Bulk Polymerization Research Articles

Chromoionophores decorated silica-polymer hybrid monolith as the solid-state optical sensor for the simultaneous detection of Pb2+, Hg2+, and Cd2+ in aqueous and cigarette samples

This work reports on fabricating a flexible and reliable three-in-one solid-phase ocular sensor to perceive and confiscate the trace Pb2+, Hg2+, and Cd2+ using a structurally customized probe-anchored porous hybrid monolithic sensor. The dual combination of silica/polymer hybrid monolith was achieved from the bulk polymerization of 3-(trimethoxysilyl) propyl methacrylate (TSPM) and pentaerythritol trimethacrylate (PETMA), i.e., poly(TSPM-co-PETMA). The monolithic template delivered a well-ordered porous structure and greater surface area that enabled the regular impregnation of chromophoric probe (TAN), i.e., (E)-1-(thiazol-2-yldiazenyl) naphthalene-2-ol onto monolith surface for sensing target analytes under lower ppb levels. FE-SEM, HR-TEM, EDAX, SAED, p-XRD, FT-IR, TGA and N2 isotherm were deployed to characterize the structural and exterior topographies of the hybrid sensor. The geometrically frozen TAN molecules onto the hybrid monolith form a charge transfer complex with the target ions, thereby rendering a consecutive color shift from light orange to brown for Pb2+, reddish maroon for Hg2+, and purplish pink for Cd2+. The sensor offered a linear response with metal ion concentrations ranging from 0.2 to 100 ppb with lower detection limit values of 0.42, 0.50, and 0.48 ppb for Pb2+, Hg2+, and Cd2+, respectively. The hybrid sensor affords distinct ion sensitivity and selectivity towards Pb2+, Hg2+, and Cd2+ with a quick response time of ≤ 80 s of contact. Furthermore, the sensor was tested with natural samples like environmental water and cigarette samples to validate the method’s real-time monitoring ability. The resultant statistical data demonstrated that the proposed colorimetric sensor was renewable and more feasible for practical application.

Mechanical and Dimensional Stability of Gelatin-Based Hydrogels Through 3D Printing-Facilitated Confined Space Assembly.

Hydrogels have emerged as promising biomaterials for tissue regeneration; yet, their inherent swelling can cause deformation and reduced mechanical properties, posing challenges for practical applications in biomedical engineering. Traditional methods to reduce hydrogel swelling often involve complex synthesis procedures with limited flexibility. Inspired by nature's efficient designs, we present here the approach to improve hydrogel performance using 3D printing-assisted microstructure engineering. By utilizing polymerization-induced phase separation of hydrogel from copolymerization of gelatin methacrylate and hydroxyethyl methacrylate (poly(GelMA-co-HEMA)) in the confined space during vat photopolymerization (VPP) 3D printing, we replicate the cuttlebone-like microstructure of hydrogels with enhanced mechanical properties and swelling resistance. We demonstrate here a 4-fold increase in elastic modulus compared to bulk polymerization of poly(GelMA-co-HEMA), together with improved mechanical and dimensional stability. This method offers promising opportunities for practical biomedical and tissue engineering applications, overcoming previous limitations in the design and performance.

Preparation and application of a new ion-imprinted polymer for nanomolar detection of mercury(II) in environmental waters

This study introduces a novel ion-imprinted polymer for the ultrasensitive detection of mercury(II) in water. The ion-imprinted polymer was synthesized via a simple bulk polymerization process using methacrylic acid as the functional monomer, ethylene glycol dimethacrylate as the cross-linker, morpholine-4-carbodithioic acid phenyl ester as the chelating agent, and ammonium persulfate as the initiator. The electrochemical mercury(II) sensing capability of the ion-imprinted polymer was studied via the modification of a cost-effective carbon paste electrode. A stripping voltammetric technique was utilized to quantify the analyte ions following open-circuit enrichment. Critical experimental parameters, including the nature and concentration of the eluent, solution pH, preconcentration duration, ion-imprinted polymer dosage, sample solution volume and reduction potential, were systematically studied and optimized. Under optimal conditions, the sensor exhibited a linear response in the range of 1.0 to 240.0 nM, with a low detection limit of 0.2 nM. The sensor demonstrated remarkable selectivity against potential interfering ions, including lead(II), cadmium(II), copper(II), zinc(II), manganese(II), iron(II), magnesium(II), calcium(II), sodium(I) and cobalt(II). The practical applicability of the developed method was successfully validated through the analysis of real water samples, suggesting its potential for environmental monitoring applications.

