title: Dispersive liquid-liquid microextraction followed by reversed phase-high performance liquid chromatography for the determination of polybrominated diphenyl ethers at trace levels in landfill leachate and environmental water samples.
abstract: A simple, rapid and efficient method, dispersive liquid-liquid microextraction (DLLME), has been developed for the extraction and preconcentration of polybrominated diphenyl ethers (PBDEs) in water samples. The factors influencing microextraction efficiencies, such as the kind and volume of extraction and dispersive solvent, the extraction time and the salt effect, were optimized. Under the optimum conditions (sample volume: 5 mL; extraction solvent: tetrachloroethane, 20.0 microL; dispersive solvent: acetonitrile, 1.00 mL; extraction time: below 5s and without salt addition), the enrichment factors and extraction recoveries were high and ranged from 268 to 305 and 87.0 to 119.1%, respectively. Linearity was observed in the range 0.05-50 ng mL(-1) for BDE-28 and BDE-99, and 0.1-100 ng mL(-1) for BDE-47 and BDE-209, respectively. Coefficients of correlation (r(2)) ranged from 0.9995 to 0.9999. The repeatability study was carried out by extracting the spiked water samples at concentration levels of 50 ng mL(-1) for BDE-28 and BDE-99, and 100 ng mL(-1) for BDE-47 and BDE-209, respectively. The relative standard deviations (R.S.D.s) varied between 3.8 and 6.3% (n=5). The limits of detection (LODs), based on signal-to-noise ratio (S/N) of 3, ranged from 12.4 to 55.6 pg mL(-1) (the wavelength of detector at 226 nm). The relative recoveries of PBDEs from tap, lake water and landfill leachate samples at spiking levels of 5, 10 and 50 ng mL(-1) were in the range of 89.7-107.6%, 114.3-119.1% and 87.0-90.9%, respectively. As a result, this method can be successfully applied for the determination of PBDEs in landfill leachate and environmental water samples.
authors.affiliation: School of Environmental Science and Public Health, Wenzhou Medical College, Wenzhou 325035, China.
authors.forename: Yanyan
authors.initials: Y
authors.lastname: Li
authors.forename: Guohui
authors.initials: G
authors.lastname: Wei
authors.forename: Jia
authors.initials: J
authors.lastname: Hu
authors.forename: Xiujuan
authors.initials: X
authors.lastname: Liu
authors.forename: Xinna
authors.initials: X
authors.lastname: Zhao
authors.forename: Xuedong
authors.initials: X
authors.lastname: Wang
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation / Q000379:methods*; D004784:Environmental Monitoring / Q000379:methods; D004987:Ethers / Q000032:analysis*; D044367:Phase Transition; D011075:Polybrominated Biphenyls / Q000032:analysis*; D012680:Sensitivity and Specificity; D012965:Sodium Chloride / Q000737:chemistry; D012995:Solubility; D012997:Solvents / Q000737:chemistry; D013997:Time Factors; D014131:Trace Elements / Q000032:analysis*; D014865:Waste Disposal, Fluid; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D004987:Ethers; D011075:Polybrominated Biphenyls; D012997:Solvents; D014131:Trace Elements; D014874:Water Pollutants, Chemical; D012965:Sodium Chloride