Home About us Contact
|
Home About us Contact | ||
|
|
||
Dimethacrylate
Kinds of Dimethacrylate Selected AbstractsA Biomimetic Potentiometric Sensor Using Molecularly Imprinted Polymer for the Cetirizine Assay in Tablets and Biological FluidsELECTROANALYSIS, Issue 18 2008Mehran Javanbakht Abstract Despite the increasing number of applications of molecularly imprinted polymers (MIPs) in analytical chemistry, the construction of a biomimetic potentiometric sensor remains still challenging. In this work, a biomimetic potentiometric sensor, based on a non-covalent imprinted polymer was fabricated for the recognition and determination of cetirizine. The MIP was synthesized by precipitation polymerization, using cetirizine dihydrochloride as a template molecule, methacrylic acid (MAA) as a functional monomer and ethylene glycol dimethacrylate (EGDMA) as a cross linking agent. The sensor showed high selectivity and a sensitive response to the template in aqueous system. The MIP-modified electrode exhibited Nernstian response (28.0±0.9 mV/decade) in a wide concentration range of 1.0×10,6 to 1.0×10,2 M with a lower detection limit of 7.0×10,7 M. The electrode has response time of ca. 20,s, high performance, high sensitivity, and good long term stability (more than 5,months). The method was satisfactory and used to the cetirizine assay in tablets and biological fluids. [source] Multi-walled carbon nanotube composites with polyacrylate prepared for open-tubular capillary electrochromatographyELECTROPHORESIS, Issue 19 2010Jian-Lian Chen Abstract A new phase containing immobilized carbon nanotubes (CNTs) was synthesized by in situ polymerization of acid-treated multi-walled CNTs using butylmethacrylate (BMA) as the monomer and ethylene dimethacrylate as the crosslinker on a silanized capillary, forming a porous-layered open-tubular column for CEC. Incorporation of CNT nanomaterials into a polymer matrix could increase the phase ratio and take advantage of the easy preparation of an OT-CEC column. The completed BMA-CNT column was characterized by SEM, ATR-IR, and EOF measurements, varying the pH and the added volume organic modifier. In the multi-walled CNTs structure, carboxylate groups were the major ionizable ligands on the phase surface exerting the EOF having electroosmotic mobility, 4.0×104,cm2,V,1,S,1, in the phosphate buffer at pH 2.8 and RSD values (n=5), 3.2, 4.1, and 4.3%, for three replicate capillaries at pH 7.6. Application of the BMA-CNT column in CEC separations of various samples, including nucleobases, nucleosides, flavonoids, and phenolic acids, proved satisfactory upon optimization of the running buffers. Their optima were found in the borate buffers at pH 9.0/50,mM, pH 9.5/10,mM/50% v/v ACN, and pH 9.5/30,mM/10% v/v methanol, respectively. The separations could also be used to assess the relative contributions of electrophoresis and chromatography to the CEC mechanism by calculating the corresponding velocity and retention factors. Discussions about interactions between the probe solutes and the bonded phase included the ,,, interactions, electrostatic repulsion, and hydrogen bonding. Furthermore, a reversed-phase mode was discovered to be involved in the chromatographic retention. [source] Assay of vitamin B in urine by capillary electrochromatography with methacrylate-based monolithic columnELECTROPHORESIS, Issue 19 2010Xiaoyi Wei Abstract A novel and simple method for the separation of major vitamin B analytes, such as thiamine, riboflavin, nicotinamide, vitamin B4, pyridoxine, has been developed by CEC using the monolithic column. It has been found that the baseline separation of the five analytes could be achieved with 5.0,mM phosphate buffer at pH 4.0. Compared with the open-tubular capillary and the bared capillary columns, the poly(butylmethacrylate-co-ethylene glycol dimethacrylate) monolithic capillary could exhibit the best resolution in the analysis. Then the method was validated and the linear calibration ranges were obtained with correlation coefficients more than 0.997. The precision and the recovery were also investigated and showed a good result. Furthermore, the proposed method was successfully applied to assay the concentration of vitamin B analytes and the metabolic situation in human urine samples. [source] Preparation and characterization of a molecularly imprinted monolithic column for pressure-assisted CEC separation of nitroimidazole drugsELECTROPHORESIS, Issue 16 2010Sulan Liao Abstract A polymethacrylate-based molecularly