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Multi-residue analysis of 90 emerging contaminants in liquid and solid environmental matrices by ultra-high-performance liquid chromatography tandem mass spectrometry. [Dataset]

Contributors

Jane Youdan
Data Collector

Ruth Barden
Data Collector

Barbara Kasprzyk-Hordern
Data Collector

Abstract

The main article describes a new analytical methodology for the determination of 90 emerging contaminants (ECs) in liquid environmental matrices (crude wastewater, final effluent and river water). The application of a novel buffer, ammonium fluoride improved signal response for several ECs determined in negative ionisation mode. Development of a microwave assisted extraction (MAE) protocol as an additional sample extraction step for solid matrices enabled 63 ECs to be simultaneously analysed in digested sludge. To the authors knowledge this is considerably more than any previously reported MAE method. To date, this is the most comprehensive multi-residue analytical method reported in the literature for the determination of ECs in both liquid and solid environmental matrices. The supplementary material associated with this file contains one figure and five tables. To date, this is the most comprehensive multi-residue analytical method reported in the literature for the determination of ECs in both liquid and solid environmental matrices.

Citation

PETRIE, B., YOUDAN, J., BARDEN, R. and KASPRZYK-HORDERN, B. 2016. Multi-residue analysis of 90 emerging contaminants in liquid and solid environmental matrices by ultra-high-performance liquid chromatography tandem mass spectrometry. [Dataset]. Journal of chromatography A [online], 1431, pages 64-78. Available from: https://www.sciencedirect.com/science/article/pii/S0021967315018051#sec0080

Acceptance Date Dec 12, 2015
Online Publication Date Dec 17, 2016
Publication Date Jan 29, 2016
Deposit Date Apr 13, 2021
Publicly Available Date Apr 13, 2021
Publisher Elsevier
DOI https://doi.org/10.1016/j.chroma.2015.12.036
Keywords Pharmaceutical; Illicit drug; Wastewater; Liquid chromatography; Sludge; Mass spectrometry; Microwave assisted extraction
Public URL https://rgu-repository.worktribe.com/output/1308245
Related Public URLs https://rgu-repository.worktribe.com/output/1269175
Type of Data PDF containing 1 figure and 5 tables
Collection Date Oct 5, 2015
Collection Method A total of 90 ECs (personal care products, pharmaceuticals and illicit drugs) were selected for method development. Selection was based upon reference to existing and proposed EU legislation, UK prescription data, metabolism and excretion from the human body, known environmental occurrence, persistence during wastewater treatment and toxicity to aquatic organisms. Chemical names and properties of selected ECs are detailed in Table S1. Initially, samples were filtered through GF/F filters (0.7 μm) and adjusted to pH 7.5 ± 0.1. Crude wastewater and final effluent (50 mL) and river water (100 mL) were spiked with 50 ng of all internal standards and loaded onto Oasis HLB cartridges. These were conditioned using 2 mL MeOH followed by 2 mL H2O at a constant flow rate of 1 mL min−1. Samples were loaded at 5 mL min−1 then dried under vacuum. Digested sludge for extraction was frozen and freeze dried (ScanVac, CoolSafe freeze dryer, Lynge, Denmark). 0.5 g was spiked with 50 ng of all internal standards and left for a minimum of 1 h. Extraction was performed using 25 mL of 50:50 MeOH:H2O (pH 2) using a 800 W MARS 6 microwave (CEM, UK). Samples were heated to 110 °C over 10 min and then maintained at this temperature for 30 min. Chromatography was performed using a Waters Acquity UPLC system (Waters, Manchester, UK). To maximise sensitivity and achieve good chromatography for these ECs exhibiting a broad range of chemistries, two chromatography methods were developed. Linearity was established by triplicate injection of a 17 point calibration curve ranging in concentration from 0.01–1000 ng mL−1. Inter-day and intra-day precision and accuracy was determined by triplicate injections of 10, 100 and 500 ng mL−1 within a 24 h period and across three separate days, respectively. Instrumental detection limits (IDLs) and instrument quantitation limits (IQLs) were calculated according to the lowest concentration which gave a signal to noise ratio of ≥3 and ≥10 respectively. Recovery of target chemicals was determined by spiking crude wastewater and final effluent at a concentration of 100 and 1000 ng L−1. For river water, concentrations of 50 and 500 ng L−1 were selected. For those chemicals determined by direct injection, concentrations of 10 and 100 μg L−1 were used. In digested sludge, recovery of analytes was assessed at spike concentrations of 50 and 100 ng g−1. For a more detailed description of the methods and materials used please see Section 2 of the published article (https://doi.org/10.1016/j.chroma.2015.12.036).

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