4.2 Article

Analyses of Nonsteroidal Anti-inflammatory Drugs in Human Plasma Using Dispersive Nano Solid-Phase Extraction and High-Performance Liquid Chromatography

Journal

CHROMATOGRAPHIA
Volume 79, Issue 3-4, Pages 145-157

Publisher

SPRINGER HEIDELBERG
DOI: 10.1007/s10337-015-3020-x

Keywords

1-Butyl-3-methylimidazolium bromide; Nonsteroidal anti-inflammatory drugs; Nano dispersive solid-phase extraction method; Sample preparation; HPLC; Phenyl column; Separation mechanism

Funding

  1. Deanship of Scientific Research at King Saud University [PRG-1436-04]

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Iron nanoparticles were synthesized by green technology. These were functionalized with 1-butyl-3-methylimidazolium bromide (ionic liquid) to enhance specificity and selectivity. Fourier transform infrared spectroscopy, energy dispersive X-ray fluorescence, X-ray diffraction, scanning electron microscopy and transmission electron microscopy were used for characterization. 1-Butyl-3-methylimidazolium bromide-functionalized iron nanoparticles (BMIF-INPs) were applied in nano dispersive solid-phase extraction for the extraction of nonsteroidal anti-inflammatory drugs (NSAIDs) from the plasma prior. The different extraction parameters such as type and amount of sorbents, agitation time, pH, desorbing solvents, desorbing volume, and desorption times were optimized. Optimum conditions were 1.5 mg mL(-1) of BMIF-INP sorbent, 20 min of agitation time, pH of 5.0, acetonitrile + 0.1 % acetic acid desorbing solvent, 600 mu L of desorbing volume and 2 min of desorbing time. The percentage recoveries of all the six NSAIDs ranged from 87.4 to 94.98 %. High-performance liquid chromatography was developed using a pentafluorophenyl column (100 x 4.6 mm; 2.6 mu m) and water-acetonitrile-acetic acid (70: 30, v/v) of pH 3.0 with acetic acid as the mobile phase. The flow rate was 1.0 mL min(-1) with detection at 240 nm. The values of k, alpha and R-s ranged from 0.83 to 19.0, 1.16 to 6.13 and 1.0 to 5.76, respectively. The developed sample preparation and chromatographic methods were fast, selective, inexpensive, economical and reproducible. These methods have good applications and may be used for analyzing these drugs in biological, environmental and industrial matrices.

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