Determination of Polybrominated Diphenyl Ethers in Riverine Sediments by Ultrasound-Assisted Microextraction (USAME), Reduced Scale Cleanup, and GC-MS

Background: PBDEs consist of synthetic chemicals frequently employed to help reducing or avoiding flame spread in a fire. As reactive flame retardants, they are covalently bound to the polymeric matrix of various domestic products. These compounds have drawn attention due to their large-scale production and use, and numerous papers have reported their presence as well as persistence in water, soil, sediment and atmospheric air, even in remote areas. The aim of this work was to develop a low cost and environmentally friendly analytical protocol to determine PBDEs in riverine sediment samples. Methods: First step consisted of optimizing instrumental parameters of GC-MS to improve the detectability of the target compounds. Then, factorial experiment designs at two levels, 23 and 24, were applied to evaluate the effects of these parameters on the GC-MS signal responses. The extraction of PBDE from the samples and the clean-up of the extracts were performed in order to ensure efficiency and low consumption of time, power and reagents. Results: GC-MS optimization allowed reduced running time associated with effective PBDE congeners separation and detection, when compared to the official proposed method. Recovery tests of extraction and clean-up steps presented satisfactory values when compared to the costly US EPA methodology. Conclusion: The results allow us to conclude that the proposed methodology is an efficient alternative for the determination of PBDEs from riverine sediments. Its advantage is related to the reduced consumption of time, power and reagents. Keywords: Flame retardants, PBDE, USAME, riverine sediment, GC-MS, polymeric matrix.