Analytical Method Development and Validation for Some Persistent Organic Pollutants in Water and Sediments by Gas Chromatography Mass Spectrometry

Document Type : Original Research Paper


1 Veterinary Control Central Research Institute, Etlik, Turkey

2 Faculty of Veterinary Medicine, Ankara University, Turkey


Many of the persistent organic pollutants (POPs) with endocrine disrupting properties are monitored regularly by risk assessors with limited resources, where analytical procedures are usually laborious, expensive, and not ecofriendly. Moreover, these analyses were frequently advanced aiming one class of pollutants, consequently inefficient to correspond the demand of monitoring a quickly rising number of pollutants in the environment. The objective of this study was to develop a single sample extraction procedure and multiple gas chromatography-mass spectrometry runs for the detection of various groups of semi volatile organics; Polychlorinated Biphenyls (28, 52, 101, 118, 138, 153, 180), Polybrominated Diphenyl Ethers (17, 47, 66, 100, 153, 183) and Organochlorine Pesticides (α-HCH, HCB, γ-HCH, Heptachlor, p,p-DDD, p,p-DDE, p,p-DDT) in sediment and water samples simultaneously. Extraction for water involved solid phase extraction using C18 and for sediment using homemade column with florisil, primary secondary amine and magnesium sulfate with ultrasonication step by acetone. This procedure was validated and applied to water samples from tap, river and lake; and sediment samples from river and lake. For both matrices and all analytes, high linearity, recovery (88-106%) with all relative standart deviation values <20% and limit of quantification levels below the tested limits were achieved. This reliable and cost effective procedure for monitoring selected multiple POP levels in water and sediment; do not require complicated device nor intensive manual efforts, which would also minimize the depletion of the organic solvents, could be used for routine detection of selected POPs.