Magnetic Sporopollenin Research Articles

A new bodipy/pillar[5]arene functionalized magnetic sporopollenin for the detection of Cu(II) and Hg(II) ions in aqueous solution

In this study, a new bodipy/pillar[5]arene functionalized magnetic MS-Sp-P[5]-bodipy microcapsule sensor was prepared based on the use of environmentally friendly for the selective and sensitive detection of Cu(II) and Hg(II) ions in aqueous media. SEM results used in the characterization process of the materials synthesized at each stage confirmed the structural and morphological changes in the pore structure, while other characterization results (FT-IR and XRD) elucidated the role of pillar[5]arene compound and bodipy dye in the synthesis of magnetic microcapsule sensors. The colloidal solution of MS-Sp-P[5]-bodipy (water/ethanol)) showed two fluorescence bands centered at 402 and 540 nm. The detection limits of MS-Sp-P[5]-bodipy for Hg(II) and Cu(II) were calculated to be 0.06 µM and 2.27 µM, respectively (at 540 nm). The linear range of the magnetic sensor for Hg(II) and Cu(II) was found to be in the range of 1–150 µM and 10–150 µM, respectively. The experimental results (response time, pH, temperature, sensitivity and selectivity) demonstrated the applicability and potential of the prepared magnetic microcapsule sensor for the detection of Cu(II) and Hg(II) in water and tap water samples containing heavy metal ions.

Magnetic sporopollenin supported magnesium nanoparticles for removal of tetracycline as an emerging contaminant from water.

Since the release of antibiotics as emerging contaminants into the environmental water can cause severe difficulties for human health, their removal from the water is necessary. In this regard, a novel environmentally friendly adsorbent was developed based on green sporopollenin, which was magnetized and modified with magnesium oxide nanoparticles to produce MSP@MgO nanocomposite. The newly developed adsorbent was applied to remove tetracycline antibiotic (TC) from aqueous media. The surface morphology of the MSP@MgO nanocomposite was characterized using FTIR, XRD, EDX, and SEM techniques. The effective parameters of the removal process were studied, and it was confirmed that the chemical structure of TC was highly affected by changes in pH solution due to different pKa; therefore, the results showed that pH 5 was the optimum. Also, the maximum sorption capacity of MSP@MgO for TC for adsorption was obtained at 109.89 mg.g-1. In addition, the adsorption models were investigated, and the process was fitted with the Langmuir model. Thermodynamic parameters showed that the process was spontaneous (ΔG < 0), endothermic (ΔH > 0) and the adsorption mechanism was following the physisorption mechanism at room temperature.

Efficient Removal of 2,4-Dichlorophenoxyacetic Acid from Aqueous Medium Using Polydopamine/Polyacrylamide Co-deposited Magnetic Sporopollenin and Optimization with Response Surface Methodology Approach

Efficient Removal of 2,4-Dichlorophenoxyacetic Acid from Aqueous Medium Using Polydopamine/Polyacrylamide Co-deposited Magnetic Sporopollenin and Optimization with Response Surface Methodology Approach

Decolorization of Rhodamine B by silver nanoparticle-loaded magnetic sporopollenin: characterization and process optimization.

Silver nanoparticles (Ag NPs) were reduced on the surface of magnetic sporopollenin (Fe3O4@SP) modified with poly-dopamine to enhance the degradation capability for Rhodamine B (RhB). The polydopamine-coated Fe3O4@SP (PDA@ Fe3O4@SP) acts as a self-reducing agent for Ag+ ions to Ag0. The structural properties of the synthesized nanocomposite were determined using Fourier transform infrared spectrometry (FTIR), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), X-ray powder diffraction (XRD), inductively coupled plasma mass spectrometry (ICP-MS), and vibrating sample magnetometer (VSM). The systematic study of the degradation process was performed using Response Surface Methodology (RSM) to determine the relationship between the four process variables, namely, initial RhB concentration, NaBH4 amount, catalyst amount, and time. Optimum points were determined for these four parameters using both matrix and numerical optimization methods. Under optimum conditions, RhB was decolorized with a yield of 98.11%. The apparent activation energy (Ea) and rate constant (k) for the degradation were 24.13kJ/mol and 0.77min-1, respectively. The reusability studies of the Ag@PDA@Fe3O4@SP exhibited more than 85% degradation ability of the dye even after five cycles. As a result, Ag@PDA@Fe3O4@SP possessed high catalytic activity, fast reduction rate, good reusability, easy separation, and simple preparation, endowing this catalyst to be used as a promising catalyst for the decolorization of dyes in aqueous solutions.

