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Journal ArticleDOI

Rapid direct injection LC-MS/MS method for analysis of prioritized indicator compounds in wastewater effluent

04 Sep 2015-Vol. 1, Iss: 5, pp 632-643
TL;DR: In this paper, the authors used a detailed literature review and scoring system to establish a list of twenty priority indicator trace organic compounds (TOrCs) in US wastewaters.
Abstract: Trace organic compounds (TOrCs) have been detected in drinking water sources for several years, raising concerns due to their potential risks to public health. The main contributor of TOrCs to drinking water is through wastewater discharges. However, there are several hundred TOrCs currently known with numerous new organic chemicals being released daily, making it unfeasible to monitor each one in water. This study used a detailed literature review and scoring system to establish a list of twenty priority indicator TOrCs in US wastewaters. Next, a rapid direct injection LC-MS/MS method for analysis of these compounds was developed without the need for an extraction step and only 80 μL sample volume while providing method reporting limits of 3–39 ng L−1 for all but one TOrC (sucralose: 302 ng L−1). The elimination of an extraction step reduced matrix effects considerably making the method suitable for wastewater analysis. Method validation including matrix spike recoveries, linearity of calibration curve and inter- and intra-day variability was successfully performed. Finally, the twenty indicator TOrCs were evaluated in four different wastewater treatment plant (WWTP) effluents through four sample campaigns spread across a year. The occurrence data indicated that all indicator TOrCs were detected in at least three out of the four WWTP effluents. Sucralose, iohexol, TCPP, acesulfame and gemfibrozil were detected in all samples at the four WWTPs indicating they could be used as indicators of wastewater influence in receiving waters. DEET, caffeine, triclosan, iopromide and others are effective indicators at showing seasonal variations, treatment process efficacy, and consumption patterns. Overall, the impact of this study will help develop more effective monitoring programs for TOrCs in water reuse schemes.

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Citations
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Journal ArticleDOI
TL;DR: Data comparisons indicate that pharmaceutical exposures in river systems are highly variable regionally, in part due to variability in prescribing practices, hydrology, wastewater management, and urbanisation and that select annual median pharmaceutical concentrations observed in this study were higher than those previously observed in the European Union and Asia thus far.

127 citations

Journal ArticleDOI
TL;DR: The present study shows the development and validation of a DI-based method by ultra-high-performance liquid chromatography quadrupole-linear ion trap analyser (UHPLC-QqLIT-MS/MS) applied to the monitoring of 115 organic microcontaminants at the ngL-1/μg L-1 level in wastewater effluents from urban WWTPs.

91 citations

Journal ArticleDOI
TL;DR: The effluent composition of the 22 TOrCs were similar within the three WWTPs but quite different to those seen in the US, indicating the importance of region-specific monitoring.

89 citations

Journal ArticleDOI
TL;DR: The results highlight the importance of analyzing water samples using multiple separation techniques and in multiple ionization modes to obtain a comprehensive chemical contaminant profile.
Abstract: Efficient strategies are required to implement comprehensive suspect screening methods using high-resolution mass spectrometry within environmental monitoring campaigns. In this study, both liquid and gas chromatography time-of-flight mass spectrometry (LC-QTOF-MS and GC-QTOF-MS) were used to screen for >5000 target and suspect compounds in the Sacramento–San Joaquin River Delta in Northern California. LC-QTOF-MS data were acquired in All-Ions fragmentation mode in both positive and negative electrospray ionization (ESI). LC suspects were identified using two accurate mass LC-QTOF-MS/MS libraries containing pesticides, pharmaceuticals, and other environmental contaminants and a custom exact mass database with predicted transformation products (TPs). The additional fragment information from the All-Ions acquisition improved the confirmation of the compound identity, with a low false positive rate (9%). Overall, 25 targets, 73 suspects, and 5 TPs were detected. GC-QTOF-MS extracts were run in negative chemi...

81 citations

Journal ArticleDOI
TL;DR: Assessing whether current in vitro bioassays are suitable to detect endocrine activity in a range of water types can help provide guidance on in vitroBioassay selection and required sample enrichment for optimised detection of endocrineactivity in environmental waters.

71 citations


Cites background from "Rapid direct injection LC-MS/MS met..."

  • ...Absolute recoveries withmore complexmatrices such aswastewater can be significantly lower, and accurate chemical quantification often requires the use of deuterated standards (Anumol et al., 2013; Anumol et al., 2015)....

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References
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Journal ArticleDOI
TL;DR: A rapid method using direct injection liquid chromatography-tandem mass spectrometry to measure eight iodinated X-ray contrast media represents the first values of ICM published in the literature for Australia.

63 citations

Journal ArticleDOI
TL;DR: Method ruggedness was demonstrated by quality control and quality assurance 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.
Abstract: 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.

62 citations

Journal ArticleDOI
TL;DR: Hydrochlorothiazide (HCTZ) is an inappropriate first-line drug in hypertension and if a "thiazide-type" diuretic is indicated, either chlorthalidone or indapamide should be selected.

56 citations

Journal ArticleDOI
TL;DR: Stream-water samples and municipal wastewater treatment facility (WWTF) discharge samples in Johnson County, northeastern Kansas, were analyzed for 55 compounds collectively described as organic wastewater compounds (OWCs), finding base-flow samples collected in streams draining predominantly urban watersheds had significantly larger concentrations of cumulative OWCs.

56 citations