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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
Ammonium acetate, ACS reagent, ≥97%
Sigma-Aldrich
Ammonium acetate, ≥99.99% trace metals basis
Supelco
Propranolol hydrochloride, Pharmaceutical Secondary Standard; Certified Reference Material
Propranolol hydrochloride, European Pharmacopoeia (EP) Reference Standard
USP
Propranolol hydrochloride, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Ammonium acetate, BioXtra, ≥98%
Sigma-Aldrich
Ammonium acetate, for molecular biology, ≥98%
Sigma-Aldrich
Ammonium acetate solution, BioUltra, for molecular biology, ~5 M in H2O
Supelco
Ammonium acetate, LiChropur, eluent additive for LC-MS
Sigma-Aldrich
Ammonium acetate, BioUltra, for molecular biology, ≥99.0%
Sigma-Aldrich
Ammonium acetate, reagent grade, ≥98%
Sigma-Aldrich
Ammonium acetate solution, for molecular biology, 7.5 M
Sigma-Aldrich
Ammonium acetate, 99.999% trace metals basis
Supelco
Melting point standard 235-237°C, analytical standard
Nifedipine, European Pharmacopoeia (EP) Reference Standard
Supelco
Trimethoprim, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Carbamazepine, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Cimetidine, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Diclofenac sodium salt, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Indomethacin, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Nifedipine, Pharmaceutical Secondary Standard; Certified Reference Material
Indomethacin, European Pharmacopoeia (EP) Reference Standard
USP
Carbamazepine, United States Pharmacopeia (USP) Reference Standard
USP
Atenolol, United States Pharmacopeia (USP) Reference Standard
USP
Trimethoprim, United States Pharmacopeia (USP) Reference Standard
Caffeine for system suitability, European Pharmacopoeia (EP) Reference Standard
USP
Indomethacin, United States Pharmacopeia (USP) Reference Standard
USP
Nifedipine, United States Pharmacopeia (USP) Reference Standard
Supelco
Diclofenac sodium salt, analytical standard