Determination of Polar Drug Residues in Sewage and Surface Water Applying Liquid Chromatography−Tandem Mass Spectrometry

Abstract

A simple and rapid method is presented for the trace-level analysis of 10 polar pharmaceutical residues in various types of water samples from the aquatic environment. Using this method, the pharmaceuticals and several drug metabolites can be analyzed in drinking and surface waters and in wastewater (treated and untreated sewage) at concentrations down to 0.01 microg/L. Samples are prepared by a simple in situ derivatization enabling the preconcentration of very polar metabolites by automated solid-phase extraction. The analytes were separated by liquid chromatography with tandem mass spectrometric detection and quantified by comparison with an internal standard. Limits of quantification were between 0.01 and 0.02 microg/L for three phenazone-type pharmaceuticals, six of their metabolites, and the antiepileptic drug carbamazepine. Except for dimethylaminophenazone, recoveries for all analytes were between 87 and 117% for raw and purified sewage, groundwater, and surface and drinking water. Investigations of some environmental samples revealed that sewage and surface water treatment causes a slight reduction of the concentrations of some analytes whereas other compounds were persistent during water treatment. Thus, some compounds were detected at the low-microgram per liter level in sewage effluents of wastewater treatment plants in Berlin (Germany) and were also found at high-nanogram per liter concentrations in Berlin surface water samples.

Analytical Methods for Polar Pollutants

“…They also showed that the composition of the eluent influences the signal response in ESI more strongly than in APCI and that adduct formation may be stronger in ESI. These latter two findings are in agreement with observations from real samples that the analyte response in APCI has been found to be less affected by coeluting matrix components than in ESI [202][203][204][205]. These are some arguments in favor of APCI.…”

Simultaneous determination of diphenylarsinic and phenylarsinic acids in amended soils by optimized solvent extraction coupled to HPLC–MS/MS

“…1, indicate that a very good liquid-phase separation efficiency was obtained. Additionally, since most studies have demonstrated that APCI is less matrix sensitive that ESI (Chen et al, 2014;Zuehlke et al, 2004), MS/MS parameters were also optimized for APCI. However, APCI was discarded for further determinations due to the lower instrumental response to both analytes and the narrow linear range especially for PAA (data not shown).…”

Quality assurance in immunoassay performance – carbamazepine immunoassay format evaluation and application on surface and waste water

“…CBZ also presents an interesting anthropogenic marker for the water cycle. The CBZ concentration in water samples can be determined by chromatographic methods such as liquid chromatographytandem mass spectrometry (LC-MS/MS) 12 or immunochemical methods. 13,14 Only recently a direct competitive enzyme immunoassay (EIA) using the enzyme horseradish peroxidase (HRP) and the chromogenic substrate 3,3 …”