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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
ABSTRAKT

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.

MATERIAŁY
Numer produktu
Marka
Opis produktu

Supelco
Naproxen, Pharmaceutical Secondary Standard; Certified Reference Material
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Acetaminophen, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Formic acid, ≥95%, FCC, FG
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Aspirin (Acetyl Salicylic Acid), Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
(S)-(+)-6-Methoxy-α-methyl-2-naphthaleneacetic acid, 98%
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Nimesulide
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Acetaminophen, meets USP testing specifications, 98.0-102.0%, powder
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Acetaminophen, BioXtra, ≥99.0%
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Ketoprofen, ≥98% (TLC)
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Aspirin, meets USP testing specifications
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Acetaminophen, analytical standard
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Naproxen, meets USP testing specifications
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Formic acid solution, BioUltra, 1.0 M in H2O
Sigma-Aldrich
4-Aminophenol, ≥98%
Sigma-Aldrich
Ammonium hydroxide solution, BioUltra, ~1 M NH3 in H2O (T)
Supelco
Naproxen, VETRANAL®, analytical standard
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4-Aminophenol, PESTANAL®, analytical standard
Sigma-Aldrich
Ketoprofen, meets USP testing specifications
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4-Aminophenol (Acetaminophen Related Compound K) (Paracetamol Impurity K), Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Ketoprofen, VETRANAL®, analytical standard
USP
Aspiryna, United States Pharmacopeia (USP) Reference Standard
USP
Acetaminofen, United States Pharmacopeia (USP) Reference Standard
USP
4-Aminophenol, United States Pharmacopeia (USP) Reference Standard
USP
Diklofenak sodowy, United States Pharmacopeia (USP) Reference Standard
Mesalazine impurity A, European Pharmacopoeia (EP) Reference Standard
USP
Ketoprofen, United States Pharmacopeia (USP) Reference Standard
USP
Naproxen, United States Pharmacopeia (USP) Reference Standard
Naproxen, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
Formic acid, ACS reagent, ≥88%
Sigma-Aldrich
Ammonium hydroxide solution, 28% NH3 in H2O, ≥99.99% trace metals basis