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Determination of 17 beta-estradiol and its metabolites in sewage effluent by solid-phase extraction and gas chromatography/mass spectrometry.

Journal of AOAC International (1998-12-16)
H B Lee, T E Peart
ABSTRACT

The paper describes a simple and quantitative method for monitoring non-conjugated 17 beta-estradiol (E2) and its metabolites estrone (E1) and estriol (E3) as environmental contaminants in municipal sewage effluents. Estrogens were preconcentrated and cleaned up by solid-phase extraction using a reversed-phase C18 cartridge. They were derivatized with pentafluoropropionic acid anhydride, and the products were analyzed by gas chromatography/mass spectrometry. Recoveries from spiked distilled water and sewage were better than 87% at fortification levels of 100 and 20 ng/L. For a 1 L sewage sample and a concentration factor of 5000, detection limits were 5 ng/L for E1 and E2 and 10 ng/L for E3. In a brief survey of Canadian wastewater, these estrogens were detected in many raw sewage and effluent samples at concentrations ranging from 6 to 109 ng/L for E1, from < 5 to 15 ng/L for E2, and from < 10 to 250 ng/L for E3.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Pentafluoropropionic acid, 97%
Sigma-Aldrich
Sodium pentafluoropropionate, 98%
Sigma-Aldrich
Silver pentafluoropropionate, 98%

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