Direkt zum Inhalt
Merck
  • Development of a SPE-UHPLC-MS/MS methodology for the determination of non-steroidal anti-inflammatory and analgesic pharmaceuticals in seawater.

Development of a SPE-UHPLC-MS/MS methodology for the determination of non-steroidal anti-inflammatory and analgesic pharmaceuticals in seawater.

Journal of pharmaceutical and biomedical analysis (2014-07-09)
Paula Paíga, Aleksandar Lolić, Floris Hellebuyck, Lúcia H M L M Santos, Manuela Correia, Cristina Delerue-Matos
ZUSAMMENFASSUNG

An analytical methodology for the simultaneous determination of seven pharmaceuticals and two metabolites belonging to the non-steroidal anti-inflammatory drugs (NSAIDs) and analgesics therapeutic groups was developed based on off-line solid-phase extraction and ultra-high performance liquid chromatography coupled to tandem mass spectrometry (SPE-UHPLC-MS/MS). Extraction conditions were optimized taking into account parameters like sorbent material, sample volume and sample pH. Method detection limits (MDLs) ranging from 0.02 to 8.18 ng/L were obtained. This methodology was successfully applied to the determination of the selected pharmaceuticals in seawater samples of Atlantic Ocean in the Northern Portuguese coast. All the pharmaceuticals have been detected in the seawater samples, with pharmaceuticals like ibuprofen, acetaminophen, ketoprofen and the metabolite hydroxyibuprofen being the most frequently detected at concentrations that can reach some hundreds of ng/L.

MATERIALIEN
Produktnummer
Marke
Produktbeschreibung

Sigma-Aldrich
Methanol, suitable for HPLC, ≥99.9%
Sigma-Aldrich
Salzsäure, ACS reagent, 37%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Ammoniumhydroxid -Lösung, ACS reagent, 28.0-30.0% NH3 basis
Sigma-Aldrich
Methanol, suitable for HPLC, gradient grade, ≥99.9%
Sigma-Aldrich
Salzsäure, ACS reagent, 37%
Sigma-Aldrich
Ameisensäure, reagent grade, ≥95%
Sigma-Aldrich
Methanol, HPLC Plus, ≥99.9%
Sigma-Aldrich
Chlorwasserstoff -Lösung, 4.0 M in dioxane
Sigma-Aldrich
Ameisensäure, ACS reagent, ≥96%
Sigma-Aldrich
Ammoniumhydroxid -Lösung, 28% NH3 in H2O, ≥99.99% trace metals basis
Sigma-Aldrich
Ameisensäure, puriss. p.a., ACS reagent, reag. Ph. Eur., ≥98%
Sigma-Aldrich
Ammoniak -Lösung, 7 N in methanol
Sigma-Aldrich
Salzsäure -Lösung, 1.0 N, BioReagent, suitable for cell culture
Sigma-Aldrich
Methanol, suitable for HPLC, gradient grade, suitable as ACS-grade LC reagent, ≥99.9%
Sigma-Aldrich
Salzsäure, meets analytical specification of Ph. Eur., BP, NF, fuming, 36.5-38%
Sigma-Aldrich
Methanol, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.8% (GC)
Sigma-Aldrich
Salzsäure, 37 wt. % in H2O, 99.999% trace metals basis
Sigma-Aldrich
Salzsäure, 36.5-38.0%, BioReagent, for molecular biology
Sigma-Aldrich
Ammoniumhydroxid -Lösung, puriss., 30-33% NH3 in H2O
Sigma-Aldrich
Salzsäure, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., fuming, ≥37%, APHA: ≤10
Sigma-Aldrich
Chlorwasserstoff -Lösung, 2.0 M in diethyl ether
Sigma-Aldrich
Methanol, Laboratory Reagent, ≥99.6%
Sigma-Aldrich
Ameisensäure, puriss., meets analytical specifications of DAC, FCC, 98.0-100%
Sigma-Aldrich
Ameisensäure, ACS reagent, ≥88%
Supelco
Salzsäure -Lösung, volumetric, 0.1 M HCl (0.1N), endotoxin free
Sigma-Aldrich
4-Aminophenol, ≥98%
Sigma-Aldrich
Ibuprofen, ≥98% (GC)
Sigma-Aldrich
Methanol, ACS spectrophotometric grade, ≥99.9%
Sigma-Aldrich
Ammoniumhydroxid -Lösung, puriss. p.a., reag. ISO, reag. Ph. Eur., ~25% NH3 basis