An entropy- TOPSIS approach to find PMMA/cellulose based biocomposite with optimum mechanical and bio-degradation properties

Poly methyl methacrylate based biocomposite has been manufactured using nanocellulose as reinforcement, which has been extracted from bagasse. The biocomposites are formed by bulk polymerization using benzoyl peroxide as initiator. The composites are evaluated by FTIR, X-ray diffraction, mechanical properties, UV analysis, scanning electron microscope, polarizing light microscope and thermo-gravimetric analysis. Variation in properties is an inherent drawback of natural fibers, for which this MCDM technique is very effective to decipher, the biocomposite with optimum properties. It has been found that when the bagasse fiber is treated with 3.5 % of sodium chlorite solution, it can produce biocomposite with PMMA. It has been observed that, cellulose grafting takes place in the PMMA chain in presence of benzoyl peroxide. Further the work has been extended with loading variation of the said cellulose fibers and 1.5 % loading has been found as the best. The novelty of the work lies in the fact that these evaluations have been substantiated by Multi-Criteria Decision Making (MCDM) technique involving ENTROPY and TOPSIS approach and successfully selected 1.5 wt % loading to fabricate the optimum biocomposite. This composite exhibited around 13.5 % biodegradation within 90 days. This film can find application in packaging field.

Bright Nanocomposites based on Quantum Dot‐Initiated Photocatalysis

Integrating quantum dots (QDs) into polymer matrix to form nanocomposites without compromising the QD photoluminescence (PL) is crucial to emerging QD light‐emitting and solar energy conversion fields. However, the most widely‐used bulk polymerization technique, where monomers serve as the QD solvent, usually leads to QD PL quenching caused by radical initiators. Here we demonstrate high‐brightness nanocomposites with near‐unity PL quantum yield (QY), through a novel QDs‐catalyzed (‐initiated) bulk polymerization without using any radical initiators. Different from previous reports where QDs were designed as photo‐sensitizers/catalysts (always with cocatalysts) and hence non‐emissive in catalytic conditions, our QDs combine high brightness with highly effective catalysis, a combination that was previously considered to be hardly possible. In our case, apart from emitting light (at a large probability), the photoexcited QDs act as ‘overall reaction’ catalysts by simultaneously employing photoexcited electrons and holes to produce active radicals without the need of any sacrificial agents. These active radicals, though with a small amount, are sufficient to initiate effective chain reaction‐dominated bulk polymerization, eliminating the requirement of extra radical initiators. This study provides new insights for understanding and development of QDs for energy applications.

Bright Nanocomposites based on Quantum Dot-Initiated Photocatalysis.

Integrating quantum dots (QDs) into polymer matrix to form nanocomposites without compromising the QD photoluminescence (PL) is crucial to emerging QD light-emitting and solar energy conversion fields. However, the most widely-used bulk polymerization technique, where monomers serve as the QD solvent, usually leads to QD PL quenching caused by radical initiators. Here we demonstrate high-brightness nanocomposites with near-unity PL quantum yield (QY), through a novel QDs-catalyzed (-initiated) bulk polymerization without using any radical initiators. Different from previous reports where QDs were designed as photo-sensitizers/catalysts (always with cocatalysts) and hence non-emissive in catalytic conditions, our QDs combine high brightness with highly effective catalysis, a combination that was previously considered to be hardly possible. In our case, apart from emitting light (at a large probability), the photoexcited QDs act as 'overall reaction' catalysts by simultaneously employing photoexcited electrons and holes to produce active radicals without the need of any sacrificial agents. These active radicals, though with a small amount, are sufficient to initiate effective chain reaction-dominated bulk polymerization, eliminating the requirement of extra radical initiators. This study provides new insights for understanding and development of QDs for energy applications.

