Magnetic Hydrogel Beads as a Reusable Adsorbent for Highly Efficient and Rapid Removal of Aluminum: Characterization, Response Surface Methodology Optimization, and Evaluation of Isotherms, Kinetics, and Thermodynamic Studies.

Biopolymers such as alginate and gelatin have attracted much attention because of their exceptional adsorption properties and biocompatibility. The magnetic hydrogel beads produced and used in this study had a core structure composed of magnetite nanoparticles and gelatin and a shell structure composed of alginate. The combination of the metal-ion binding ability of alginate and the mechanical strength of gelatin in magnetic hydrogel beads presents a new approach for the removal of metal from water sources. The beads were designed for aluminum removal and fully characterized using various methods, including Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, scanning electron microscopy-energy-dispersive X-ray spectroscopy, vibrating sample magnetometry, microcomputed tomography, and dynamic mechanical analysis. Statistical experimental designs were employed to optimize the parameters of the adsorption and recovery processes. Plackett-Burman Design, Box-Behnken Design, and Central Composite Design were used for identifying the significant factors and optimizing the parameters of the adsorption and recovery processes, respectively. The optimum parameters determined for adsorption are as follows: pH: 4, contact time: 30 min, adsorbent amount: 600 mg; recovery time: reagent 1 M HNO3; and contact time: 40 min. The adsorption process was described by using the Langmuir isotherm model. It reveals a homogeneous bead surface and monolayer adsorption with an adsorption capacity of 5.25 mg g-1. Limit of detection and limit of quantification values were calculated as 4.3 and 14 µg L-1, respectively. The adsorption process was described by a pseudo-second-order kinetic model, which assumes that chemisorption is the rate-controlling mechanism. Thermodynamic studies indicate that adsorption is spontaneous and endothermic. The adsorbent was reusable for 10 successive adsorption-desorption cycles with a quantitative adsorption of 98.2% ± 0.3% and a recovery of 99.4% ± 2.6%. The minimum adsorbent dose was determined as 30 g L-1 to achieve quantitative adsorption of aluminum. The effects of the inorganic ions were also investigated. The proposed method was applied to tap water and carboy water samples, and the results indicate that magnetic hydrogel beads can be an effective and reusable bioadsorbent for the detection and removal of aluminum in water samples. The recovery values obtained by using the developed method were quantitative and consistent with the results obtained from the inductively coupled plasma optical emission spectrometer.

A Fluorimetric Method Based On Magnetic Molecularly Imprinted Polymer For Selective Detection Of Chlorferon.

In the present work, reusable magnetic molecularly imprinted polymers have been used for the first time as an adsorbent for the determination of chlorferon. Magnetic molecularly imprinted polymers have been used for the selective separation of chlorferon from the solution and sensitive fluorimetric determination has been performed using the native fluorescence of chlorferon. The developed method is rapid and determination of chlorferon was completed in an hour. Limit of detection (LOD) of the method was found to be 0.0027 µM and the linearity of the calibration graph was observed within the range of 0.01-0.36 µM (2.5 - 75 µg L-1). Adsorption isotherms point out the multilayer adsorption and the heterogeneous distribution of binding sites for imprinted polymer and homogeneous binding site for non-imprinted polymer. The adsorption capacities of imprinted polymer and non-imprinted polymer were calculated as 2.03 µmol g-1 and 0.96 µmol g-1, respectively and the imprinting factor was found to be 2.11. The interference effects of some organic compounds and characterization studies were also evaluated. The method has been applied to honey and tap water samples and the recoveries were found to be in the range of 91.3 and 101.1 %.

Sensitive and selective determination of imidacloprid with magnetic molecularly imprinted polymer by using LC/Q-TOF/MS.

In this paper, magnetic-molecularly imprinted polymer was used for the preconcentration of trace levels of imidacloprid in water and apple samples prior to liquid chromatography-quadrupole-time-of-flight mass spectrometric determination. The selectivity of the magnetic polymer was united with the sensitivity and the high resolving power of the chromatographic system. The developed method showed a linear range from 10.0 to 500.0 µg/L. The quantitative recoveries were obtained for water and apple samples in the range of 92.0%-99.0 %. The relative standard deviations of intra-day and inter-day tests were found to be in the range of 0.8%-1.2% and 1.2%-1.6 %, respectively. In addition, the same magnetic-molecularly imprinted polymer (MMIP) can be used at least ten cycles for the determination of imidacloprid. The preconcentration factor of the method was found to be 2.5, and the total preconcentration procedure can be completed in 1 h. Characterization of synthesised particles were executed with various techniques. Due to its suitable limit of detection, dynamic linear range, sensitivity and selectivity, the developed method seemed to be ideal for the determination and preconcentration of imidacloprid in water and fruit samples.

