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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
(±)-Propranolol hydrochloride, analytical standard
Naproxen, European Pharmacopoeia (EP) Reference Standard
Supelco
Mettler-Toledo Calibration substance ME 18872, Caffeine, traceable to primary standards (LGC)
Supelco
Ketoprofen, VETRANAL®, analytical standard
Diazepam, European Pharmacopoeia (EP) Reference Standard
Diclofenac sodium, European Pharmacopoeia (EP) Reference Standard
Caffeine, European Pharmacopoeia (EP) Reference Standard
Supelco
Nimesulide, Pharmaceutical Secondary Standard; Certified Reference Material
Trimethoprim for system suitability, European Pharmacopoeia (EP) Reference Standard
Gemfibrozil, European Pharmacopoeia (EP) Reference Standard
Gemfibrozil for system suitability, European Pharmacopoeia (EP) Reference Standard
Cimetidine for peak identification, European Pharmacopoeia (EP) Reference Standard
Furosemide for peak identification, European Pharmacopoeia (EP) Reference Standard
Supelco
Flurbiprofen, Pharmaceutical Secondary Standard; Certified Reference Material
Cimetidine for system suitability, European Pharmacopoeia (EP) Reference Standard
Supelco
Caffeine, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
Supelco
Sulfamethoxazole, Pharmaceutical Secondary Standard; Certified Reference Material
Ketoprofen, European Pharmacopoeia (EP) Reference Standard
Supelco
Gemfibrozil, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Diazepam solution, 1.0 mg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®
USP
Sulfamethoxazole, United States Pharmacopeia (USP) Reference Standard
Flurbiprofen, European Pharmacopoeia (EP) Reference Standard
Supelco
Ketoprofen, Pharmaceutical Secondary Standard; Certified Reference Material
Nimesulide for peak identification, European Pharmacopoeia (EP) Reference Standard
Sulfamethoxazole, European Pharmacopoeia (EP) Reference Standard
USP
Diclofenac sodium, United States Pharmacopeia (USP) Reference Standard
USP
Ketoprofen, United States Pharmacopeia (USP) Reference Standard
Supelco
Caffeine, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Furosemide, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Naproxen, Pharmaceutical Secondary Standard; Certified Reference Material