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Determination of Steroidal Estrogens in Flushed Dairy Manure Wastewater by Gas Chromatography-Mass Spectrometry

^a Soil and Water Science Department, P.O. Box 110510, University of Florida, Gainesville, FL 32611-0510
^b Analytical Toxicology Core Laboratory, P.O. Box 110885, University of Florida, Gainesville, FL 32611-0885

^* Corresponding author (travish{at}ufl.edu)

Received for publication July 22, 2005. There is a critical need to accurately measure the concentrations of natural steroidal estrogens in flushed dairy manure wastewater (FDMW) to assess any potential risk of waterway contamination resulting from land application. Estrogens are a concern because low concentrations (10-100 ng L^–1) in water can adversely affect aquatic vertebrate species such as fish, turtles, and frogs by disrupting the normal function of their endocrine systems. The objective of this study was to develop a sample preparation method that permits the quantification of four natural steroidal estrogens (17-estradiol, 17ß-estradiol, estrone, and estriol) in FDMW by gas chromatography-mass spectrometry (GC-MS). Solid-phase extraction with graphitized carbon black was used for the bulk extraction of estrogens from FDMW and additional sample purification was accomplished with C-18. The sample preparation method allowed estrogens to be detected accurately by GC-MS in FDMW. Spiked recovery experiments indicated that the method is satisfactory for measuring the estrogens of interest in FDMW with average recovery of >90%. As expected in FDMW, characterization of the estrogen profile revealed a large abundance of 17-estradiol relative to 17ß-estradiol and estrone. Estriol was not detected in FDMW. The methodology developed in this research helps provide an analytical foundation for the quantification of steroidal estrogens in FDMW by GC-MS.

Abbreviations: FDMW, flushed dairy manure wastewater • GC-MS, gas chromatography-mass spectrometry • SPE, solid-phase extraction