imprinted monolithic column bearing mixed functional monomers, using non-covalent imprinting approach, was designed for the rapid separation of nitroimidazole compounds. The new monolithic column has been prepared via simple in situ polymerization of 2-hydroxyethyl methacrylate, dimethylaminoethyl methacrylate and ethylene dimethacrylate, using (S)-ornidazole ((S)-ONZ) as template in a binary porogenic mixture consisting of toluene and dodecanol. The composition of the polymerization mixture was systematically altered and optimized by altering the amount of monomers as well as the composition of the porogenic solvent. The column performance was evaluated in pressure-assisted CEC mode. Separation conditions such as pH, voltage, amount of organic modifier and salt concentration were studied. The optimized monolithic column resulted in excellent separation of a group of structurally related nitroimidazole drugs within 10,min in isocratic elution condition. Column efficiencies of 99,000, 80,000, 103,000, 60,000 and 99,000,plates/m were obtained for metronidazole, secnidazole, ronidazole, tinidazole and dimetridazole, respectively. Parallel experiments were carried out using molecularly imprinted and non-imprinted capillary columns. The separation might be the result of combined effects including hydrophobic, hydrogen bonding and the imprinting cavities on the (S)-ONZ-imprinted monolithic column. [source] Parameters governing reproducibility of flow properties of porous monoliths photopatterned within microfluidic channelsELECTROPHORESIS, Issue 14 2010Mei He Abstract We report the patternability as well as the reproducibility and stability of flow resistance of polymer monolithic beds photopatterned within microfluidic channels as a function of initial reagent composition and preparation conditions. 2-Hydroxyethyl methacrylate and ethylene dimethacrylate-based polymer monoliths were selectively photopatterned within microchannels and their flow resistance was evaluated using a photobleaching, TOF linear flow rate measurement method developed in our lab. This measurement technique was found to be significantly more informative for columns formed in microfluidic channels compared with bulk monolith characterization by mercury intrusion porosimetry. 1-Octanol was determined to provide sharp bed edge formation and relatively low flow resistance by photopatterning relative to other porogenic solvents. Compared with literature formulations which did not achieve good flow stability and reproducibility from batch to batch, using 2-hydroxyethyl methacrylate, ethylene dimethacrylate and 1-octanol as porogenic solvents, less than 4% RSD was achieved in flow stability over 7 days for monoliths prepared with 60,80% crosslinker(monomer+crosslinker) ratio. Column-to-column variation of 5% RSD was obtained in this composition range. These results demonstrate that photopatterning of uniform polymer monolithic beds, which is critical for applications in multiplexed microfluidic systems, requires careful attention to the parameters that affect reproducibility, specifically the porogenic solvent choice and the crosslinker to monomer ratio. [source] Preparation and evaluation of the highly cross-linked poly(1-hexadecane-co-trimethylolpropane trimethacrylate) monolithic column for capillary electrochromatographyELECTROPHORESIS, Issue 20 2009Minghua Lu Abstract In this paper, a novel highly cross-linked porous monolithic stationary phase having a long alkyl chain ligand (C16) was introduced and evaluated in CEC. The monolithic stationary phase was prepared by in situ copolymerization of 1-hexadecene, trimethylolpropane trimethacrylate, and 2-acrylamido-2-methyl-1-propanesulfonic acid (AMPS) in the presence of ternary porogenic solvent (cyclohexanol/1,4-butanediol/water). In preparing monoliths, the ternary cross-linker trimethylolpropane trimethacrylate was usually applied to preparing molecularly imprinted polymers or molecularly imprinted solid-phase extraction, instead of binary cross-linker ethylene dimethacrylate. 