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SPE-LC/ESI/MS: A simple and reproducible method for detection and quantification of 17ß-estradiol in aqueous samples.

Published by the American Society of Agricultural and Biological Engineers, St. Joseph, Michigan

Citation:  2010 Pittsburgh, Pennsylvania, June 20 - June 23, 2010  1009234.(doi:10.13031/2013.30043)
Authors:   Senorpe Asem-Hiablie, Clinton D Church, Isoken T Aighewi, Arthur L Allen, Paul Spock, Eric B May
Keywords:   17 ß-estradiol, solid phase extraction (SPE), LC/ESI/MS

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 17-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 100 ng/mL, 10 ng/mL and 1 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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