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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
(±)-Propranolol hydrochloride, ≥99% (TLC), powder
Sigma-Aldrich
Naproxen, meets USP testing specifications
Sigma-Aldrich
Caffeine, meets USP testing specifications, anhydrous
Sigma-Aldrich
Caffeine, BioXtra
Supelco
Sulfamethoxazole
Supelco
Gemfibrozil, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Sulfamethoxazole, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
(S)-(+)-6-Methoxy-α-methyl-2-naphthaleneacetic acid, 98%
Furosemide, European Pharmacopoeia (EP) Reference Standard
USP
Furosemide, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Nimesulide
Sigma-Aldrich
Ketoprofen, meets USP testing specifications
Supelco
Furosemide, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Caffeine Melting Point Standard, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Naproxen, Pharmaceutical Secondary Standard; Certified Reference Material
Furosemide for peak identification, European Pharmacopoeia (EP) Reference Standard
Cimetidine for system suitability, European Pharmacopoeia (EP) Reference Standard
Cimetidine for peak identification, European Pharmacopoeia (EP) Reference Standard
Naproxen, European Pharmacopoeia (EP) Reference Standard
Caffeine, European Pharmacopoeia (EP) Reference Standard
Nimesulide, European Pharmacopoeia (EP) Reference Standard
Nimesulide for peak identification, European Pharmacopoeia (EP) Reference Standard
Sulfamethoxazole, European Pharmacopoeia (EP) Reference Standard
Supelco
Nimesulide, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
(±)-Propranolol hydrochloride, analytical standard
Gemfibrozil, European Pharmacopoeia (EP) Reference Standard
Ketoprofen, European Pharmacopoeia (EP) Reference Standard
Supelco
Diazepam solution, 1.0 mg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®
Diclofenac sodium, European Pharmacopoeia (EP) Reference Standard
Gemfibrozil for system suitability, European Pharmacopoeia (EP) Reference Standard