1-Hexadecene was introduced to provide the non-polar sites (C16) for chromatographic retention, while AMPS was used to generate the EOF for transporting the mobile phase through the monolithic capillary. Monolithic columns were prepared by optimizing proportion of porogenic solvent and AMPS content in the polymerization solution as well as the cross-linkers. The monolithic stationary phases could generate a strong and stable EOF in various pH values and exhibit an RP-chromatographic behavior for neutral compounds. For charged compounds, the separation was mainly based on the association of hydrophobic, electrostatic and electrophoretic interaction. [source] Methacrylate-based monolithic column with mixed-mode hydrophilic interaction/strong cation-exchange stationary phase for capillary liquid chromatography and pressure-assisted CECELECTROPHORESIS, Issue 19 2008Jian Lin Abstract A novel porous polymethacrylate-based monolithic column by in situ copolymerization of 3-sulfopropyl methacrylate (SPMA) and pentaerythritol triacrylate in a binary porogenic solvent consisting of cyclohexanol/ethylene glycol was prepared. The monolith possessed in their structures bonded sulfonate groups and hydroxyl groups and was evaluated as a hydrophilic interaction and strong cation-exchange stationary phases in capillary liquid chromatography (cLC) and pressure-assisted CEC using small polar neutral and charged solutes. While the SPMA was introduced as multifunctional monomer, the pentaerythritol triacrylate was used to replace ethylene glycol dimethacrylate as cross-linker with much more hydrophilicity due to a hydroxyl sub-layer. The different characterization of monolithic stationary phases were specially designed and easily prepared by altering the amount of SPMA in the polymerization solution as well as the composition of the porogenic solvent for cLC and pressure-assisted CEC. The resulting monolith showed the different trends about the effect of the permeabilities on efficiency in the pressure-assisted CEC and cLC modes. A typical hydrophilic interaction chromatography mechanism was observed at higher organic solvent content (ACN%>70%) for polar neutral analytes. For polar charged analytes, both hydrophilic interaction and electrostatic interaction contributed to their retention. Therefore, for charged analytes, selectivity can be readily manipulated by changing the composition of the mobile phase (e.g., pH, ionic strength and organic modifier). With the optimized monolithic column, high plate counts reaching greater than 170,000,plates/m for pressure-assisted CEC and 105,000 plates/m for cLC were easily obtained, respectively. [source] Confinement effects on the morphology of photopatterned porous polymer monoliths for capillary and microchip electrophoresis of proteinsELECTROPHORESIS, Issue 14 2008Mei He Abstract We find that the morphology of porous polymer monoliths photopatterned within capillaries and microchannels is substantially influenced by the dimensions of confinement. Porous polymer monoliths were prepared by UV-initiated free-radical polymerization using either the hydrophilic or hydrophobic monomers 2-hydroxyethyl methacrylate or butyl methacrylate, cross-linker ethylene dimethacrylate and different porogenic solvents to produce bulk pore diameters between 3.2 and 0.4,µm. The extent of deformation from the bulk porous structure under confinement strongly depends on the ratio of characteristic length of the confined space to the monolith pore size. The effects are similar in cylindrical capillaries and D-shaped microfluidic channels. Bulk-like porosity is observed for a confinement dimension to pore size ratio >10, and significant deviation is observed for a ratio <5. At the extreme limit of deformation a smooth polymer layer ,300 nm thick is formed on the surface of the capillary or microchannel. Surface tension or wetting also plays a role, with greater wetting enhancing deformation of the bulk structure. The films created by extreme deformation provide a rapid and effective strategy to create robust wall coatings, with the ability to photograft various surface chemistries onto the coating. This approach is demonstrated through cationic films used for electroosmotic flow control and neutral hydrophilic coatings for electrophoresis of proteins. [source] Macrocyclic polyamine-modified poly(glycidyl methacrylate- co -ethylene dimethacrylate) monolith for capillary electrochromatographyELECTROPHORESIS, Issue 11 2008Yun Tian Abstract 1,4,10,13,16-Pentaazatricycloheneicosane-9,17-dione (macrocyclic polyamine)-modified polymer-based monolithic column for CEC was prepared by ring opening reaction of epoxide groups from poly(glycidyl methacrylate- co -ethylene dimethacrylate) (GMA- co -EDMA) monolith with macrocyclic polyamine. Conditions such as reaction time and concentration of macrocyclic polyamine for the modification reaction were optimized to generate substantial EOF and enough chromatographic interactions. Anodic