Magnetic sporopollenin supported polyaniline developed for removal of lead ions from wastewater: Kinetic, isotherm and thermodynamic studies

This study evaluated the synthesis of novel binary functionaladsorbent based on sporopollenin, magnetic nanoparticles, and polyaniline to produce MSP-PANI. The MSP-PANI was applied to enhance uptake of lead ions (Pb2+) from wastewater samples. The functionalities, surface morphology, magnetic properties, and elemental composition of the newly synthesized nanocomposite were investigated using Fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscopy (FE-SEM), vibration sample magnetometer (VSM), and energy-dispersive X-ray spectroscopy (EDX), respectively. The experimental condition for the adsorption process was MSP/PANI ratio 1:1, pH ∼6, adsorbent dosage 40 mg, and contact time 90 min at room temperature. Under the proposed condition, lead ions removal were obtained as 83%, 88% and 95% for MSPE, PANI, and MSP/PANI, respectively. Based on the experimental and predicted data, the adsorption was corresponded to the psudo-second-order (R2 = 0.999) kinetics model, and the adsorption equilibrium corresponded to the Langmuir model (R2 = 0.996). Langmuir isotherm showed the maximum adsorption capacity of MSP-PANI for lead ions was 163 mg/g and followed the monolayer pattern. Hence, thermodynamic model under Van't Hoff equation suggested that the adsorption mechanism was physio-sorption with endothermic nature. Therefore, this research can help the researchers to use magnetic nanoparticles for lead removal in highly polluted areas.

Green sporopollenin supported cyanocalixarene based magnetic adsorbent for pesticides removal from water: Kinetic and equilibrium studies

In this study, magnetic sporopollenin supported cyanocalixarene (MSP-CyCalix) nanocomposite was synthesized and introduced as an adsorbent material for the removal of pesticides from aqueous media. MSP-CyCalix was characterized by different analytical techniques FTIR, SEM, EDX, BET, VSMand TEM. Chlorpyrifos and hexaconazole pesticides were chosen as model analytes solutions for testing the adsorption efficiency of MSP-CyCalix adsorbent. The adsorption results showed that the incorporated cyano functional groups significantly increased the chemical reactivity and adsorption capacity for pesticides. To obtain the highest possible performance, experimental parameters such as pH, salt, dosage and time were optimized. Adsorption kinetics and isotherms models showed that pesticide adsorption process was well fitted with the pseudo-second-order and Langmuir models with a maximum adsorption capacity of 13.88 mg g−1 and 12.34 mg g−1 and a removal efficiency of >90% for both pesticides. Lastly, MSP-CyCalix maintained a removal efficiency of >80% for ten cycles and 60% after the eleventh cycles of usage. The results proved that MSP-CyCalix nanocomposite can be used as an efficient adsorbent for the removal of pesticide residues from water.

New effective 3-aminopropyltrimethoxysilane functionalized magnetic sporopollenin-based silica coated graphene oxide adsorbent for removal of Pb(II) from aqueous environment

