Abstract
Calixarene framework functionalized bio-polymeric magnetic composites (MSp-TDI-calix) were synthesized and utilized as magnetic solid-phase extraction (MSPE) sorbent for the extraction of non-steroidal anti-inflammatory drugs (NSAIDs), namely indoprofen (INP), ketoprofen (KTP), ibuprofen (IBP) and fenoprofen (FNP), from environmental water samples. MSp-TDI-calix was characterized by FT-IR, XRD, FESEM, EDX, VSM and BET analysis, and the results were compared with Sp-TDI and Sp-TDI-calix. To maximize the extraction performance of MSp-TDI-calix decisive MSPE affective parameters such as sorbent amount, extraction time, sample volume, type of organic eluent, volume of organic eluent, desorption time and pH were comprehensively optimized prior to HPLC-DAD determination. The analytical validity of the proposed MSPE method was evaluated under optimized conditions and the following figures of merit were acquired: linearity with good determination coefficient (R2 ≥ 0.991) over the concentration range of 0.5–500 µg/L, limits of detection (LODs) ranged from 0.06–0.26 µg/L and limits of quantitation (LOQ) between 0.20–0.89 µg/L. Excellent reproducibility and repeatability under harsh environment with inter-day and intra-day relative standard deviations were obtained in the range of 2.5–3.2% and 2.4–3.9% respectively. The proposed method was successfully applied for analysis of NSAIDs in tap water, drinking water and river water with recovery efficiency ranging from 88.1–115.8% with %RSD of 1.6–4.6%.
Highlights
From an environmental point of view, the mixing of pharmaceuticals as well as their degraded products into natural streams is of great concern (Lacey et al, 2008; Toledo-Neira & Álvarez Lueje, 2015)
In Sp-TDI, the presence of IR bands at 2,280 cm−1 may be attributed to the isocyanate peak while appearance of the IR band at 1,645 cm−1 confirmed the existence of aromatic rings
The IR bands at 1,604 cm−1 and 1,233 cm−1 indicates the presence of C=O and C–N stretches of the formed carbamate linkages between isocyanate proving the incorporation of isocyanate functionalities on the surface of sporopollenin
Summary
From an environmental point of view, the mixing of pharmaceuticals as well as their degraded products into natural streams is of great concern (Lacey et al, 2008; Toledo-Neira & Álvarez Lueje, 2015). The NSAIDs may transfer to natural streams through hospital and pharmaceutical units, effluent, as well as private household manure (ToledoNeira & Álvarez Lueje, 2015) These drugs pose toxic effects in aquatic ecosystems and may cause harm to marine life and to humans (Aguilar-Arteaga et al, 2010). It is a challenge to reach down to this detection level due to complicated matrix effects in real samples and this needs to be adequately addressed Several analytical techniques such as gas chromatography (GC) (Samaras et al, 2011), capillary electrophoresis (CE) (Macià et al, 2004), liquid chromatography mass spectrometry (LC-MS) (Toledo-Neira & Álvarez Lueje, 2015) and high performance liquid chromatography (HPLC) (Aguilar-Arteaga et al, 2010) have been employed for NSAIDs determination. Due to high resolution, great automation and high reproducibility, HPLC is considered as one of the most commonly used techniques (Fan et al, 2014)
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