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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
RESUMEN

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.

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Metanol, suitable for HPLC, ≥99.9%
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Ácido clorhídrico, ACS reagent, 37%
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Metanol, ACS reagent, ≥99.8%
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Hidróxido de amonio solution, ACS reagent, 28.0-30.0% NH3 basis
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Metanol, suitable for HPLC, gradient grade, ≥99.9%
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Ácido clorhídrico, ACS reagent, 37%
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Ácido fórmico, reagent grade, ≥95%
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Metanol, HPLC Plus, ≥99.9%
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Cloruro de hidrógeno solution, 4.0 M in dioxane
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Ácido fórmico, ACS reagent, ≥96%
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Hidróxido de amonio solution, 28% NH3 in H2O, ≥99.99% trace metals basis
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Ammonia solution, 7 N in methanol
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Ácido clorhídrico solution, 1.0 N, BioReagent, suitable for cell culture
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Metanol, suitable for HPLC, gradient grade, suitable as ACS-grade LC reagent, ≥99.9%
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Metanol, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.8% (GC)
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Ácido clorhídrico, 36.5-38.0%, BioReagent, for molecular biology
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Ácido clorhídrico, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., fuming, ≥37%, APHA: ≤10
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Cloruro de hidrógeno solution, 2.0 M in diethyl ether
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Hidróxido de amonio solution, puriss., 30-33% NH3 in H2O
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Ácido clorhídrico solution, volumetric, 0.1 M HCl (0.1N), endotoxin free
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Ibuprofen, ≥98% (GC)
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4-Aminophenol, ≥98%
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Metanol, Absolute - Acetone free
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