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QUANTITATION OF ESTROGENS IN GROUND WATER AND SWINE LAGOON SAMPLE USING SOLID PHASE EXTRACTION, PENTAFLUROBENZYL/TRIMETHYLSILYL DERIVATIZATIONS AND GAS CHROMATOGRAPHY NEGATIVE ION CHEMICAL IONIZATION/MASS SPECTROMETRY/MASS SPECTROMETRY
Citation:
Fine, D., G. P. Breidenbach, T. L. Price, AND S R. Hutchins*. QUANTITATION OF ESTROGENS IN GROUND WATER AND SWINE LAGOON SAMPLE USING SOLID PHASE EXTRACTION, PENTAFLUROBENZYL/TRIMETHYLSILYL DERIVATIZATIONS AND GAS CHROMATOGRAPHY NEGATIVE ION CHEMICAL IONIZATION/MASS SPECTROMETRY/MASS SPECTROMETRY. Elsevier (ed.), JOURNAL OF CHROMATOGRAPHY A 1017:167-185, (2003).
Description:
A method was developed for the confirmed identification and quantitation of 17B-estradiol, estrone, 17B-ethynylestrodial and 16a-hydroxy-17B-estradiol (estriol) in ground water and swine lagoon samples. Centrifuged and filtered samples were extracted using solid phase extraction and extracts were derivatized using pentafluorobenzyl bromide and N-trimethylsilylimidazole. Analysis was done using negative ion chemical ionization (NICI) gas chromatography/mass spectrometry/mass spectrometry (GC/MS/MS). Deuterated analogs of each of the estrogens were used as isotope dilution standards and were added to the samples before extraction. A limit of quantitation of 1 ng/L in ground water was obtained using 500 mL of ground water sample, 1.0 mL of extract volume and the lowest calibration standard of 0.5 pg/ L. For a 25 mL swine lagoon sample, the limit of quantitation was 40 ng/L. The average recovery of the four estrogens spiked into 500 mL of distilled water and ground water samples (n+16) at 2 ng/L was 103% (s.d. 14%). For 25 mL of swine lagoon samples spiked at 500, 1000, and 10,000 ng/L, the average recovery for the four estrogens was 103% (s.d. 15%). The method detection limits of the four estrogens in a 500 mL sample volume ranged from 0.2 to 0.5 ng/L. In swine lagoon samples from three different types of swine operations, estrone was found at levels up to 25,000 ng/L, followed by estriol and estradiol up to levels at 10,000 ng/L and 3,000 ng/L, respectively. It was found that pretreatment of swine lagoon samples with formaldehyde was necessary to prevent conversion of estradiol to estrone.