4.5 Article

Improved derivatization protocol for simultaneous determination of alkylphenol ethoxylates and brominated flame retardants followed by gas chromatography-mass spectrometry analyses

Journal

WATER SCIENCE AND TECHNOLOGY
Volume 69, Issue 12, Pages 2389-2396

Publisher

IWA PUBLISHING
DOI: 10.2166/wst.2014.144

Keywords

alkylphenol ethoxylates; brominated flame retardants; gas chromatography-mass spectrometry; heptafluorobutyric anhydride derivatization; simultaneous determination

Funding

  1. Rand Water
  2. Tshwane University of Technology

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An improved derivatization protocol for the simultaneous determination of alkylphenol ethoxylates and brominated flame retardants with heptafluorobutyric anhydride under triethylamine amine base was investigated. The derivatization reaction was completed in 30 min at 50 W C using hexane as solvent. Under these conditions, it was observed that alkylphenol ethoxylates and tetrabromobisphenol A were derivatized successfully in the presence of hexabromocyclododecane, lower congeners of polybrominated biphenyls and polybrominated diphenyl ethers. The improved protocol was applied to the recover of the analytes of interest from a simulated water sample after solid phase extraction. The recoveries achieved were above 60%. The limit of detection and limit of quantification ranged from 0.01-0.20 and 0.05-0.66 mu g L-1, respectively. The improved derivatization procedure was also successfully applied to determine trace amounts of these compounds in environmental water samples. The concentrations of the targeted analytes from the environmental samples were determined from limit of quantification. The levels of the targeted compounds in the environmental samples ranged from nd-7.63 +/-2.83 mu g L-1.

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