A method involving solid-phase extraction for pre-concentration of bisphenol A, octyl and nonyl phenol, estrogenic compounds, and selected pharmaceuticals from surface and wastewater samples was developed. This sample preparation method is compatible with the use of liquid chromatography-negative ion electrospray-tandem mass spectrometry (LC-ESI<sup>-</sup>-MS/MS) and provides simultaneous analysis of a wider group of target analytes in a complex sample matrix. Some of these target analytes are prone to stability problems in solvents such as methanol or reduced mass spectrometric sensitivity in the presence of additives. To avoid issues with reduced mass spectrometric sensitivity of target analytes, the sample preparation and mobile phase (and MS system) were selected to be free of additives such as formic acid or ammonium acetate. Solid phase extraction with octadecylsilane sorbent was used for sample preparation with acetonitrile used for the elution solvent to minimize issues with degradation of analytes. Just prior to LC-ESI<sup>-</sup>-MS/MS analysis the sample extracts were diluted 1:1 v/v with methanol to minimize loss of MS sensitivity while maintaining good analyte stability. Average recoveries for all the analytes were from 82.4 to 112 %. Matrix effects were determined in upstream and downstream surface water and in raw and treated wastewater from six wastewater treatment plants located in Saskatchewan. The detection limits for bisphenol A, octylphenol and nonylphenol were 1-2 ng/L and for diethylstilbestrol, 17-β-estradiol, estriol, estrone, 17-α-ethinylestradiol, prednisone, and prednisolone were 1-10 ng/L. Bisphenol A was detected in all raw wastewater samples with concentrations from133-645 ng/L. Estrone and 17-β estradiol were detected in 83% and 67% of the raw wastewater samples, respectively. The first detection of prednisone and prednisolone in wastewater in Canada are presented.

Analysis of bisphenol A, octyl and nonyl phenol, estrogens, and other selected pharmaceuticals in surface and wastewater by liquid chromatography-negative ion electrospray-tandem mass spectrometry

2019 Fall National Meeting

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