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  • Pharmaceuticals in the freshwater invertebrate, Gammarus pulex, determined using pulverised liquid extraction, solid phase extraction and liquid chromatography-tandem mass spectrometry.

Pharmaceuticals in the freshwater invertebrate, Gammarus pulex, determined using pulverised liquid extraction, solid phase extraction and liquid chromatography-tandem mass spectrometry.

The Science of the total environment (2014-12-30)
Thomas H Miller, Gillian L McEneff, Rebecca J Brown, Stewart F Owen, Nicolas R Bury, Leon P Barron
ABSTRACT

The development, characterisation and application of a new analytical method for multi-residue PPCP determination in the freshwater amphipod, Gammarus pulex are presented. Analysis was performed using pulverised liquid extraction (PuLE), solid phase extraction (SPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). Qualitative method performance offered excellent limits of detection at <20 ng g(-1) for 18 out of 29 compounds. For quantitative application, linearity and precision were considered acceptable for 10 compounds across the ng-μg g(-1) range (R2≥0.99; ≤20% relative standard deviation respectively). The method was applied to the analysis of G. pulex and river water sourced from six tributaries of the River Thames. Carbamazepine, diazepam, nimesulide, trimethoprim and warfarin were determined in G. pulex samples at low ng g(-1) (dry weight) concentrations across these sites. Temazepam and diclofenac were also detected, but were not quantifiable. Six pharmaceuticals were quantified in surface waters across the eight sites at concentrations ranging from 3 to 344 ng L(-1). The possibility for confirmatory detection and subsequent quantification of pharmaceutical residues in benthic organisms such as G. pulex will enable further understanding on the susceptibility and ecological effects of PPCPs in the aquatic environment.

MATERIALS
Product Number
Brand
Product Description

Supelco
Trimethoprim, VETRANAL®, analytical standard
Sigma-Aldrich
Indomethacin, 98.5-100.5% (in accordance with EP)
Sigma-Aldrich
Indomethacin, meets USP testing specifications
Sigma-Aldrich
Trimethoprim, ≥98.5%
Supelco
Ibuprofen sodium salt, ≥98% (GC)
Supelco
Warfarin, analytical standard
Sigma-Aldrich
Ammonium acetate, reagent grade, ≥98%
Sigma-Aldrich
Ammonium acetate solution, for molecular biology, 7.5 M
Sigma-Aldrich
Atenolol, ≥98% (TLC), powder
Sigma-Aldrich
Ammonium acetate, ≥99.99% trace metals basis
Supelco
Carbamazepine, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Trimethoprim, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Ammonium acetate, ACS reagent, ≥97%
Supelco
Diclofenac sodium salt, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Propranolol hydrochloride, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Indomethacin, Pharmaceutical Secondary Standard; Certified Reference Material
Mefenamic acid, European Pharmacopoeia (EP) Reference Standard
Supelco
Mefenamic acid, analytical standard
Diclofenac for system suitability, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
Furosemide
Sigma-Aldrich
Caffeine, powder, ReagentPlus®
Sigma-Aldrich
Caffeine, Sigma Reference Standard, vial of 250 mg
Sigma-Aldrich
Caffeine, anhydrous, tested according to Ph. Eur.
Supelco
Sulfamethoxazole
Sigma-Aldrich
Caffeine, anhydrous, 99%, FCC, FG