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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
Hydrogen chloride solution, 3 M in cyclopentyl methyl ether (CPME)
Sigma-Aldrich
Methanol, SAJ special grade
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Hydrochloric acid solution, 0.5 M
Sigma-Aldrich
Hydrochloric acid solution, 12 M
Sigma-Aldrich
Hydrochloric acid solution, 2 M
Sigma-Aldrich
Hydrochloric acid solution, 1 M
Sigma-Aldrich
Hydrochloric acid solution, 6 M
Sigma-Aldrich
Hydrogen chloride – ethanol solution, 0.1 M in ethanol
Sigma-Aldrich
Hydrochloric acid solution, 0.2 M
Paracetamol, European Pharmacopoeia (EP) Reference Standard
Ibuprofen, European Pharmacopoeia (EP) Reference Standard
Acetylsalicylic acid, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
Ammonia-14N, 99.99 atom % 14N
Sigma-Aldrich
Methanol, HPLC Plus, ≥99.9%, poly-coated bottles
Supelco
Diclofenac sodium salt, Pharmaceutical Secondary Standard; Certified Reference Material
Ibuprofen for peak identification, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
Methanol, suitable for HPLC, gradient grade, 99.93%
Supelco
Ibuprofen
Sigma-Aldrich
Methanol, anhydrous, 99.8%
Supelco
Hydrogen chloride – 2-propanol solution, ~1.25 M HCl (T), for GC derivatization, LiChropur
Supelco
Hydrogen chloride – ethanol solution, ~1.25 M HCl, for GC derivatization, LiChropur
Supelco
Hydrogen chloride – methanol solution, ~1.25 m HCl (T), for GC derivatization, LiChropur
Supelco
Methanol, analytical standard
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Ammonia, anhydrous, ≥99.98%
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Hydrochloric acid solution, 1.0 N, BioReagent, suitable for cell culture
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p-Acetamidophenyl β-D-glucuronide sodium salt, >98% (TLC)
Sigma-Aldrich
Ibuprofen, ≥98% (GC)
Sigma-Aldrich
Diclofenac sodium salt
Sigma-Aldrich
Hydrochloric acid, 36.5-38.0%, BioReagent, for molecular biology
Sigma-Aldrich
Acetylsalicylic acid, analytical standard