Development of a SPE–UHPLC–MS/MS methodology for the determination of non-steroidal anti-inflammatory and analgesic pharmaceuticals in seawater

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.

Efficient biotransformation of non-steroid anti-inflammatory drugs by endophytic and epiphytic fungi from dried leaves of a medicinal plant, Plantago lanceolata L.

“…The compound showed peaks identical to those described in the literature (Macdonald et al, 1991;Dickinson et al, 1994). As in the case of DIC, the halogenated ring was untouched; MS (Paíga et al, 2015), most probably the isobutyl sidechain is hydroxylated. The found fragmentation pathway was similar to that described for alkyl-phenols in (Bajpai et al, 2005).…”

“…The usage of high amounts results in appearance of these compounds and their metabolites in wastewater and also surface waters, as conventional wastewater treatment processes are unable to completely eliminate them (Domaradzka et al, 2015). Despite not being present at high concentrations enough to cause acute toxicity (they are typically detected in the ng l -1 to µg l -1 range (Paíga et al, 2015)), the risk of chronic toxicity can be significant (Domaradzka et al, 2015). For some pharmaceuticals, including the NSAIDs ibuprofen and naproxen, the toxic concentration against Hydra attenuata was found to be close to that detected in wastewater effluents (Quinn et al, 2008).…”

Optimization of the Ion Source-Mass Spectrometry Parameters in Non-Steroidal Anti-Inflammatory and Analgesic Pharmaceuticals Analysis by a Design of Experiments Approach

“…In a previous publication of the authors [19], the MS ion source parameters were optimized using OFAT approach. As a result the NGF and DGF flow rates of 2.6 and 12.5 L·min , with a step of 25°C), and 13 experiments to study the HBT (range from 200 to 500°C spaced by 25°C).…”

“…As the change of those two parameters is very small, the operator assigned to do this work can unintentionally introduce an error. Thus, ESI position and ESI protrusion were set according to the results obtained in the work of Paíga et al [19]. There were, therefore, five parameters [interface voltage (IV, kV), drying gas flow rate (DGF, L·min …”

“…Recent research emphasizes the importance of using statistics in the optimization [7,19]. The present study employs a design of experiment (DoE) strategy in order to find the optimum conditions for the MS ion source parameters reducing significantly the number of runs in the optimization step.…”