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In this study, we present hydrazide functionalized magnetic nanoparticles as a sorbent prepared by a new and facile method. Scanning electron microscope and Fourier transform infrared were used for characterizing the synthesized nanoparticles. The ability of the sorbent to extract N-terminal serine and threonine peptides was evaluated. The peptides were modified by oxidation of the hydroxyl group in the 1,2-amino alcohol structure before extraction. These aldehyde-forms of peptides were specifically bonded to the hydrazide groups of the sorbent. The formed hydrazone bonds were cleaved in the presence of hydroxylamine reagent. Finally, the oximated peptides were released and quantified with a high-performance liquid chromatography-diode array spectroscopy. The effects of experimental parameters including extraction time, elution time and elution volume on extraction efficiency were also investigated. The required time for the extraction process to reach equilibrium and elution time was only 8 h. The adsorption efficiency of the sorbent was 79 and 77% for peptides with N-terminal serine and threonine, respectively. The sorbent showed good specificity for extracting the peptides. In addition, the extraction efficiency of the sorbent remained constant in the presence of a non-N-terminal serine and threonine peptide as interference., (© 2018 John Wiley & Sons, Ltd.)

The application of layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disks for solid-phase extraction is reported for the first time. Al 2 O 3 is embedded in a polymer matrix followed by an in situ metal-exchange process to obtain a layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disk with excellent flow-through properties. The extraction performance of the prepared disks is evaluated as a proof of concept for the automated extraction using sequential injection analysis of organic acids (p-hydroxybenzoic acid, 3,4-dihydroxybenzoic acid, gallic acid) following an anion-exchange mechanism. After the solid-phase extraction, phenolic acids were quantified by reversed-phase high-performance liquid chromatography with diode-array detection using a core-shell silica-C18 stationary phase and isocratic elution (acetonitrile/0.5% acetic acid in pure water, 5:95, v/v). High sensitivity and reproducibility were obtained with limits of detection in the range of 0.12-0.25 μg/L (sample volume, 4 mL), and relative standard deviations between 2.9 and 3.4% (10 μg/L, n = 6). Enrichment factors of 34-39 were obtained. Layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disks had an average lifetime of 50 extractions. Analyte recoveries ranged from 93 to 96% for grape juice and nonalcoholic beer samples., (© 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

In this paper, we report an environmentally-friendly and low cost synthetic approach for large-scale fabrication of 2-dimentional porous Ni/Co-NO 3 -based layered double hydroxide (Ni/Co-NO 3 -LDH) nanosheet through ultrasonic-assisted process. The synthesis procedure used ethylene glycol/water system as an eco-friendly solvent system. The synthesized LDH was characterized by FE-SEM, TEM, XRD, and FT-IR techniques. FE-SEM and TEM images showed porous structure surface morphology of the synthesized LDH. Also, For Ni/Co-NO 3 -LDH, a hexagonal ultrathin layered was obtained owing to ultrasonic irradiation and applied processing conditions. The prepared LDH was used as sorbent in dispersive micro solid-phase extraction procedure. Two phenolic acids including p-hydroxybenzoic acid and p-coumaric acid were selected as model compounds. Some experimental factors affecting the extraction efficiency of the analytes were investigated and optimized. Finally, the sorbent was used for the extraction of model compound from fruit juice samples followed by high performance liquid chromatography. Linear dynamic range of 0.5-500µgL -1 with a low detection limit (0.1µgL -1 ) was obtained by the method. The relative standard deviations were 2.5 and 4.3% for p-hydroxybenzoic acid and p-coumaric acid, respectively. All recoveries were between 82 and 92%., (Copyright © 2017 Elsevier B.V. All rights reserved.)

We present for the first time the application of metal-organic framework (MOF) mixed-matrix disks (MMD) for the automated flow-through solid-phase extraction (SPE) of environmental pollutants. Zirconium terephthalate UiO-66 and UiO-66-NH 2 MOFs with different size (90, 200 and 300nm) have been incorporated into mechanically stable polyvinylidene difluoride (PVDF) disks. The performance of the MOF-MMDs for automated SPE of seven substituted phenols prior to HPLC analysis has been evaluated using the sequential injection analysis technique. MOF-MMDs enabled the simultaneous extraction of phenols with the concomitant size exclusion of molecules of larger size. The best extraction performance was obtained using a MOF-MMD containing 90nm UiO-66-NH 2 crystals. Using the selected MOF-MMD, detection limits ranging from 0.1 to 0.2μgL -1 were obtained. Relative standard deviations ranged from 3.9 to 5.3% intra-day, and 4.7-5.7% inter-day. Membrane batch-to-batch reproducibility was from 5.2 to 6.4%. Three different groundwater samples were analyzed with the proposed method using MOF-MMDs, obtaining recoveries ranging from 90 to 98% for all tested analytes., (Copyright © 2017 Elsevier B.V. All rights reserved.)

