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Superparamagnetic Fe 3 O 4 @SiO 2 core–shell composite nanoparticles for the mixed hemimicelle solid‐phase extraction of benzodiazepines from hair and wastewater samples before high‐performance liquid chromatography analysis
Author(s) -
EsmaeiliShahri Effat,
Es'haghi Zarrin
Publication year - 2015
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201500743
Subject(s) - nanoparticle , solid phase extraction , superparamagnetism , fourier transform infrared spectroscopy , chemistry , analytical chemistry (journal) , detection limit , extraction (chemistry) , magnetic nanoparticles , scanning electron microscope , materials science , nuclear chemistry , chromatography , chemical engineering , magnetization , nanotechnology , quantum mechanics , magnetic field , composite material , physics , engineering
Magnetic Fe 3 O 4 /SiO 2 composite core–shell nanoparticles were synthesized, characterized, and applied for the surfactant‐assisted solid‐phase extraction of five benzodiazepines diazepam, oxazepam, clonazepam, alprazolam, and midazolam, from human hair and wastewater samples before high‐performance liquid chromatography with diode array detection. The nanocomposite was synthesized in two steps. First, Fe 3 O 4 nanoparticles were prepared by the chemical co‐precipitation method of Fe(III) and Fe(II) as reaction substrates and NH 3 /H 2 O as precipitant. Second, the surface of Fe 3 O 4 nanoparticles was modified with shell silica by Stober method using tetraethylorthosilicate. The Fe 3 O 4 /SiO 2 composite were characterized by X‐ray diffraction, scanning electron microscopy, Fourier transform infrared spectroscopy, and vibrating sample magnetometry. To enhance their adsorptive tendency toward benzodiazepines, cetyltrimethylammonium bromide was added, which was adsorbed on the surface of the Fe 3 O 4 /SiO 2 nanoparticles and formed mixed hemimicelles. The main parameters affecting the efficiency of the method were thoroughly investigated. Under optimum conditions, the calibration curves were linear in the range of 0.10–15 μgmL −1 . The relative standard deviations ranged from 2.73 to 7.07%. The correlation coefficients varied from 0.9930 to 0.9996.