Kinetics and scale inhibition application studies towards bulk and RAFT copolymerization of maleic anhydride and acrylic acid

Poly(maleic anhydride) (PMA) is commonly reckoned as a better water scale inhibitor than poly(acrylic acid) (PAA) since each maleic anhydride unit can supply two carboxylic acid groups. However, pure PMA is difficult to achieve because the steric effect of its monomer MA. Herein, we synthesize copoly(MA-AA) copolymer by bulk polymerization method (bulk-copoly(MA-AA)), which avoids the use of any solvents which have to be removed afterwards. In addition, we also synthesize copoly(MA-AA) by reversible addition-fragmentation chain transfer (RAFT) polymerization method to afford RAFT-copoly(MA-AA) with low polydispersity index (PDI) less than 1.2, and the performance of RAFT-copoly(MA-AA) in water scale inhibition is more excellent relative to bulk-copoly(MA-AA). We also synthesize other copoly(MA-AA) copolymers by varying the molar ratio of MA to AA to study the polymerization mechanism. Through the static scale inhibition experiment, it is concluded that when the concentration of copoly(MA-AA) is 80 mg/L, the scale inhibition performance of RAFT-copoly(MA-AA) can reach 96.50 % which is the best among the control samples. It is also found that only 1:1 alternating copolymerization of MA and AA could be achieved as demonstrated by 1H nuclear magnetic resonance spectra of the copolymers, evidencing the strong steric hindrance of MA for its homo-polymerization.

Selective Methylation of Cyclic Ether Towards Highly Elastic Solid Electrolyte Interphase for Silicon-based Anodes.

Silicon (Si)-based anodes offer high theoretical capacity for lithium-ion batteries but suffer from severe volume changes and continuous solid electrolyte interphase (SEI) degradation. Here, we address these challenges by selective methylation of 1,3-dioxolane (DOL), thus shifting the unstable bulk polymerization to controlled interfacial reactions and resulting in a highly elastic SEI. Comparative studies of 2-methyl-1,3-dioxolane (2MDOL) and 4-methyl-1,3-dioxolane (4MDOL) reveal that 4MDOL, with its larger ring strain and more stable radical intermediates due to hyperconjugation effect, promotes the formation of high-molecular-weight polymeric species at the electrode-electrolyte interface. This elastic, polymer-rich SEI effectively accommodates volume changes of Si and inhibits continuous side reactions. Our designed electrolyte enables Si-based anode to achieve 85.4% capacity retention after 400 cycles at 0.5 C without additives, significantly outperforming conventional carbonate-based electrolytes. Full cells also demonstrate stable long-term cycling. This work provides new insights into molecular-level electrolyte design for high-performance Si anodes, offering a promising pathway toward next-generation lithium-ion batteries with enhanced energy density and longevity.

Microwave-assisted supramolecular double crosslinked chitosan-based molecularly imprinted polymer for synergistic recognition and selective recovery of Cd(II) and As(V) from water: Performance and mechanistic insights

A novel model of the sustainable double crosslinked molecularly imprinted polymer (D-Crosslinked MIP) represented as a supramolecular imprinted polymer was synthesized via the bulk polymerization method. The primary crosslinking was fabricated using biomacromolecule chitosan as a functional monomer and glutaraldehyde as a crosslinker. The primary crosslinked was subjected to dynamic interactions in a secondary crosslinking by binding Al2O3-NPs and TiO2-NPs, forming the supramolecular D-Crosslinked-MIP. The dually crosslinked formed from combining three distinct crosslinkers in one system for the interaction with As(V) and Cd(II). A microwave was employed to evaluate the performance of the designed material in selectivity and extraction of metal ions from water. The FT-IR, XRD, TG/DTA, SEM-EDX, TEM, and XPS were used to verify the characteristics of (D-nano-Al2O3@Crosslinked Chitosan@D-nano-TiO2). The type of solvents, selectivity, interferences, microwave-contact time, pH, temperatures, concentrations, and regeneration were investigated. By using the D-Crosslinked-MIP, at 15 s, Cd(II) revealed a recovery capacity of 99.03 %, Qmax 862.07 mg/g, while As(V) demonstrated a recovery capacity of 99.06 %, Qmax 850.75 mg/g. The D-Crosslinked-MIP exhibited BETs of 69.01 m2/g with a pore volume of 0.2340 cm3/g owing to polymeric crosslinking by metal oxide NPs. The kinetics, isotherm models, and mechanisms of dually crosslinking and extraction of toxic metals were discussed.

