The use of copper(II) isonicotinate-based micro-solid-phase extraction for the analysis of polybrominated diphenyl ethers in soils

A micro-solid-phase extraction (mu-SPE) device was developed by filling copper(II) isonicotinate coordination polymer (Cu(4-C5H4N-COO)(2)(H2O)(4)) into a porous polypropylene envelope, and the mu-SPE, coupling with gas chromatography (GC) with a micro-cell electron capture detector (mu-ECD), was used for extraction and determination of PBDEs in soils. Variables affecting extraction procedures, including temperature, water volume, extraction time, and desorption time, were investigated in a spiked soil, and the parameters were optimized. Under the optimal experimental conditions, the method detection limits for seven PBDEs (BDE-28, 47, 99, 100, 153, 154, and 183) were in the range of 0.026-0.066 ng g(-1), and the reproducibility was satisfactory with the relative standard deviation in range of 1.3-10.1%. Good linear relationship between PBDEs concentrations and GC signals (defined as peak area) was obtained in the range between 0.1 and 200 ng g(-1). The recovery of the seven PBDEs by mu-SPE varied from 70 to 90%, which was comparable to that determined by accelerated solvent extraction method. Finally, the proposed method was used to determine PBDEs in several field-contaminated soils, and it was suggested that the mu-SPE is a promising alternative microextraction technique for the detection of PBDEs in soils. (C) 2012 Elsevier B.V. All rights reserved.