Polyacrylonitrile/MIL-53(Fe) electrospun nanofiber for pipette-tip micro solid phase extraction of nitrazepam and oxazep
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ORIGINAL PAPER
Polyacrylonitrile/MIL-53(Fe) electrospun nanofiber for pipette-tip micro solid phase extraction of nitrazepam and oxazepam followed by HPLC analysis Shima Amini 1 & Homeira Ebrahimzadeh 1 & Shahram Seidi 2 & Niloofar Jalilian 1 Received: 18 July 2019 / Accepted: 3 January 2020 # Springer-Verlag GmbH Austria, part of Springer Nature 2020
Abstract Nanofibers were prepared from a nanocomposite consisting of polyacrylonitrile and a metal-organic framework of type MIL53(Fe) by electrospinning. They are shown to be a viable sorbent for pipette-tip solid-phase extraction for the extraction of the benzodiazepine drugs nitrazepam and oxazepam. The nanofibers were characterized by scanning electron microscopy, energy dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy and X-ray diffraction. The effects of sample pH value and volume, composition, and amount of electrospun nanofibers, the number of adsorption cycles and the type and volume of the eluent were optimized. Following extraction the drugs were quantified by HPLC. Under the optimized conditions, response is linear for both drugs in the 5.0–1000 ng mL−1 concentration range. The limits of detection for oxazepam and nitrazepam are 1.5 and 2.5 ng mL−1, respectively, and the relative standard deviations at the levels of 50, 100 and 250 ng mL−1 (for n = 3) are ≤7.6%. The method was successfully applied for determination of drugs in spiked wastewater and biological fluids. Keywords Composite nanosorbent . Miniaturization . Metal organic framework . Sample preparation . Microextraction . Benzodiazepines . Biological fluid . Waste water analysis
Introduction Benzodiazepines (BZDs) are widely consumed for the therapy of anxiety and sleeping disorders, but excessive consumption of these drugs can lead to unwanted side effects, such as memory loss, depression and loss of balance [1, 2]. High performance liquid chromatography (HPLC) [3], gas chromatography [4], thin-layer chromatography (TLC) [5] and other chromatographic methods have been reported for the determination of BZDs [6–8]. However, trace determination of
Electronic supplementary material The online version of this article (https://doi.org/10.1007/s00604-020-4112-3) contains supplementary material, which is available to authorized users. * Homeira Ebrahimzadeh [email protected] 1
Faculty of Chemistry and Petroleum Sciences, Department of Analytical Chemistry and Pollutants, Shahid Beheshti University, G.C., Evin, Tehran 19839-69411, Iran
2
Faculty of Chemistry, Department of Analytical Chemistry, K.N. Toosi University of Technology, Tehran 19697, Iran
analytes in complex matrices is the bottle-neck of an analytical procedure and to overcome this limitation; a sample preparation step is necessary before the final analysis [9, 10]. Nowadays, researchers focus on the development of miniaturized extraction methods, which often lead to the improvement of preconcentration factors and decreasing of the solvent consumption [11–13]. Pipette tip micro solid-phase extraction (PT- μSPE)
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