A new effective adsorbent, 3-aminopropyltrimethoxysilane functionalized magnetic sporopollenin (MSp@SiO2NH2) based silica-coated graphene oxide (GO), (GO@SiO2-MSp@SiO2NH2) was successfully synthesized and applied for the first time in the removal of hazardous Pb(II) ions from aqueous solution. The properties of the composite were characterized using Fourier-transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDX) and vibrating-sample magnetometery (VSM). Evaluation of GO@SiO2-MSp@SiO2NH2 adsorption performance at optimum conditions revealed that the adsorbent has a maximum adsorption capacity of 323.5 mg/g for Pb(II) using 50–200 mg/L initial Pb(II) ions concentrations. Initial and final concentrations of Pb(II) ions in aqueous solution were analyzed using graphite furnace atomic absorption spectroscopy (GF-ASS). The adsorption behavior of Pb(II) ions onto GO@SiO2-MSp@SiO2NH2 was studied using Langmuir, Freundlich and Temkin isotherms models. The values of coefficient of determination showed that the adsorption best fitted the Langmuir model (R2 = 0.9994). Kinetic studies suggested that the adsorption of Pb(II) ion followed a pseudo-second-order rate model (R2 = 1.00) and thermodynamic studies revealed that the adsorption process is endothermic and spontaneous. The effect of co-existing ions on Pb(II) ion adsorption were also studied and found to have considerable effects only at higher matrix concentration. The adsorbent can be reused up to ten times and retain its good adsorption capacity. In addition, GO@SiO2-MSp@SiO2NH2 showed great potential for Pb(II)removal from industrial wastewater samples.

Facile liquid-phase deposition synthesis of titania-coated magnetic sporopollenin for the selective capture of phosphopeptides.

Titania-grafted magnetic sporopollenin is synthesized by the liquid-phase deposition (LPD) technique, characterized by SEM, EDX, and nitrogen adsorption porosimetry, and used for the selective enrichment of phosphorylated peptides. The material is low cost because of easier availability of pollens and has rich surface chemistry which enables strong attachment of titania onto magnetic sporopollenin. The material shows higher selectivity of 1:1000 with β-casein spiked in BSA. Higher sensitivity of 10fmol is recorded for phosphopeptides from standard β-casein digest. Twenty phosphorylated peptides are enriched from milk digest and four endogenous phosphopeptides from diluted human serum. The magnetic property of titania-coated magnetic sporopollenin facilitates the fast and effective isolation of phosphopeptides from complex mixtures through external magnet. The material is finally applied to tryptic digest of rat brain cell lysate for phosphopeptide enrichment where 2718 phosphopeptides are identified by using LC-MS/MS with C18 column. Titania-coated magnetic sporopollenin captures both mono-phosphorylated (2489) and multi-phosphorylated peptides (229) due to strong affinity of TiO2 with phosphates. TiO2-coated magnetic material also shows better enrichment efficiency in comparison to commercial TiO2. Graphical abstract.

Candida rugosa lipase encapsulated with magnetic sporopollenin: design and enantioselective hydrolysis of racemic arylpropanoic acid esters

The aim of this study was to prepare the encapsulation of Candida rugosa lipase (CRL) with magnetic sporopollenin. The sporopollenin was covalent immobilized onto magnetic nanoparticles (Fe3O4), grafted amino (APTES), or epoxy groups (EPPTMS). CRL was sol-gel encapsulated in the presence of magnetic sporopollenin/Fe3O4 nanoparticles. The influence of activation agents ([3-(2,3-epoxypropoxy) propyl] trimethoxysilane (EPPTMS), (3-Aminopropyl)triethoxysilane (APTES) and pH and thermal stabilities of the biocatalyst were assessed. Experimental data showed the improved catalytic activity at different pH and temperature values. At 60 °C, free lipase lost its initial activity within 80 min of time, although the encapsulated lipases retained their initial activities of about 65% by APTES and 60% by EPPTMS after 120 min of heat treatment at 60 °C. The catalytic properties of the encapsulated lipases were utilized to hydrolysis of racemic aromatic carboxylic acid methyl esters (Naproxen and 2-phenoxypropionic acid). The results show that the sporopollenin-based encapsulated lipase (Fe-A-Spo-E) has greater enantioselectivity and conversion in comparison with the encapsulated lipase without supports (lipase-enc).

Synthesis of piperazine functionalized magnetic sporopollenin: a new organic-inorganic hybrid material for the removal of lead(II) and arsenic(III) from aqueous solution.

