Analysis of estrogens in river water and effluents using solid-phase extraction and gas chromatography-negative chemical ionisation mass spectrometryof the pentafluorobenzoyl derivatives

A procedure was developed for the analysis of estrogens in environmental wa ter and effluents. Samples were extracted by passing through polymer-impreg nated solid-phase extraction discs or C-18 cartridges. followed by gas chro matography-negative chemical ionisation mass spectrometry of the pentafluor obenzoyl derivatives. The derivatives were stable and gave diagnostic negat ive molecular ions as the base peak for each of the major estrogens studied . The absolute recovery of estrogens spiked into clean groundwater using th e disc procedure was 84-116% at the 10 ng l(-1) level (calculation not base d on use of internal standards). Using doubly deuterated estradiol as inter nal standard added prior to extraction, the % relative standard deviation o f estrogen extraction and analysis in spiked groundwater at the 10 ng l(-1) level was 2.6-9.8%. Detection limits were 0.2 ng l(-1) or below for the ma jor estrogens, based on a 2.5 litre sample. The most abundant estrogen was estrone, with concentrations over the range 6.4-29 ng l(-1) in effluents, a nd 0.2 to 17 ng l(-1) in water from the River Thames, (C) 2001 Elsevier Sci ence B.V. All rights reserved.