Selective Methylation of Cyclic Ether Towards Highly Elastic Solid Electrolyte Interphase for Silicon‐based Anodes

Silicon (Si)‐based anodes offer high theoretical capacity for lithium‐ion batteries but suffer from severe volume changes and continuous solid electrolyte interphase (SEI) degradation. Here, we address these challenges by selective methylation of 1,3‐dioxolane (DOL), thus shifting the unstable bulk polymerization to controlled interfacial reactions and resulting in a highly elastic SEI. Comparative studies of 2‐methyl‐1,3‐dioxolane (2MDOL) and 4‐methyl‐1,3‐dioxolane (4MDOL) reveal that 4MDOL, with its larger ring strain and more stable radical intermediates due to hyperconjugation effect, promotes the formation of high‐molecular‐weight polymeric species at the electrode‐electrolyte interface. This elastic, polymer‐rich SEI effectively accommodates volume changes of Si and inhibits continuous side reactions. Our designed electrolyte enables Si‐based anode to achieve 85.4% capacity retention after 400 cycles at 0.5 C without additives, significantly outperforming conventional carbonate‐based electrolytes. Full cells also demonstrate stable long‐term cycling. This work provides new insights into molecular‐level electrolyte design for high‐performance Si anodes, offering a promising pathway toward next‐generation lithium‐ion batteries with enhanced energy density and longevity.

Surface coupling of molecularly imprinted polymers as strategy to improve sulfamethoxazole removal from water by carbons produced from spent brewery grain

This work aims to assess the surface coupling of molecularly imprinted polymers (MIP) on carbon adsorbents produced from spent brewery grain, namely biochar (BC) and activated carbon (AC), as a strategy to improve selectivity and the adsorptive removal of the antibiotic sulfamethoxazole (SMX) from water. BC and AC were produced by microwave-assisted pyrolysis, and MIP was obtained by fast bulk polymerization. Two different methodologies were used for the molecular imprinting of BC and AC, the resulting materials being tested for SMX adsorption. Then, after selecting the most favourable molecular imprinting methodology, different mass ratios of MIP:BC or MIP:AC were used to produce and evaluate eight different materials. Molecular imprinting was shown to significantly improve the performance of BC for the target application, and one of the produced composites (MIP1-BC-s(1:3)) was selected for further kinetic and equilibrium studies and comparison with individual MIP and BC. The kinetic behaviour was properly described by both the pseudo-first and pseudo-second order models. Regarding equilibrium isotherms, they fitted the Freundlich and Langmuir models, with MIP1-BC-s(1:3) reaching a maximum adsorption capacity (qm) of 25 ± 1 μmol g-1, 19 % higher than BC. In comparison with other seven pharmaceuticals, the adsorption of SMX onto MIP1-BC-s(1:3) was remarkably higher, as for the specific recognition of this antibiotic by the coupled MIP. The pH study evidenced that SMX removal was higher under acidic conditions. Regeneration experiments showed that MIP1-BC-s(1:3) provided good adsorption performance, which was stable during five regeneration-reutilization cycles. Overall, this study has demonstrated that coupling with MIP may be a suitable strategy to improve the adsorption properties and performance of biochar for antibiotics removal from water, increasing its suitability for practical applications.

