Abstract

A magnetic solid-phase extraction (MSPE) procedure on the newly synthesized magnetic β-cyclodextrin functionalized with toluene diisocyanate (TDI) as a linker and further modified with bio-polymeric spores of sporopollenin (MSp-TDI-βCD), was developed for the extraction of nonsteroidal anti-inflammatory drugs (NSAIDs), namely, indoprofen (INP), ketoprofen (KTP), ibuprofen (IBP) and fenoprofen (FNP) from water samples prior to their HPLC-DAD determination. The newly synthesized MSp-TDI-βCD was comprehensibly characterized using FT-IR, XRD, SEM-EDX, BET and VSM analyses. The separation of selected NSAIDs on MSp-TDI-βCD from aqueous solution was simply achieved by applying an external magnetic field via a permanent magnet. The MSPE parameters affecting extraction performance, i.e. sorbent dosage, sample volume, extraction and desorption time, type of organic eluent and volume and solution pH were investigated and optimized. The proposed method showed linear range between 0.5 and 500 ng ml−1, low limit of detection at S/N = 3 (0.16–0.37 ng ml−1) and limit of quantification at S/N = 10 (0.53–1.22 ng ml−1). The inter-day (n = 15) and intra-day (n = 5) precision for the proposed methods given by relative standard deviation (RSD%) was in the range of 2.5–4.0 and 2.1–5.5, respectively. The extraction recoveries of NSAIDs from environmental samples (tap, drinking and river water) ranged from 92.5% to 123.6%, with satisfactory precision (RSD% less than 12.4%).

Highlights

  • In the past few decades, massive manufacturing of pharmaceutical products has been creating serious environmental problems because contaminated effluents of pharmaceutical products contain highly stable and persistent environmental pollutants [1,2,3]

  • Literature survey indicated that determination of nonsteroidal anti-inflammatory drugs (NSAIDs) in waste water samples, involving pre-concentration step and separation followed by quantification, is necessary due to its low concentration in complex matrix [6,7]

  • Sporopollenin surface was connected with toluene diisocyanate (TDI) as a linker by connecting at para position of isocyanate group

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Summary

Introduction

In the past few decades, massive manufacturing of pharmaceutical products has been creating serious environmental problems because contaminated effluents of pharmaceutical products contain highly stable and persistent environmental pollutants [1,2,3]. Wastewater from hospitals, pharmaceutical industries and private households, by virtue of these therapeutic drug agents, leads to the contamination of water sources and poses a severe threat to human health [1,2]. By virtue of well-known toxicity and detrimental effect, the precise determination and detoxification of NSAIDs contaminated aqueous environment is of significant importance [4,5]. Literature survey indicated that determination of NSAIDs in waste water samples, involving pre-concentration step and separation followed by quantification, is necessary due to its low concentration in complex matrix [6,7]. The selectivity issues play an important role in the determination of NSAIDs in water samples [8]

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