title: Determination of organophosphorus flame retardants in fish by pressurized liquid extraction using aqueous solutions and solid-phase microextraction coupled with gas chromatography-flame photometric detector.
abstract: A novel method was developed for the determination of organophosphorus flame retardants (PFRs) in fish. The method consists of a combination of pressurized liquid extraction (PLE) using aqueous solutions and solid-phase microextraction (SPME), followed by gas chromatography-flame photometric detector (GC-FPD). The experimental parameters that influenced extraction efficiency were systematically evaluated. The optimal responses were observed by extracting 1g of fish meat with the solution of water:acetonitrile (90:10, v/v) at 150°C for 5min and acid-washed silica gel used as lipid sorbent. The obtained extract was then analyzed by SPME coupled with GC-FPD without any additional clean-up steps. Under the optimal conditions, the proposed procedure showed a wide linear range (0.90-5000ngg(-1)) obtained by analyzing the spiked fish samples with increasing concentrations of PFRs and correlation coefficient (R) ranged from 0.9900 to 0.9992. The detection limits (S/N=3) were in the range of 0.010-0.208ngg(-1) with standard deviations (RSDs) ranging from 2.0% to 9.0%. The intra-day and inter-day variations were less than 9.0% and 7.8%, respectively. The proposed method was successfully applied to the determination of PFRs in real fish samples with recoveries varying from 79.8% to 107.3%. The results demonstrate that the proposed method is highly effective for analyzing PFRs in fish samples.
authors.affiliation: State Key Laboratory of Pollution Control and Resource Reuse, School of the Environment, Nanjing University, Nanjing 210023, PR China; State Environmental Protection Key Laboratory of Monitoring and Analysis for Organic Pollutants in Surface Water, Nanjing 210036, PR China; Environment Monitoring Center of Jiangsu Province, Nanjing 210036, PR China. Electronic address: gaozhanqi2005@163.com.
authors.forename: Zhanqi
authors.initials: Z
authors.lastname: Gao
authors.affiliation: State Key Laboratory of Pollution Control and Resource Reuse, School of the Environment, Nanjing University, Nanjing 210023, PR China.
authors.forename: Yuehua
authors.initials: Y
authors.lastname: Deng
authors.affiliation: State Key Laboratory of Pollution Control and Resource Reuse, School of the Environment, Nanjing University, Nanjing 210023, PR China.
authors.forename: Wenting
authors.initials: W
authors.lastname: Yuan
authors.affiliation: State Key Laboratory of Pollution Control and Resource Reuse, School of the Environment, Nanjing University, Nanjing 210023, PR China. Electronic address: hhew@nju.edu.cn.
authors.forename: Huan
authors.initials: H
authors.lastname: He
authors.affiliation: State Key Laboratory of Pollution Control and Resource Reuse, School of the Environment, Nanjing University, Nanjing 210023, PR China.
authors.forename: Shaogui
authors.initials: S
authors.lastname: Yang
authors.affiliation: State Key Laboratory of Pollution Control and Resource Reuse, School of the Environment, Nanjing University, Nanjing 210023, PR China. Electronic address: envidean@nju.edu.cn.
authors.forename: Cheng
authors.initials: C
authors.lastname: Sun
mesh_terms: D000818:Animals; D002849:Chromatography, Gas; D004784:Environmental Monitoring / Q000379:methods*; D005399:Fishes; D005411:Flame Retardants / Q000032:analysis*; D057230:Limit of Detection; D018482:Muscle, Skeletal / Q000737:chemistry*; D010755:Organophosphates / Q000032:analysis; D010783:Photometry; D052617:Solid Phase Microextraction; D014867:Water / Q000737:chemistry; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D005411:Flame Retardants; D010755:Organophosphates; D014874:Water Pollutants, Chemical; D014867:Water
keywords: Aqueous solutions; Fish; Organophosphorus flame retardants; Pressurized liquid extraction; Solid-phase microextraction