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ARS Home Northeast Area University Park, Pennsylvania Pasture Systems & Watershed Management Research Research Publications at this Location





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Title:   Author  item
                                            ASEM-HIABLIE, SENORPE - Pennsylvania State Universityitem
                                            Church, Clintonitem
                                            ALLEN, ARTHUR - University Of Maryland Eastern Shore (UMES)item
                                            Spock, Paulitem
                                            MAY, ERIC - University Of Maryland Eastern Shore (UMES)
  Submitted to: Proceedings of the American Society of Agricultural and Biological Engineers International (ASABE)
                                    Publication Type: Proceedings
                                    Publication Acceptance Date: 5/20/2010
                                    Publication  Date: 6/20/2010
                                    Citation: Asem-Hiablie, S., Church, C., Aighewi, I. T., Allen, A.L., Spock, P.S., May, E.B. 2010. SPE-LC/ESI/MS: a simple and reproducible method for detection and quantification of 17beta-estradiol in aqueous samples. Proceedings of the American Society of Agricultural and Biological Engineers International (ASABE). Paper No. 1009234Interpretive Summary: An interpretive summary is not required.
                                Technical Abstract: Steroid estrogens contained in wastewater discharge from sewage treatment plants and agricultural run-off can alter endocrine function in exposed wildlife at part per trillion (ng/L) levels. Detection and quantification of estrogens in the environment at these levels pose numerous analytical challenges. This study aimed to develop a reproducible, accurate, and simple method for 17beta-estradiol (E2) quantification from environmental water samples. Extraction efficiencies of three solid phase extraction (SPE) cartridges; ENVI-Carb®, Oasis HLB Glass® and Oasis HLB Plus® were tested by trial extractions of 500 mL ultrapure water spiked to 1 ng/mL, 10 ng/mL and 100 ng/mL. The Oasis HLB Plus® cartridges yielded the best mean extraction efficiencies of 120.50 +/-  8.02 %; 113.23 +/-  9.77 % and 105.2 +/-  21.16 % for 1 ng/mL, 10 ng/mL and 100 ng/mL ultrapure water spikes respectively. Further tests of extractions efficiencies for field water samples showed reduced mean extraction efficiencies of 80.6 +/- 13.1 % for concentrations ranging from 40-15000 ng/L. This suggests the need for further clean-up of heavily loaded aqueous samples. Detection and quantification was by LC/MS using electrospray ionization (ESI) in negative ionization mode. Presence of precursor ion 271 (m/z) and product ion 183 (m/z) identified E2. A limit of quantification (LOQ) of 10 ng/L was established by finding the lowest point on the calibration curve whose signal-to-noise ratio was at least 3. Validation of the LOQ by analysis of 7 replicates of 40 ng/L field spikes by the SPE-LC/ESI/MS procedure yielded a mean recoveries of 81.98 +/- 8.5%.


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