Changes in amorphous structure and reaction acceleration during bulk polymerization of methacrylates

Changes in amorphous structure and reaction acceleration during bulk polymerization of methacrylates

Ultrasound‐assisted liquid phase exfoliation of boron nitride nanosheets as fillers for polyacrylate pressure‐sensitive adhesives with enhanced thermal conductivity

AbstractHexagonal boron nitride (h‐BN) is widely used as a filler to improve the thermal conductivity of polymers due to the high thermal conductivity, electrical insulation, and chemical stability. However, the small lateral‐size and poor compatibility limit h‐BN's performances and applications in thermal management. Here, boron nitride nanosheets (BNNSs) were prepared by liquid‐phase ultrasonic exfoliation using isopropanol (IPA) as solvent. Specifically, the BNNSs obtained by ultrasonication for 8 h with an initial concentration of h‐BN of 8 mg/mL have the best exfoliation effect and a high yield of 19.8%, showing a large lateral‐size of 1–2 μm and an ultra‐thin thickness. Then, the resulting BNNSs can be modified by grafting silane coupling agent of KH560 (m‐BNNSs), their micromorphology and chemical composition are characterized by various microscopies and spectrometers. Subsequently, polyacrylate pressure‐sensitive adhesives (PSAs) composites are prepared using m‐BNNSs as a thermally conductive filler by UV bulk polymerization, their thermal conductivity can be greatly improved by 250% compared with that of pure PSAs. For comparison, the thermal conductivity of m‐BNNSs/PSAs composites with filler content of 25 wt% is as high as 0.4382 W/(m K), which is 1.6 times higher than that of h‐BN/PSAs composites. In addition, the incorporation of BNNSs will improve the thermal stability, hardness, and 180° peeling force of the PSAs composites, which will stimulate the practical application of PSAs materials.

Computer simulation‐guided template selection for a molecularly imprinted polymer for selective trifluralin adsorption

AbstractTo meet selective adsorption toward trifluralin, a novel molecularly imprinted polymer (MIP) was fabricated by the dummy template molecular imprinting technology. First, computational simulation was performed to select a suitable dummy template, 3,5‐dinitro‐4‐methylbenzoic acid (T1), based on the maximum basis set superposition error (BSSE)‐corrected binding interaction energy (ΔE) of the monomer N‐vinylpyrrolidone (NVP)‐T1 complex and its structural overlap with trifluralin. Then, the MIP was prepared via the bulk polymerization. The adsorption experiments showed the MIP exhibited a trifluralin adsorption capacity of 5.1 mg g−1, an imprinting factor (IF) of 2.2, and short adsorption equilibrium time of 5 min. The adsorption of trifluralin conformed to the Freundlich adsorption (R2 = 0.985) and pseudo‐second‐order model (R2 = 0.999). In addition, the MIP exhibited selectivity to trifluralin over other adsorbents, including structural analogs (pendimethalin and oryzalin), pesticide (carbendazim), and nitrocompounds (nitrofurantoin, furazolidone, and furaltadone), with the selectivity factor (β) in the range of 1.2–3.0, respectively. In trifluralin/oryzalin mixture, the IF toward oryzalin was still as high as 1.9. The removal rate of the MIP to trifluralin in environmental water samples ranged from 90.08% to 99.04%. This study provides theoretical and experimental insights for the preparation of MIP using dummy templates.

Development of a Molecularly Imprinted Polymer for Determination of Atenolol Based on Selective Solid Phase Extraction and Application in Pharmaceutical Samples

This paper demonstrates the synthesis and storage of molecular-imprinted polymers (MIP) at room temperature using bulk polymerization of atenolol (Ate), which is characterized by high sensitivity, low costs, and high stability. The research used 0.99:6:20 mmol ratios of template, monomer, and cross-linking agents for the polymerization in order to ensure an appropriate adsorption capacity. By making MIP for atenolol as Ate-MIP, which could be looked at with a UV-VIS spectrophotometer at 276 nm, Fourier- transform infrared spectroscopy (FT-IR), and scanning electron microscopy (SEM), a functional monomer of allyl chloride with cross-linking ethylene glycol dimethyl acrylate was made. Mass spectrometric (MS) detection may use allyl chloride to determine atenolol levels in pharmaceutical preparations. The GC/MS methods developed in this study are accurate, sensitive, and precise and can be easily applied to (NOVATEN/India and ATENOIOI/U.K.) tablets in pharmaceutical preparation. The elution process was applied to the template (Ate) from the Ate-MIP, which developed cavities, caused by using porogenic solutions of methanol, chloroform, and acetic acid (70:20:10, respectively). The maximum adsorption capacity of Ate-MIP was 2.9957 µmol/g, and the ratio of template to monomer was 1:1 in adherence to the Langmuir isotherm model. A solid-phase extraction (SPE) syringe packed with molecular imprinted polymers (MIPs) was used to selectively separate and pre-concentrate Ate from aqueous solutions and estimations of atenolol.

