title: Development of pressurized liquid extraction and solid-phase microextraction combined with gas chromatography and flame photometric detection for the determination of organophosphate esters in sediments.
abstract: Organophosphate esters have been extensively used as flame retardants and plasticizers. The analysis of organophosphate esters in the environment is a hot topic because many of them are toxic and persistent. We developed a novel procedure for determining organophosphate esters in sediment. In this work, pressurized liquid extraction and solid-phase microextraction are used for sample preparation to extract and concentrate the analytes, which are then analyzed by gas chromatography with flame photometric detection. The extraction parameters of pressurized liquid extraction were investigated and optimized by orthogonal design and then evaluated by range analysis and analysis of variance. Under the optimal conditions, the proposed procedure showed wide linear ranges (0.90-100 ng/g) with correlation coefficients ranging from 0.9921 to 0.9990. The detection limits of the method were in the range of 0.009-0.280 ng/g with standard deviations ranging from 2.2 to 9.5%. Recoveries of the proposed method ranged from 82.3 to 108.9% with relative standard deviations <8.4%. The obtained method was applied successfully to the determination of organophosphate esters in real sediments with recoveries varying from 79.8 to 107.3%. The proposed method was proved to be simple, easy, and sensitive for analyzing organophosphate esters in sediment samples.
authors.affiliation: State Key Laboratory of Pollution Control and Resource Reuse, School of the Environment, Nanjing University, Nanjing, P. R. China; Jiangsu Entry Exit Inspection and Quarantine Bureau, Nanjing, P. R. China.
authors.forename: Jianming
authors.initials: J
authors.lastname: Zheng
authors.forename: Zhanqi
authors.initials: Z
authors.lastname: Gao
authors.forename: Wenting
authors.initials: W
authors.lastname: Yuan
authors.forename: Huan
authors.initials: H
authors.lastname: He
authors.forename: Shaogui
authors.initials: S
authors.lastname: Yang
authors.forename: Cheng
authors.initials: C
authors.lastname: Sun
mesh_terms: D002849:Chromatography, Gas / Q000379:methods*; D004952:Esters / Q000032:analysis / Q000302:isolation & purification*; D019015:Geologic Sediments / Q000737:chemistry*; D059625:Liquid-Liquid Extraction / Q000379:methods*; D009943:Organophosphorus Compounds / Q000032:analysis / Q000302:isolation & purification*; D052617:Solid Phase Microextraction / Q000379:methods*
chemical_list: D004952:Esters; D009943:Organophosphorus Compounds
keywords: Organophosphate esters; Pressurized liquid extraction; Sediments; Solid-phase microextraction