期刊
JOURNAL OF CHROMATOGRAPHY A
卷 1366, 期 -, 页码 31-37出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2014.09.028
关键词
Organophosphorus flame retardants; Pressurized liquid extraction; Aqueous solutions; Solid-phase microextraction; Fish
资金
- National Science Foundation of China [21207061]
- National Natural Science Foundation of China [51278242]
- Doctoral Fund of Ministry of Education of China [20120091120017]
- China Postdoctoral Science Foundation [2013M541646]
- Environment Monitoring Fund of Jiangsu Province [1208, 1115]
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 1 g of fish meat with the solution of water:acetonitrile (90:10, v/v) at 150 degrees C for 5 min 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 (0.90-5000 ng g(-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 0.010-0.208 ng g(-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. (C) 2014 Elsevier B.V. All rights reserved.
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