Regiocontrol of the Bulk Polymerization of Lysine Ethyl Ester by the Selection of Suitable Immobilized Enzyme Catalysts.

The development of a green and facile method for the controlled synthesis of functional polypeptides is desired for sustainable material applications. In this study, the regioselective synthesis of poly(l-lysine) (polyLys) via enzyme-catalyzed aminolysis was achieved by bulk polymerization of l-lysine ethyl ester (Lys-OEt) using immobilized Candida antarctica lipase Novozym 435 (IM-lipase) or trypsin (IM-trypsin). Structural characterization of the obtained polyLys revealed that IM-lipase resulted solely in ε-linked amide bond formation, whereas IM-trypsin predominantly provided α-linked polyLys. Optimization of the conditions for the bulk polymerization using immobilized enzymes resulted in high monomer conversion and a high degree of polymerization, with excellent regioselectivity. Molecular docking simulations revealed different binding conformations of Lys-OEt to the catalytic pockets of lipase and trypsin, which putatively resulted in different amino moieties being used for amide bond formation. The immobilized enzymes were recovered and recycled for bulk polymerization, and the initial activity was maintained in the case of IM-trypsin. The obtained α- and ε-linked polyLys products exhibited different degradability against proteolysis, demonstrating the possibility of versatile applications as sustainable materials. This enzymatic regioregular control enabled the synthesis of well-defined polypeptide-based materials with a diverging structural variety.

Enhancing foamability and flame‐retardancy of polylactic acid bead foams through inter‐beads bulk polymerization and continuous phase dispersion of LDHs

AbstractPoly (lactic acid) (PLA) bead foam has a promising application because of its renewable and naturally degradable nature. However, its processing is greatly limited by inherent shortcomings such as the complex polycrystals‐inducing strategy. Herein, we developed a strategy of bulk polymerization reaction of polyvinyl acetate (PVAc) to sinter PLA beads to prepare EPLA foams accompanied by supercritical CO2 foaming technology. In order to enhance the sintering behavior and flame‐retardancy of EPLA foams, two‐dimensional nanolayered double hydroxides (LDHs) were introduced and dispersed in the continuous phase of the sintering layers. The formation of unique dispersion of LDHs and sintering structure of PVAc generated substantial increase in the crystallinity, melt elasticity, and sintering strength of EPLA foams, which facilitated the growth and stabilization of cells. Thus, the cell‐density and expansion ratio could be increased to 8.62 × 106 cell/cm3 to 9.31‐fold, respectively. Moreover, the mechanical properties of the EPLA foams were improved. The tensile strength and the compression strength increased to 2.96 and 62.5 MPa. Additionally, with adding 7 wt.% LDH, the EPLA foam reached UL‐94 V‐0 rating with high limiting oxygen index value of 29.1% and char residue of 20.4%. This study provides a novel strategy for the preparation of flame‐retardant EPLA foams with low density, three dimensional complex shapes, as well as excellent mechanical properties.

