4.3 Article

Dispersive Liquid-Liquid Microextraction Based on Solidification of Floating Organic Drop with High Performance Liquid Chromatography for Determination of Decabrominated Diphenyl Ether in Surficial Sediments

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CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
卷 38, 期 1, 页码 62-66

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ELSEVIER SCIENCE INC
DOI: 10.1016/S1872-2040(09)60016-5

关键词

Dispersive liquid-liquid microextraction; Solidification of floating organic drop; High performance liquid chromatography-ultraviolet detection; Sediment; Decabrominated diphenyl ether; Back propagation artificial neural network

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A method for the determination of decabrominated diphenyl ether(decaBDE) in sediment samples at trace level using dispersive liquid-liquid microextraction based on the solidification of floating organic drop (DLLME-SFO) and high performance liquid chromatography-ultraviolet detector(HPLC-UV) has developed. Based on the data of interactive orthogonal array design, the optimization experimental conditions were obtained with BP artificial neural network model : 1.00 mL, methanol as dispersive solvent, 35.0 mu L dodecanol as extractive solvent, 10.00% NaCl, pH 5, and extraction in 10 min. The extraction recovery (ER) was 62.22% at the extraction conditions. The proposed method exhibited a wide linear range (3.5 - 1400 ng/g) with R-2 = 0.9921. The limit of detection(LOD) and the limit of quantification(LOQ) of this method were 2.3 pg/g(S/N = 2) and 5.6 pg/g(S/N = 5), respectively. The recoveries of real samples at different spiking levels of decaBDE were 104.2%, 98.4% and 97.7%, respectively. Extraction, concentration and separation procedures for decaBDE from the sediment sample were carried out by one step, and hence, the process of DLLME-SFO for decaBDE was shortened.

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