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Optimized determination of polybrominated diphenyl ethers by ultrasound‐assisted liquid–liquid extraction and high‐performance liquid chromatography
Authors:Kuang He  YuanCai Lv  YuanCai Chen
Affiliation:1. Ministry of Education Key Laboratory of Pollution Control and Ecological Remediation for Industrial Agglomeration Area, College of Environment and Energy, South China University of Technology, , Guangzhou, P. R. China;2. State Key Laboratory of Pulp and Paper Engineering, College of Light Industry and Food Science, South China University of Technology, , Guangzhou, P. R. China
Abstract:A method based on ultrasound‐assisted liquid–liquid extraction and high‐performance liquid chromatography has been optimized for the determination of six polybrominated diphenyl ether congeners. The optimal condition relevant to the extraction was first investigated, more than 98.7 ± 0.7% recovery was achieved with dichloromethane as extractant, 5 min extraction time, and three cycles of ultrasound‐assisted liquid–liquid extraction. Then multiple function was employed to optimize polybrominated diphenyl ether detection conditions with overall resolution and chromatography signal area as the responses. The condition chosen in this experiment was methanol/water 93:7 v/v, flow rate 0.80 mL/min, column temperature 30.0°C. The optimized technique revealed good linearity (R2 > 0.9962 over a concentration range of 1–100 μg/L) and repeatability (relative standard deviation < 6.3%). Furthermore, the detection limit (S/N = 3) of the method were ranged from 0.02 to 0.13 μg/L and the quantification limit (S/N = 10) ranged from 0.07 to 0.35 μg/L. Finally, the proposed method was applied to spiked samples and satisfactory results were achieved. These results indicate that ultrasound‐assisted liquid–liquid extraction coupled with high‐performance liquid chromatography was effective to identify and quantify the complex polybrominated diphenyl ethers in effluent samples.
Keywords:High‐performance liquid chromatography  Liquid–  liquid extraction  Polybrominated diphenyl ethers  Sonication
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