Solid-phase extraction combined with dispersive liquid-liquid microextraction for the determination for polybrominated diphenyl ethers in different environmental matrices

摘要

An analytical method. solid-phase extraction combined with dispersive liquid-liquid microextration (SPE-DLLME). was established to determine polybrominated diphenyl ethers (PBDEs) in water and plant samples. After concentration and purification of the samples in LC-C18 column, 1.0-mL elution sample containing 22.0 mu L 1,1,2,2-tetrachloroethane was injected rapidly into the 5.0-mL pure water. After extraction and centrifuging, the sedimented phase was injected rapidly into gas chromatography with electron-capture detection (GC-ECD). For water samples, enrichment factors (EFs) are in the range of 6838-9405 under the optimum conditions. The calibration curves are linear in the range of 0.1-100 ngL(-1) (BDEs 28, 47) and 0.5-500 ng L-1 (BDEs 100, 99,85,154,153). The relative standard deviations (RSDs) and the limits of detection (LODs) are in the range of 4.2-7.9% (n = 5) and 0.03-0.15 ng L-1, respectively. For plant samples, RSDs and LODs are in the range of 5.9-11.3% and 0.04-0.16 mu g kg(-1), respectively. The relative recoveries of well, river, sea. leachate, and clover samples, spiked with different levels of PBDEs, are 66.8-94.1%, 72.2-100.5%, 74.5-110.4%, 62.1-105.1%, 66.1-91.7%, 62.4-88.9%, and 64.5-83.2%, respectively. The results show that SPE-DLLME is a Suitable method for the determination of PBDEs in water and plant samples.