waters. Among these contaminants, some can persist in natural waters and potentially have acute and chronic effects on aquatic organisms. Phthalate esters (PEs) which are o-, m- and p- derivatives of phthalic acid have a wide variety of industrial, agricultural and domestic applications, but by far the most important is their usage as plasticizers that improve the flexibility and workability of polymeric materials. Because of these properties, in the recent years, the production and usage of PEs have increased significantly. The PEs can migrate from the material to the environment. Since the rates of photolysis and chemical hydrolysis of phthalate esters are very slow, metabolic breakdown by microorganisms is considered to be one of the major routes for the environmental degradation of these widely spread pollutants in aquatic and terrestrial systems, such as sewage, soils, sediments, and surface waters. o-Phthalic acid esters have been found in the seawater, sediment, fish, atolla, shrimps and in algae, whereas p-phthalic acid dimethyl ester only in algae. The phthalates, especially di-(2-ethylhexyl) phthalate (DEHP) are toxic marine organism and considered as important pollutants of sea. Accordingly, for the phthalate esters analysis at trace levels in complex matrixes, such as water samples, developing fast and reliable analytical protocols are basically of significant importance for monitoring the phthalate ester-contaminated samples. The chemical fingerprinting of PEs was determined by gas chromatography combined with mass spectrometry (GC/MS) (at the SIM mode). Potential risks to aquatic organisms by four commercial phthalate esters, diethyl (DEP), di-n-butyl (DBP), butylbenzyl (BBP), and di(2-ethylhexyl)phthalate (DERP) were assessed using the measured and calculated concentrations inthe Golden Horn (Halic) surface waters. DEP, DBP, BBP and DEHP were present in all the dissolved water samples analyzed and dominated by DBP, DEHP. The total 4PEs concentrations, ranging, respectively from 17.7 to 59.1 mu g/L were measured in the dissolved phases.