Abstract
An effective and sensitive method is necessary for the determination of polybrominated diphenyl ethers (PBDEs) pollutants in water. In this study, effervescent-assisted dispersive liquid-liquid microextraction with solidification of the aqueous phase (EA-DLLME-SAP), followed by Gas Chromatography-Tandem Mass Spectrometry (GC-MS-MS) quantitative analysis, was established for the preconcentration and determination of PBDEs in real environmental water samples. 1,1,2,2-Tetrachloroethane was used as the extractant and directly dispersed into the water phase of the aqueous samples with the aid of a large number of carbon dioxide bubbles generated via the acid-base reaction of acetic acid and sodium bicarbonate, which did not require the use of a dispersant during the extraction process. The key factors affecting the extraction recovery were optimized, and an internal standard was used for quantitative analysis, which gave good linearity ranges of 1–100 ng·L−1 (BDEs 28, 47, 99, and 100), 2–200 ng·L−1 (BDEs 153, 154, and 183) and 5–500 ng·L−1 (BDE 209) with limits of quantification in the range of 1.0–5.0 ng·L−1. The accuracy was verified with relative standard deviations < 8.5% observed in tap, lake, river and reservoir water samples with relative recoveries ranging from 67.2 to 102.6%. The presented method contributes to the determination of PBDEs in environmental water samples.
Highlights
Polybrominated diphenyl ethers (PBDEs), which have 209 theoretical congeners, are widely used as flame retardants in furnishings, wood, paper and textiles, especially in electronic products, due to their low price and excellent fire resistance [1]
Dispersive liquid-liquid microextraction (DLLME), a ternary solvent system [19], is an innovation based on liquid phase microextraction (LPME), which exhibits high extraction efficiencies under the assistance of various auxiliary treatment steps, such as vortex, ultrasound, microwave and air [20,21,22,23]
A method combining effervescent-assisted dispersive liquid-liquid microextraction with the solidification of the aqueous phase (EA-DLLME-SAP) and Gas Chromatography-Mass Spectrometry (GC-MS)-MS analysis was developed to solve the problem of fast and effective dispersion of the extractant added to aqueous samples
Summary
Polybrominated diphenyl ethers (PBDEs), which have 209 theoretical congeners, are widely used as flame retardants in furnishings, wood, paper and textiles, especially in electronic products, due to their low price and excellent fire resistance [1]. Dispersive liquid-liquid microextraction (DLLME), a ternary solvent system [19], is an innovation based on LPME, which exhibits high extraction efficiencies under the assistance of various auxiliary treatment steps, such as vortex, ultrasound, microwave and air [20,21,22,23] These assistance technologies usually require the use of additional equipment or are labor-intensive. The combination of effervescent extraction, aqueous phase solidification and DLLME technologies enables the complete collection of the organic phase, thereby allowing the efficient and environmentally friendly analysis of PBDEs in aqueous samples. A method combining effervescent-assisted dispersive liquid-liquid microextraction with the solidification of the aqueous phase (EA-DLLME-SAP) and GC-MS-MS analysis was developed to solve the problem of fast and effective dispersion of the extractant added to aqueous samples. The performance of this method was compared with other technologies
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