Polymer Microspheres Carrying Schiff-Base Ligands for Metal Ion Adsorption Obtained via Pickering Emulsion Polymerization

Several traditional methods for producing polymer microparticle adsorbents for metal ions exist, such as bulk polymerization followed by milling and crushing the material to micron-size particles, precipitation from organic solvents, and suspension polymerization utilizing surfactants. Alternative methods that are easily scalable and are environmentally friendly are in high demand. This study employs Pickering Emulsion Polymerization Technology (PEmPTech) to synthesize nanostructured polymer microspheres that incorporate Schiff-base ligands, which can be utilized for metal ion adsorption, and specifically Cu(II) ions. Our innovative approach makes use of nanoparticle-stabilized, surfactant-free emulsions/suspensions, enabling the straightforward production of ligand-bearing microspheres while allowing for the precise modulation of the polymer matrix chemistry to maximize adsorption capacities. Through this method, we demonstrate notable enhancements in Cu(II) ion adsorption, which correlates with both the polarity of the monomers used and the concentration of Schiff-base ligands within the microspheres. Notably, our results offer insights into the structure–activity relationships essential for designing tailored adsorbents. This work provides a scalable method to produce high-performance adsorbents and also contributes to sustainable methodologies by excluding harmful surfactants and solvents.

الاستخلاص الانتقائي للكليميبيرايد في المستحضرات الصيدلانية وفي مصل الانسان عن طريق تقنية MIP-SPE المركبة

This paper demonstrates that the synthesizing and storage of molecular-imprinted polymers (MIP) at room temperature using bulk polymerisation of Glimepiride (Glim.) is characterized by high sensitivity, reduced costs, increased stability, and extended life. The research used 1:15:20 mmol ratios of template, monomer and cross-linking agents for the polymerisation in order to ensure an appropriate adsorption capacity. Benzoyl peroxide BPO was employed as the initiator for the functional monomer Allyl chloride C3H5Cl , cross-linked with Ethylene glycol dimethacrylate EGDMA C10H14O4, thereby creating MIP for Glimepiride (Glim-MIP) that could be characterised with UV-Visible Spectrophotometry at 274.5nm, for pharmaceutical drugs. Fourier-transform infrared spectroscopy (FTIR) and Scanning electron microscopy (SEM) was used for the human serum. The elution process that was applied to the template (Glim.) from the Glim-MIP created cavities that were caused by the porogenic mixture solvents that were created from (acetic acid, methanol) 1:9 respectively, successfully removed by repeated washing for 20 hours, the polymer was dried at room temperature. The maximum adsorption capacity was 11.7797 µmol/g using (0.1) g weight of Glim-MIP. which adhered to the Langmuir isotherm model. A solid-phase extraction (SPE) syringe packed with molecular imprinted polymers (MIPs) was employed to selectively separate and pre-concentrate the Glimepiride in multiple pharmaceutical drugs from several sources. The human serum was based on the use of deionized water to dilute the serum, followed by heating of the serum with methanol. Subsequently, few drops of 1N hydrochloric acid were applied to detect Glimepiride at UV region 274.5 nm by applying the standard addition method.

Enhancement in Sensitivity and Selectivity of Electrochemical Technique with CuO/g-C3N4 Nanocomposite Combined with Molecularly Imprinted Polymer for Melamine Detection.

This study focused on enhancing the sensitivity and selectivity to detect melamine by utilizing a photoelectrochemical method. This was achieved by combining a melamine-imprinted polymer with a CuO/g-C3N4 nanocomposite, which was synthesized through chemical precipitation and calcination. The resulting nanocomposite exhibits improved carrier mobility and photoelectrochemical properties. A molecularly imprinted receptor for selective detection was created through bulk polymerization with methacrylic acid and a melamine template. The characterization of the nanocomposite was performed using X-ray photoelectron spectroscopy for the chemical oxidation state, X-ray diffraction patterns for the crystalline structure, and ultraviolet/visible/near-infrared spectroscopy for optical properties. The CuO/g-C3N4 nanocomposite exhibits photoactivity under visible light. The modified electrode, incorporating the CuO/g-C3N4 nanocomposite and melamine-imprinted polymer, demonstrates a linear detection range of 2.5 to 50 nM, a sensitivity of 4.172 nA/nM for melamine, and a low detection limit of 0.42 nM. It shows good reproducibility and high selectivity to melamine, proving effective against interferences and real samples, showcasing the benefits of the molecularly imprinted polymer.