A method of ultrasound-dispersive liquid-liquid microextraction (US-DLLME) combined with high-performance liquid chromatography/variable wavelength detection (HPLC-VWD) has been developed for rapid measuring tetrabromobisphenol A and its five derivatives in water. Parameters affecting the extraction efficiency including the extraction solvents and dispersive solvents and their volume, ionic strength of the sample, and ultrasound time were optimized, and further validated by orthogonal array design (OAD). The optimized conditions provided enrichment factors for analytes of 74-490. Most analytes had linear responses between 2 and 500 μg L(-1), with correlation coefficients (r(2)) of 0.9923-0.9994. Limits of detection were 0.13-0.63 μg L(-1). Relative standard deviations (RSDs) for five replicates ranged from 2.6% to 4.5% for all analytes. When applied to spiked samples of real water, the method provided recoveries of 88.6-106.3% for tap water, 87.8-108.5% for Mi River water, 82.7-113.5% for chemical wastewater, 45.5-115.3% for urine, and 46.4-126.2% for fruit juice, with RSDs (n=5) less than 4%, 6%, 8%, 10%, and 9% respectively.
Keywords: Brominated flame retardants; Dispersive liquid–liquid microextraction; High-performance liquid chromatography; Ultrasound-assisted method.
© 2013 Published by Elsevier B.V.