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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

Supelco
Acetaminophen, Pharmaceutical Secondary Standard; Certified Reference Material
Pricing and availability is not currently available.
Supelco
Naproxen, Pharmaceutical Secondary Standard; Certified Reference Material
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Sigma-Aldrich
Formic acid, JIS special grade, ≥98.0%
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(S)-(+)-6-Methoxy-α-methyl-2-naphthaleneacetic acid, 98%
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Methanol-12C, 99.95 atom % 12C
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Sigma-Aldrich
Acetaminophen, BioXtra, ≥99.0%
Pricing and availability is not currently available.
Sigma-Aldrich
Ketoprofen, ≥98% (TLC)
Pricing and availability is not currently available.
Sigma-Aldrich
Ketoprofen, meets USP testing specifications
Pricing and availability is not currently available.
Sigma-Aldrich
Nimesulide
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Sigma-Aldrich
Naproxen, meets USP testing specifications
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Sigma-Aldrich
Aspirin, meets USP testing specifications
Pricing and availability is not currently available.
Sigma-Aldrich
Acetaminophen, analytical standard
Pricing and availability is not currently available.
Sigma-Aldrich
Formic acid solution, BioUltra, 1.0 M in H2O
Pricing and availability is not currently available.
Sigma-Aldrich
Ammonium hydroxide solution, BioUltra, ~1 M NH3 in H2O (T)
Pricing and availability is not currently available.
Sigma-Aldrich
4-Aminophenol, ≥98%
Pricing and availability is not currently available.
Supelco
4-Aminophenol, PESTANAL®, analytical standard
Pricing and availability is not currently available.
Sigma-Aldrich
Formic acid, ≥95%, FCC, FG
Pricing and availability is not currently available.
Ketoprofen, European Pharmacopoeia (EP) Reference Standard
Pricing and availability is not currently available.
Diclofenac sodium, European Pharmacopoeia (EP) Reference Standard
Pricing and availability is not currently available.
Supelco
Acetaminophen solution, 1.0 mg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®
Pricing and availability is not currently available.
Supelco
Methanol solution, contains 0.10 % (v/v) formic acid, UHPLC, suitable for mass spectrometry (MS), ≥99.5%
Pricing and availability is not currently available.
Sigma-Aldrich
Acetaminophen, meets USP testing specifications, 98.0-102.0%, powder
Pricing and availability is not currently available.
USP
4-Aminophenol, United States Pharmacopeia (USP) Reference Standard
Pricing and availability is not currently available.
Mesalazine impurity A, European Pharmacopoeia (EP) Reference Standard
Pricing and availability is not currently available.
Nimesulide, European Pharmacopoeia (EP) Reference Standard
Pricing and availability is not currently available.
Supelco
Ketoprofen, Pharmaceutical Secondary Standard; Certified Reference Material
Pricing and availability is not currently available.
Naproxen, European Pharmacopoeia (EP) Reference Standard
Pricing and availability is not currently available.
USP
Ketoprofen, United States Pharmacopeia (USP) Reference Standard
Pricing and availability is not currently available.
Sigma-Aldrich
Formic acid, ACS reagent, ≥96%
Pricing and availability is not currently available.
Sigma-Aldrich
Ammonium hydroxide solution, puriss., 30-33% NH3 in H2O
Pricing and availability is not currently available.