In this work, a polypyrrole/multiwalled carbon nanotubes composite decorated with Fe3 O4 nanoparticles was chemically synthesized and applied as a novel adsorbent for the extraction of methocarbamol from human plasma. Electrospray ionization ion mobility spectrometry was used for the determination of the analyte. The properties of the magnetic-modified adsorbent were characterized by scanning electron microscopy, transmission electron microscopy, Fourier transform IR spectroscopy, and X-ray diffraction. The effects of experimental parameters on the extraction efficiency of the sorbent were investigated. Under the optimized conditions, the linear dynamic range was found to be 2-150 ng/mL with the detection limit of 0.9 ng/mL. The relative standard deviation was 5.3% for three replicate measurements of methocarbamol in plasma sample. The extraction efficiency of the sorbent for the determination of different drugs with various polarities was also compared to that of Fe3 O4 -polypyrrole and Fe3 O4 -multiwalled carbon nanotubes sorbents. Finally, the method was used for the determination of methocarbamol in blood samples., (© 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

We have prepared a solid phase for the extraction of chlorobenzenes (CBs) by coating magnetic (Fe3 O4 ) nanoparticles with silica via a sol-gel process using a mixture of tetraethoxysilane and triethoxyphenylsilane. The nanoparticles were characterized by SEM, energy-dispersive spectroscopy, and X-ray diffractometry. The nanoparticles were used for the extraction of 1,4-dichlorobenzene (1,4-DCB), 1,2,3-trichlorobenzene (1,2,3-TCB), 1,2,4-trichlorobenzene (1,2,4-TCB), and 1,2,3,4-tetrachlorobenzene (1,2,3,4-TeCB) from water, followed by their determination by GC-electron capture detection. Under optimal conditions, enrichment factors ranging from 220 to 360 were obtained. All determination coefficients (r(2)) are >0.99, and linear response is found in range 0.025-1.5 μg/L (at the lower end), and 6-120 μg/L (at the higher end). Detection limits are 6, 10, 11, and 500 ng/L for 1,2,3,4-TeCB, 1,2,4-TCB, 1,2,3-TCB, and 1,4-DCB, respectively. All RSDs are <6% (for n = 5). The method was successfully applied to the determination of CBs in environmental water samples., (© 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

Hollow fiber-based liquid-liquid-liquid microextraction (HF-LLLME) followed by flow injection analysis and diode array detection (FIA-DAD) was applied as a simple and sensitive quantitative method for the determination of phenazopyridine in urine and plasma samples. Flow injection system included a conventional HPLC system (without a chromatographic column) and a diode array detector. The extraction of phenazopyridine was carried out using diphenyl ether as the organic phase for filling the pores of the hollow fiber wall, and 0.1 M H(2)SO(4) solution as acceptor phase in the lumen of the fiber. The factors affecting the HF-LLLME and flow injection analysis including type of organic solvent, pH of donor phase, extraction temperature, extraction time, stirring rate, and pH of mobile phase were investigated and the optimal extraction conditions were established. With the consumption of 5 mL of sample solution, the enrichment factor was about 230. The limit of detection was 0.5 μg/L with inter- and intra-day precision being (RSD%) 6.9 and 4.9, respectively. Excellent linearity was found between 5 and 200 μg/L., (Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

A new ion-imprinted polymer (IIP) material was synthesized by copolymerization of 4-vinylpyridine as monomer, ethyleneglycoldimethacrylate as crosslinking agent and 2,2'-azobis-sobutyronitrile as initiator in the presence of Ni-dithizone complex. The IIP was used as sorbent in a solid-phase extraction column. The effects of sampling volume, elution conditions, sample pH and sample flow rate on the extraction of Ni ions form water samples were studied. The maximum adsorption capacity and the relative selectivity coefficients of imprinted polymer for Ni(II)/Co(II), Ni(II)/Cu(II) and Ni(II)/Cd(II) were calculated. Compared with non-imprinted polymer particles, the IIP had higher selectivity for Ni(II). The relative selectivity factor (alpha(r)) values of Ni(II)/Co(II), Ni(II)/Cu(II) and Ni(II)/Cd(II) were 21.6, 54.3, and 22.7, respectively, which are greater than 1. The relative standard deviation of the five replicate determinations of Ni(II) was 3.4%. The detection limit for 150 mL of sample was 1.6 microg L(-1) using flame atomic absorption spectrometry. The developed method was successfully applied to the determination of trace nickel in water samples with satisfactory results.