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Environ Sci Technol. 2008 Jun 1;42(11):4068-75.

Optimization of a multiresidual method for the determination of waterborne emerging organic pollutants using solid-phase extraction and liquid chromatography/tandem mass spectrometry and isotope dilution mass spectrometry.

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Applied Chromatography Section, Laboratory Services Branch, Ontario Ministry of the Environment, 125 Resources Road, Etobiocke, Ontario, Canada M9P 3V6.


A high-throughput, liquid chromatography/tandem mass spectrometry (LC/MS-MS) method has been developed for the determination of 51 emerging organic pollutants (EOPs) in environmental waters. The method was validated for the analysis of 38 pharmaceutically active, 10 endocrine disrupting, and three perfluoroalkylated compounds. Method performance parameters, including sample preservatives, pH values used in the solid-phase extraction (SPE), sample storage, sample extract storage time, and matrix effects were discussed in detail for different aquatic matrices, including drinking water, wastewater, and surface water. Isotope-labeled compounds were used as injection internal standards (IIS) or isotope dilution quantitation standards (IDQS) to improve the data quality, investigate the behavior of matrix effects during SPE sample preparation and LC/MS-MS analysis, and to validate isotope dilution mass spectrometric (IDMS) determination of selected compounds. Method detection limits were determined to be in the low ng/L range forthe compounds evaluated. By application of this method to the analysis of effluents and samples downstream of a wastewater treatment plant, more than 35 target EOPs were quantified. We demonstrated method ruggedness by quality control and quality assurance (QC/QA) data, showed that matrix effects were dependent on modes of electrospray ionization, and could not be removed via SPE or cleanup procedures, exerting the same effect to target compounds in both raw and extracted samples. Both 13C- and 2H-labeled IDQS could be added to samples before sample extraction, and their recoveries used to correct matrix effects in LC/MS-MS EOP analyses.

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