Multiwalled carbon nanotubes coated fibers for solid-phase microextraction of polybrominated diphenyl ethers in water and milk samples before gas chromatography with electron-capture detection

• Published in: Journal of Chromatography A 2006-12, Vol.1137 (1), p.8-14
• Main Authors: Wang, Jun-Xia, Jiang, Dong-Qing, Gu, Zhi-Yuan, Yan, Xiu-Ping
• Format: Article
• Language: English
• Subjects: Analysis methods; Analytical chemistry; Animals; Applied sciences; Biological and medical sciences; Carbon nanotubes; Cattle; Chemistry; Chromatographic methods and physical methods associated with chromatography; Chromatography, Gas - methods; electron capture detection; Exact sciences and technology; food analysis; food contamination; Food Contamination - analysis; Food industries; Fundamental and applied biological sciences. Psychology; Gas chromatographic methods; Gas chromatography; Hydrocarbons, Brominated - analysis; microextraction; Milk; Milk - chemistry; Milk and cheese industries. Ice creams; multiwalled carbon nanotubes coated fibers; Nanotubes, Carbon; Natural water pollution; Other wastewaters; Phenyl Ethers - analysis; Pollution; polybrominated biphenyls; Polybrominated diphenyl ethers; solid phase extraction; Solid Phase Microextraction - instrumentation; Solid Phase Microextraction - methods; Solid-phase microextraction; synthetic fibers; Wastewaters; Water; Water Pollutants, Chemical - analysis; Water treatment and pollution
• ISSN: 0021-9673
• DOI: 10.1016/j.chroma.2006.10.003

Determination of polybrominated diphenyl ethers (PBDEs) in environmental samples has raised great concerns due to the widespread use of PBDEs and their potential risk to humans. Solid-phase microextraction (SPME) is a fast, simple, cost-effective, and green sample preparation technique and is widely used for environmental analysis, but reports on the application of SPME for determination of PBDEs are very limited, and only a few publications dealing with commercial SPME fibers are available for extraction of PBDEs. Herein, we report a novel SPME method using multiwalled carbon nanotubes (MWCNTs) as the SPME fiber coating for gas chromatography with electron-capture detection (GC-ECD) of PBDEs in environmental samples. The MWCNTs coating gave much higher enhancement factors (616–1756) than poly (5% dibenzene–95% dimethylsiloxane) coating (139–384) and activated carbon coating (193–423). Thirty-minute extraction of 10 mL of sample solution using the MWCNTs coated fiber for GC-ECD determination yielded the limits of detection of 3.6–8.6 ng L −1 and exhibited good linearity of the calibration functions ( r 2 > 0.995). The precision (RSD%, n = 4) for peak area and retention time at the 500 ng L −1 level was 6.9–8.8% and 0.6–0.9%, respectively. The developed method was successfully applied for the analysis of real samples including local river water, wastewater, and milk samples. The recovery of the PBDEs at 500 ng L −1 spiked in these samples ranged from 90 to 119%. No PBDEs were detected in the river water and skimmed milk samples, whereas in the wastewater sample, 134–215 ng L −1 of PBDEs were found. The PBDEs were detected in all whole fat milk samples, ranging from 13 to 484 ng L −1. In a semiskimmed milk sample, only BDE-47 was found at 21 ng L −1.