Pressurised hot water extraction followed by headspace solid-phase microextraction and gas chromatography-tandem mass spectrometry for the determination of N-nitrosamines in sewage sludge

A method for the quantitative determination of the nine EPA N-nitrosamines in sewage sludge was developed by using pressurised hot water extraction (PHWE) followed by headspace solid-phase microextraction (HS-SPME) and gas chromatography coupled to chemical ionization ion trap tandem mass spectrometry (GC-Cl-MS-MS). The pressurised hot water extraction was optimized using a central composite design with regard to operational parameters such as temperature, extraction time and pH of water as extracting solvent. The optimum conditions were: water at pH 7.5 as extracting solvent, temperature of 125 degrees C and extraction time of 5 min. The sewage sludge extract was automatically analyzed by HS-SPME using a divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber and GC-Cl-MS-MS. The limits of detection of all compounds were lower than 0.15 mu g/kg of dry weight (d.w.) of sewage sludge. The repeatability and reproducibility between days (10 mu g/kg d.w.) expressed as relative standard deviation were lower than 16 and 19%, respectively. The method was applied to determine the N-nitrosamines in sewage sludge from urban and industrial sewage treatment plants (STPs) and from a potable water treatment plant. Some N-nitrosamines were determined in the samples and N-nitrosodiethylamine (NDEA) and N-nitrosodi-n-butylamine (NDBA) showed the highest values (371 and 305 mu g/kg (d.w.), respectively) in sewage from industrial STPs. (C) 2011 Elsevier B.V. All rights reserved.