Al-Khazrajy, Omar S.A. and Boxall, Alistair B.A. orcid.org/0000-0003-3823-7516 (2017) Determination of pharmaceuticals in freshwater sediments using ultrasonic-assisted extraction with SPE clean-up and HPLC-DAD or LC-ESI-MS/MS detection. Analytical methods. pp. 4190-4200. ISSN 1759-9679
Abstract
A robust and sensitive analytical method is presented for the extraction and determination of six pharmaceuticals in freshwater sediments. The pharmaceuticals were extracted from sediment using ultrasonic extraction with 2% NH4OH in methanol (MeOH), followed by extraction into 2% formic acid in MeOH and then MeOH only. The resulting extracts were then analysed, after clean-up on HLB solid phase extraction cartridges, using a single gradient run using a Zorbax Eclipse XDB-C18 (150 × 4.6 mm, 5 μm) column and a mobile phase consisting of 10 mM ammonium acetate and MeOH (pH = 4.8). Analytes were detected and quantified using either Diode Array Detector (DAD) or tandem mass spectrometry (MS/MS) with electrospray ionization in positive mode. Validation studies were carried out using ten sediments sampled from the UK and Iraq with a wide range of characteristics. The mean calculated recoveries for fortified samples in all studied sediments ranged from 74.5 to 114.6% for atenolol, 72.3 to 124.9% for amitriptyline, 76.5 to 105% for mefenamic acid and 70.1 to 102% for diltiazem. Cimetidine and ranitidine showed lower recoveries which ranged from 40.2 to 68.4% and 30.4 to 55.2% respectively. Relative standard deviations (RSD) of recoveries for all sediment-pharmaceutical combinations ranged from 1.6 to 15.8%. The detection limits in sediments for the six analytes ranged from 15 to 58.5 ng g-1 and 0.03 to 3.5 ng g-1, dry weight, for HPLC-UV and LC-ESI-MS/MS respectively. Overall the results indicate that the developed method is effective for use in monitoring the concentrations of pharmaceuticals in aquatic sediments in different regions.
Metadata
Item Type: | Article |
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Authors/Creators: |
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Copyright, Publisher and Additional Information: | © 2017, The Royal Society of Chemistry. This is an author-produced version of the published paper. Uploaded in accordance with the publisher’s self-archiving policy. Further copying may not be permitted; contact the publisher for details. |
Dates: |
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Institution: | The University of York |
Academic Units: | The University of York > Faculty of Sciences (York) > Environment and Geography (York) |
Depositing User: | Pure (York) |
Date Deposited: | 08 Aug 2017 09:45 |
Last Modified: | 08 Feb 2025 00:24 |
Published Version: | https://doi.org/10.1039/c7ay00650k |
Status: | Published |
Refereed: | Yes |
Identification Number: | 10.1039/c7ay00650k |
Related URLs: | |
Open Archives Initiative ID (OAI ID): | oai:eprints.whiterose.ac.uk:119887 |
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Description: Determination of pharmaceuticals in freshwater sediments