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Headspace solid-phase microextraction with novel sol–gel permethylated-β-cyclodextrin/hydroxyl-termination silicone oil fiber for determination of polybrominated diphenyl ethers by gas chromatography–mass spectrometry in soil
Authors:Jingjing Zhou  Fangxing Yang  Dongmei Cha  Zhaorui Zeng  Ying Xu
Institution:

aDepartment of Chemistry, Wuhan University, Wuhan 430072, China

bState Key Laboratory of Freshwater Ecology and Biotechnology, Institute of Hydrobiology, Chinese Academy of Sciences, Wuhan 430072, China

cKey Laboratory for Analytical Chemistry of the State Ethnic Affairs Commission, College of Chemistry and Material Science, South-Central University for Nationalities, Wuhan 430074, China

Abstract:A simple, sensitive, and accurate method for determination of polybrominated diphenyl ethers (PBDEs) in soil has been developed based on headspace solid-phase microextraction (HS-SPME) followed by gas chromatography–mass spectrometry (GC–MS). Permethylated-β-cyclodextrin/hydroxyl-termination silicone oil (PM-β-CD/OH-TSO) fiber was first prepared by sol–gel technology and employed in SPME procedure. By exploiting the superiorities of sol–gel coating technique and the advantages of the high hydrophobic doughnut-shaped cavity of PM-β-CD, the novel fiber showed desirable operational stability and extraction ability. After optimization on extraction conditions like water addition, extraction temperature, extraction time, salts effect, and solvents addition, the method was validated in soil samples, achieving good linearity (r > 0.999), precision (R.S.D. < 10%), accuracy (recovery > 78%), and detection limits (S/N = 3) raging from 13.0 to 78.3 pg/g.
Keywords:Solid-phase microextraction  Polybrominated diphenyl ethers  β-Cyclodextrin  Soil
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