Determination of Basic Antidepressants and Their N-Desmethyl Metabolites in Raw Sewage and Wastewater Using Solid-Phase Extraction and Liquid Chromatography−Tandem Mass Spectrometry

Abstract

A novel analytical method has been developed for the determination of six basic antidepressants (venlafaxine, sertraline, paroxetine, citalopram, amitriptyline, and fluoxetine) and four of their metabolites (O-desmethylvenlafaxine, desmethylsertraline, nortriptyline, and norfluoxetine) in raw sewage and roughly primary-treated wastewater. For analytical development purposes, two ion exchange solid-phase extraction cartridges were compared. Extracts were analyzed using liquid chromatography-tandem mass spectrometry (LC-MS/MS) with positive-mode electrospray (+ESI) and selected reaction monitoring transitions. The choice of a basic mobile phase significantly improved the instrumental sensitivity (by up to 14-fold for norfluoxetine) relative to common +ESI acidic mobile phases. In addition to the remarkable gain in sensitivity, negligible matrix effects were also observed in the raw sewage samples. Analyte recoveries ranged from 80 to 103% and effluent detection limits from 0.048 to 0.10 ng/L. Samples collected at the Montreal Wastewater Treatment Plant showed the unequivocal presence of all the target compounds at concentrations of 2-346 ng/L. The target antidepressants were also detected in samples taken from the effluent receiving waters (i.e., the St. Lawrence River) but at lower concentrations (0.41-69 ng/L). The highly sensitive proposed method constitutes one of the best means for monitoring the environmental occurrence of tricyclic antidepressants, selective serotonin reuptake inhibitors (SSRIs), and some of their metabolites.

Ecotoxicological aspects related to the presence of pharmaceuticals in the aquatic environment

“…This pharmaceutical was also detected in surface waters [23,188], groundwaters [28] and drinking water [32]. Other SSRIs, such as fluvoxamine, sertraline and paroxetine have also been detected in STP influents and effluents [186][187][188] as well as seawater (Nor-way) [187]. Antidepressants were detected at low concentrations (ng L −1 ) which may not represent isolated threats to non-target organisms when considering the respective contribution.…”

“…Fluoxetine is a typical example, being detected in STP influents at concentrations of 0.4-18.7 ng L −1 and in effluents in the lower range of 0.12-8.4 ng L −1 [186][187][188]. This pharmaceutical was also detected in surface waters [23,188], groundwaters [28] and drinking water [32].…”

“…Fluoxetine is a typical example, being detected in STP influents at concentrations of 0.4-18.7 ng L −1 and in effluents in the lower range of 0.12-8.4 ng L −1 [186][187][188]. This pharmaceutical was also detected in surface waters [23,188], groundwaters [28] and drinking water [32]. Other SSRIs, such as fluvoxamine, sertraline and paroxetine have also been detected in STP influents and effluents [186][187][188] as well as seawater (Nor-way) [187].…”

The derivatization and analysis of anticancer pharmaceuticals in the presence of tricyclic antidepressants by gas chromatography

“…There are some reports describing the negative impact of antiandrogen flutamide on the fish reproduction by disrupting the endocrine function and supressing reproductive behavior [8,9]. The presence of antidepressants in the STP effluents was already shown by Lajeunesse et al [10]. Also, they were detected in surface waters, as well as in the fish tissues [11].…”

Fluoxetine accumulation and metabolism as exposure biomarker to better understand biological effects in gastropods

“…1 Numerous studies have explored the sensitivity of invertebrates to waterborne fluoxetine showing marked differences of sensitivity. In a previous study, the New-Zealand mudsnail, Potamopyrgus antipodarum, and the European valve snail, Valvata piscinalis, were exposed to waterborne fluoxetine (3.7-100 µg/L) during 42 days.…”