A method was developed for analysis of low levels of natural (estradiol, estrone, estriol) and synthetic (ethynylestradiol) estrogens in ground water and swine waste lagoon effluent. The method includes solid phase extraction of the estrogens, preparation of pentafluorobenzyl derivatives of phenolic groups and trimethylsilyl derivatives of hydroxy groups, and analysis using negative ion chemical ionization gas chromatography/mass spectrometry/mass spectrometry. Deuterated estrogens are added to each sample prior to solid phase extraction to provide an isotope dilution method for correction of matrix effects. Method detection limits are approximately 0.4 ng/L in ground water and 8 ng/L in swine lagoon effluent. This method was used to evaluate the potential for ground water contamination by swine concentrated animal feeding operations (CAFOs) through either land application of swine effluent wastewater or leakage from storage lagoons. Several lagoons and monitoring wells from each of two facilities (a nursery and a farrowing sow operation) were sampled and analyzed for all four estrogens. For the nursery, lagoon effluent concentrations ranged from 390 to 620 ng/L for estrone, 180 to 220 ng/L for estriol, and 40 to 50 ng/L for estradiol. For the farrowing sow operation, digester and primary lagoon effluent concentrations ranged from 9,600 to 24,900 ng/L for estrone, 5,000 to 10,400 ng/L for estriol, and 2,200 to 3,000 ng/L for estradiol. Ethynylestradiol was not detected in any of the lagoon or ground water samples. Natural estrogen concentrations in ground water samples were generally less than 0.4 ng/L, although a few of wells at the nursery operation showed quantifiable but low levels. These data show that swine lagoons contain significant concentrations of natural environmental estrogens, but additional work is needed to better define analytical limits and develop storage and preservation techniques for improved sample quality assurance before an assessment of the potential for ground water contamination can be made.
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