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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

Sigma-Aldrich
Indomethacin, meets USP testing specifications
Sigma-Aldrich
Sulfamethazine sodium salt, ≥98%
Supelco
Ibuprofen sodium salt, ≥98% (GC)
Sigma-Aldrich
Bezafibrate, ≥98%, solid
Sigma-Aldrich
Trimethoprim, ≥98.5%
Sigma-Aldrich
Nifedipine, ≥98% (HPLC), powder
Sigma-Aldrich
Diclofenac sodium salt
Sigma-Aldrich
Carbamazepine, powder
Sigma-Aldrich
Ammonium acetate, reagent grade, ≥98%
Sigma-Aldrich
Mefenamic acid
Sigma-Aldrich
Carbamazepine, meets USP testing specifications
Sigma-Aldrich
Ammonium acetate, BioXtra, ≥98%
Supelco
Warfarin, analytical standard
Sigma-Aldrich
Atenolol, ≥98% (TLC), powder
Sigma-Aldrich
Ammonium acetate, for molecular biology, ≥98%
Sigma-Aldrich
Ammonium acetate solution, BioUltra, for molecular biology, ~5 M in H2O
Sigma-Aldrich
Cimetidine
Sigma-Aldrich
Ammonium acetate, 99.999% trace metals basis
Supelco
Trimethoprim, VETRANAL®, analytical standard
Supelco
Warfarin, PESTANAL®, analytical standard
Supelco
Ammonium acetate, LiChropur, eluent additive for LC-MS
Sigma-Aldrich
Trimethoprim, ≥99.0% (HPLC)
Diazepam for system suitability, European Pharmacopoeia (EP) Reference Standard
Atenolol, European Pharmacopoeia (EP) Reference Standard
Bezafibrate, European Pharmacopoeia (EP) Reference Standard
Carbamazepine, European Pharmacopoeia (EP) Reference Standard
Supelco
Bezafibrate, analytical standard
Supelco
Indomethacin, Pharmaceutical Secondary Standard; Certified Reference Material
Propranolol hydrochloride for performance test, European Pharmacopoeia (EP) Reference Standard
Propranolol hydrochloride, European Pharmacopoeia (EP) Reference Standard