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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
초록

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
제품 번호
브랜드
제품 설명

Sigma-Aldrich
Ammonia-14N, 99.99 atom % 14N
Acetylsalicylic acid for peak identification, European Pharmacopoeia (EP) Reference Standard
Diclofenac for system suitability, European Pharmacopoeia (EP) Reference Standard
Paracetamol, European Pharmacopoeia (EP) Reference Standard
Acetylsalicylic acid, European Pharmacopoeia (EP) Reference Standard
Ibuprofen for peak identification, European Pharmacopoeia (EP) Reference Standard
Supelco
Hydrogen chloride – ethanol solution, ~1.25 M HCl, LiChropur
Sigma-Aldrich
p-Acetamidophenyl β-D-glucuronide sodium salt, >98% (TLC)
Sigma-Aldrich
Hydrogen chloride solution, 3 M in cyclopentyl methyl ether (CPME)
Sigma-Aldrich
Ammonia solution, 0.4 M in THF
Sigma-Aldrich
Ammonia solution, 0.4 M in dioxane
Sigma-Aldrich
Ammonia solution, 4 M in methanol
Sigma-Aldrich
Ammonia solution, 2.0 M in ethanol
Sigma-Aldrich
Acetylsalicylic acid, analytical standard
Sigma-Aldrich
Acetylsalicylic acid, ≥99.0%
Sigma-Aldrich
Diclofenac sodium salt
Supelco
Diclofenac sodium salt, analytical standard
Supelco
Methanol, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Methanol, Laboratory Reagent, ≥99.6%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, suitable for HPLC, ≥99.9%
Supelco
Methanol, analytical standard
Sigma-Aldrich
Methanol, ACS spectrophotometric grade, ≥99.9%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Hydrochloric acid solution, ~6 M in H2O, for amino acid analysis
Sigma-Aldrich
Hydrochloric acid solution, 1.0 N, BioReagent, suitable for cell culture
USP
Ibuprofen, United States Pharmacopeia (USP) Reference Standard
Supelco
Ibuprofen
Sigma-Aldrich
Hydrogen chloride solution, 4.0 M in dioxane
Sigma-Aldrich
Hydrochloric acid solution, 32 wt. % in H2O, FCC