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  • 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
ABSTRACT

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.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
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Hydrogen chloride – ethanol solution, ~1.25 M HCl, for GC derivatization, LiChropur
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Ammonia-14N, 99.99 atom % 14N
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Hydrochloric acid solution, 32 wt. % in H2O, FCC
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Ibuprofen, European Pharmacopoeia (EP) Reference Standard
Acetylsalicylic acid, European Pharmacopoeia (EP) Reference Standard
Ibuprofen for peak identification, European Pharmacopoeia (EP) Reference Standard
Supelco
Ibuprofen, Pharmaceutical Secondary Standard; Certified Reference Material
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Hydrogen chloride – methanol solution, ~1.25 m HCl (T), for GC derivatization, LiChropur
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Ammonia solution, 4 M in methanol
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Methanol, Pharmaceutical Secondary Standard; Certified Reference Material
Diclofenac for system suitability, European Pharmacopoeia (EP) Reference Standard
Acetylsalicylic acid for peak identification, European Pharmacopoeia (EP) Reference Standard