The present work describes the successful functionalization/magnetization of bio-polymeric spores of Lycopodium clavatum (sporopollenin) with 1-(2-hydroxyethyl) piperazine. Analytical techniques, i.e., Fourier transform infrared (FT-IR), field emission scanning electron microscope (FESEM), energy-dispersive X-ray spectroscopy (EDS), and vibrating sample magnetometer (VSM), were used to confirm the formation of 1-(2-hydroxyethyl) piperazine-functionalized magnetic sporopollenin (MNPs-Sp-HEP). The proposed adsorbent (MNPs-Sp-HEP) was used for the removal of noxious Pb(II) and As(III) metal ions from aqueous media through a batch-wise method. Different experimental parameters were optimized for the effective removal of selected noxious metal ions. Maximum adsorption capacity (q m ) 13.36 and 69.85mgg-1 for Pb(II) and As(III), respectively, were obtained. Thermodynamic parameters such as free energy (ΔG°), entropy (ΔS°), and enthalpy (ΔH°) were also studied from the adsorption results and were used to elaborate the mechanism of their confiscation. The obtained results indicated that newly adsorbent can be successfully applied for the decontamination of noxious Pb(II) and As(III) from the aqueous environment.

The removal of organophosphorus pesticides from water using a new amino-substituted calixarene-based magnetic sporopollenin

This study describes the synthesis, characterization and application of a new amino-substituted p-tert-butylcalix[4]arene-based magnetic sporopollenin, Calix-EPPTMS-MS (4), for the removal of two toxic organophosphorus pesticides from water.

Synthesis of N-methylglucamine functionalized calix[4]arene based magnetic sporopollenin for the removal of boron from aqueous environment

The present study deals with the synthesis of new N-methylglucamine functionalized calix[4]arene based magnetic sporopollenin (4) and its application for the removal of boron from aqueous environment. The newly prepared calix[4]arene immobilized material 4 is characterized by SEM, EDS and FT-IR spectroscopy. The sorption efficiency of newly calix[4]arene-based magnetic material 4 for boron from aqueous media was evaluated through the solid–liquid sorption experiments. During the sorption process, various kinds of interactions such as electrostatic repulsion, deprotonation of the hydroxyl groups of sorbent 4, and dissociation of H3BO3 into anions/cations were monitored. The sorption of boron on material 4 is highly pH dependent and significant percent sorption (84%) was achieved at pH=7.5. The sorption behavior was analyzed by Langmuir and Freundlich isotherms. The values of correlation coefficients (R2) showed that the Langmuir isotherm model found to be best fit. Experimental data revealed that material 4 is an efficient sorbent which can be effectively used for the boron decontamination of aqueous media.

Enantioselective enzymatic hydrolysis of racemic drugs by encapsulation in sol–gel magnetic sporopollenin

Candida rugosa lipase was encapsulated within a sol-gel procedure and improved considerably by fluoride-catalyzed hydrolysis of mixtures of octyltriethoxysilane and tetraethoxysilane in the presence of magnetic sporopollenin. The catalytic properties of the immobilized lipases were evaluated into model reactions, i.e., the hydrolysis of p-nitrophenylpalmitate (p-NPP), and the enantioselective hydrolysis of racemic naproxen methyl ester, mandelic acid methyl ester or 2-phenoxypropionic acid methyl ester that were studied in aqueous buffer solution/isooctane reaction system. The encapsulated magnetic sporopollenin (Spo-M-E) was found to give 319 U/g of support with 342% activity yield. It has been observed that the percent activity yields and enantioselectivity of the magnetic sporopollenin encapsulated lipase were higher than that of the encapsulated lipase without support. The substrate specificity of the encapsulated lipase revealed more efficient hydrolysis of the racemic naproxen methyl ester and 2-phenoxypropionic acid methyl ester than racemic mandelic acid methyl ester. It was observed that excellent enantioselectivity (E > 400) was obtained for encapsulated lipase with magnetic sporopollenin with an ee value of S-Naproxen and R-2 phenoxypropionic acid about 98%.