Highly sensitive and selective method for the rapid determination and preconcentration of haloperidol by using a magnetite-molecularly imprinted polymer.

A sensitive and selective method based on the determination of haloperidol with the usage of magnetite-molecularly imprinted polymer and high-resolution liquid chromatography has been developed. This novel method is rapid as the detection procedure for haloperidol can be completed within a total time of 1 h. The same imprinted polymer can be used for the determination of haloperidol at least 20 times. The proposed method has been succesfully applied to synthetic urine and serum samples and the recoveries of the spiked samples were in the range of 94.7-100.7%. The limit of detection and limit of quantification of the method were 2.25 and 7.50 µg/L, respectively. Linearity of the calibration graph was observed within the range of 10-250 µg/L. By combining the high capacity, high selectivity, and reusability of the magnetic adsorbent with the dynamic calibration range, high sensitivity and high resolution of liquid chromatography with quadrupole time-of-flight mass spectrometry, the proposed method is an ideal method for the determination and preconcentration of trace levels of haloperidol. A magnetite-molecularly imprinted polymer has been used for the first time as a selective adsorbent for the determination of haloperidol.

Development of rapid, sensitive and selective fluorimetric method for determination of 1-naphthalene acetic acid in cucumber by using magnetite-molecularly imprinted polymer.

In this study, a novel method based on the determination of 1-naphthalene acetic acid with the usage of magnetite-molecularly imprinted polymer prior to fluorimetric detection has been developed. Magnetite-molecularly imprinted polymer has been used for the first time as selective adsorbent for the determination of 1-naphthalene acetic acid. The adsorption capacity of the synthesized polymer was found to be 2.18 ±â€¯0.36 mg g-1 (n = 3). Limit of detection (LOD) and limit of quantification (LOQ) of the method were found to be 0.75 and 2.50 µg L-1, respectively. Linearity of the calibration graph for the proposed method was observed within the range of 20-700 µg L-1. The proposed method seems to be rapid where the detection procedure for 1-naphthalene acetic acid can be completed within a total time of 1 h. The same imprinted polymer can be used for the determination of 1-naphthalene acetic acid with quantitative sorption and recovery values repeatedly for at least ten times. The effects of some potential organic interferences were investigated. Proposed method has been successfully applied to determine 1-naphthalene acetic acid in cucumber, where the recoveries of the spiked samples were found to be in the range of 93.7-104.5%. Characterization of the synthesized polymer was also evaluated. By combining the high capacity, cheapness, reusability and selectivity of the magnetic adsorbent with the dynamic calibration range, rapidity, simplicity, and sensitivity of fluorimetry, the proposed method seems to be an ideal method for the determination of trace levels of 1-naphthalene acetic acid.

Selective and sensitive fluorimetric determination of carbendazim in apple and orange after preconcentration with magnetite-molecularly imprinted polymer.

In this study, magnetite-molecularly imprinted polymer has been used for the first time as selective adsorbent before the fluorimetric determination of carbendazim. Adsorption capacity of the magnetite-molecularly imprinted polymer was found to be 2.31±0.63mgg-1 (n=3). Limit of detection (LOD) and limit of quantification (LOQ) of the method were found to be 2.3 and 7.8µgL-1, respectively. Calibration graph was linear in the range of 10-1000µgL-1. Rapidity is an important advantage of the method where re-binding and recovery processes of carbendazim can be completed within an hour. The same imprinted polymer can be used for the determination of carbendazim without any capacity loss repeatedly for at least ten times. Proposed method has been successfully applied to determine carbendazim residues in apple and orange, where the recoveries of the spiked samples were found to be in the range of 95.7-103%. Characterization of the adsorbent and the effects of some potential interferences were also evaluated. With the reasonably high capacity and reusability of the adsorbent, dynamic calibration range, rapidity, simplicity, cost-effectiveness and with suitable LOD and LOQ, the proposed method is an ideal method for the determination of carbendazim.