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United States Department of Agriculture

Agricultural Research Service

Title: Determination of Alkylphenol and Alkylphenolethoxylates in Biota by Liquid Chromatography with Detection by Tandem Mass Spectrometry and Fluorescence Spectroscopy

Authors
item Schmitz-Afonso, Isabelle - USDA/FAS
item Loyo-Rosales, Jorge - UNIV. OF MARYLAND
item Aviles, Maria DE La Paz - UNIV. OF MARYLAND
item Ratther, B. - USGS
item Rice, Clifford

Submitted to: Journal of Chromatography
Publication Type: Peer Reviewed Journal
Publication Acceptance Date: May 21, 2003
Publication Date: August 22, 2003
Citation: Schmitz-Afonso, I., Loyo-Rosales, J., Aviles, M., Ratther, B., Rice, C. 2003. Determination of alkylphenol and alkylphenolethoxylates in biota by liquid chromatography with detection by tandem mass spectrometry and fluorescence spectroscopy. Journal of Chromatography A. 1010:25-35.

Interpretive Summary: Quantitative methods for the determination of the non-ionic surfactants (octylphenol, nonylphenol and their corresponding ethoxylates (1 to 5)) in biota are needed.because the compounds may have endocrine activity while they are present in the internal tissues of these organisms. Extraction methods were developed for egg and fish utilizing a pressurized solvent extraction method (accelerated solvent extraction (ASE)). The solvent extracts from this device were passed through sorption cartridge materials composed of commercially-produced octadecylsilica or aminopropyl materials. Identification and quantification were accomplished by separating the compounds using liquid chromatography and followed by tandem mass spectrometry (LC/MS/MS). The results from this method were compared to another analytical system that is currently used but does not provide direct identification of the compounds. The LC/MS/MS provided high sensitivity and specificity required for these complex matrices and an accurate quantitation when appropriate internal standards were used. These methods were successfully applied to walleye and carp from the Great Lakes area and osprey eggs from Chesapeake Bay. Environmental scientists are beginning to use this technology in examining pollutant fate and transport. New strategies will be developed to minimize release of these compounds to the ecosystems.

Technical Abstract: This paper presents a quantitative method for the simultaneous determination of octylphenol, nonylphenol and the corresponding ethoxylates (1 to 5) in biota. Extraction methods were developed for egg and fish matrices based on accelerated solvent extraction (ASE) followed by a solid-phase extraction cleanup, using octadecylsilica or aminopropyl cartridges. Identification and quantification were accomplished by liquid chromatography-tandem mass spectrometry (LC/MS/MS) and compared to the traditional liquid-chromatography with fluorescence spectroscopy detection. LC/MS/MS provides high sensitivity and specificity required for these complex matrices and an accurate quantitation with the use of appropriate internal standards. Quantification limits by LC/MS/MS ranged from 4 to 12 ng/g in eggs, and from 6 to 22 ng/g in fish samples. These methods were successfully applied to walleye (Stizostedion vitreum) and carp (Cyprinus carpio) from the Great Lakes area and to osprey eggs from Chesapeake Bay. Total levels found in the fish samples were as high as 8.2 ug/g wet weight and up to 18 ng/g wet weight in osprey egg samples.

Last Modified: 11/27/2014