Solid phase extraction, QuEChERS cleanup, dansylation with LC-MS/MS detection as an improved method for analyzing five estrogens in wastewater

Author(s): Gunatilake, S.; Steelhammer, S.; Kwon, J.; Xia, K.; Armbrust, K.; Rodriguez, J.; Mlsna, T.

An improved method for the analysis of estriol (E3), estrone (E1), 17α-estradiol (αE2), 17Β-estradiol (ΒE2), and 17α-ethinylestradiol (EE2) in wastewater is described. The method includes sample preparation using solid-phase extraction followed by a "QuEChERS" (Quick Easy Cheap Effective Rugged Safe) cleanup, and a LC-MS-MS detection. Solid phase extraction was carried out using Oasis HLB cartridges and a dispersive solid phase cleanup pack containing MgSO4, PSA and C-18. The resulting extract was then derivatized with dansyl chloride. Separation was achieved on an Agilent Zorbex Extend C-18, Narrow Bore RR, (2.1 x 100mm, 3.5 µm) column and quantification was accomplished in the positive ion mode using multiple reaction monitoring. The cleanup method is quick, efficient, inexpensive, and requires only 200 ml of water. Reliable linearities were obtained for all the calibration curves (r2 > 0.995). Calculated matrix effects were less than 12% for all the analytes and hence, matrix matched calibration curves were not needed. The recoveries for the estrogens ranged from 81–103% with a high repeatability (n=3, RSD ≤ 9%) and low limits of quantification (0.6–0.9 ng/L). The method was used to analyze effluent and influent wastewaters in three Mississippi wastewater treatment plants but is broadly applicable for the determination of trace estrogens in any municipal wastewater samples.

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