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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
ZUSAMMENFASSUNG

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.

MATERIALIEN
Produktnummer
Marke
Produktbeschreibung

Sigma-Aldrich
Ammoniumacetat, ACS reagent, ≥97%
Sigma-Aldrich
Ammoniumacetat, ≥99.99% trace metals basis
Sigma-Aldrich
Ammoniumacetat, for molecular biology, ≥98%
Sigma-Aldrich
Ammoniumacetat -Lösung, for molecular biology, 7.5 M
Sigma-Aldrich
Indomethacin, 98.5-100.5% (in accordance with EP)
Sigma-Aldrich
Trimethoprim, ≥98.5%
Sigma-Aldrich
Koffein, anhydrous, 99%, FCC, FG
Sigma-Aldrich
(±)-Propranolol -hydrochlorid, ≥99% (TLC), powder
Sigma-Aldrich
Diclofenac Natriumsalz
Sigma-Aldrich
Ammoniumacetat, 99.999% trace metals basis
Sigma-Aldrich
Trimethoprim, ≥99.0% (HPLC)
USP
Koffein, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Carbamazepin, powder
Sigma-Aldrich
Furosemid
Sigma-Aldrich
Diazepam
Supelco
Diazepam -Lösung, 1.0 mg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®
Sigma-Aldrich
Atenolol, ≥98% (TLC), powder
Sigma-Aldrich
Nifedipin, ≥98% (HPLC), powder
Sigma-Aldrich
Koffein, powder, ReagentPlus®
Sigma-Aldrich
Ketoprofen, ≥98% (TLC)
Supelco
Koffein, Pharmaceutical Secondary Standard; Certified Reference Material
USP
Koffein-Schmelzpunkt-Standard, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Indomethacin, meets USP testing specifications
USP
Diclofenacnatrium, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Cimetidin
Supelco
Ammoniumacetat, LiChropur, eluent additive for LC-MS
USP
Propranolol -hydrochlorid, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Bezafibrat, ≥98%, solid
USP
Naproxen, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Mefenaminsäure