EOF was observed in the pH range of 2.0,8.0 studied due to the protonation of macrcyclic polyamine at the surface of the monolith. Morphology of the monolithic column was examined by SEM and the incorporation of macrocyclic polyamine to the poly(GMA- co -EDMA) monolith was characterized by infrared (IR) spectra. Successful separation of inorganic anions, isomeric benzenediols, and benzoic acid derivatives on the monolithic column was achieved for CEC. In addition to hydrophobic interaction, hydrogen bonding and electrostatic interaction played a significant role in the separation process. [source] CEC separation of heterocyclic amines using methacrylate monolithic columnsELECTROPHORESIS, Issue 11 2007Elena Barceló-Barrachina Abstract Two methacrylate-based monolithic columns, one with a negatively charged group (sulfonic group) and another with a new monomer N,N -dimethylamino ethyl acrylate (DMAEA), were prepared and tested for the separation of basic compounds by CEC. This new monolithic stationary phase was prepared by the in situ polymerization of DMAEA with butyl methacrylate and ethylene dimethacrylate, using a ternary porogenic solvent consisting of water, 1-propanol and 1,4-butanediol. The performance of this column was evaluated by means of the analysis of a family of heterocyclic amines. Separation conditions such as pH, amount of organic modifier, ionic strength and elution mode (normal or counterdirectional flow) were studied. At the optimal running electrolyte composition, and using the counterdirectional mode, symmetrical electrochromatographic peaks were obtained, with the number of theoretical plates up to 30,000 and a good resolution between closely related peaks. The 2-acrylamido-2-methyl-1-propane-sulfonic acid column was used for CEC-MS, taking advantage of the compatibility of its elution mode (normal flow) with the MS coupling. [source] Open-tubular capillary columns with a porous layer of monolithic polymer for highly efficient and fast separations in electrochromatographyELECTROPHORESIS, Issue 21 2006Sebastiaan Eeltink Abstract Open-tubular columns for CEC separations having inner-wall coated with a thin layer of porous monolithic polymer have been studied. A two-step process including (i),UV-initiated polymerization leading to a layer of porous poly(butyl methacrylate- co -ethylene dimethacrylate), and (ii),UV-initiated grafting of ionizable monomers appear to be well suited for the preparation of these columns. The thickness of the porous polymer layer is controlled by the percentage of monomers in the polymerization mixture and/or length of the irradiation time. The layer thickness significantly affects retention, efficiency, and resolution in open-tubular CEC. Under optimized conditions, column efficiencies up to 400,000 plates/m can be achieved. Use of higher temperature and application of pressure enables a significant acceleration of the open-tubular CEC separations. [source] (S)-Ibuprofen-imprinted polymers incorporating ,-methacryloxypropyl-trimethoxysilane for CEC separation of ibuprofen enantiomersELECTROPHORESIS, Issue 21 2006Qi-Liang Deng Abstract In this report, a novel preparation method of molecularly imprinted polymers (MIPs) for CEC was developed. Molecularly imprinted monolithic columns for (S)-ibuprofen were prepared and evaluated, in which charged entities responsible for establishing EOF have been derived from ,-methacryloxypropyltrimethoxysilane (,-MAPS), which was hydrolyzed following copolymerization with 4-vinylpyridine (4-VPY) and ethylene glycol dimethacrylate,(EDMA). The EOF and molecular recognition of the stationary phase were investigated in aqueous and nonaqueous media, respectively. The experimental results indicated that the material showed a reasonably stable EOF and the prepared separation materials were capable of separating racemic ibuprofen, a task that could not be accomplished by MIPs prepared in parallel, using methacrylic acid (MAA) as a functional monomer. The efficiency at pH,3.2 for the first-eluted enantiomer and the last-eluted enantiomer (the imprinted analyte) were 128,700 and 2100,plates/m, respectively. [source] Capillary electrochromatography with zwitterionic stationary phase on the lysine-bonded poly(glycidyl methacrylate- co -ethylene dimethacrylate) monolithic capillary columnELECTROPHORESIS, Issue 12 2006Xiaoli Dong Abstract A polymer-based neutral monolithic capillary column was prepared by radical polymerization of glycidyl methacrylate and ethylene dimethacrylate in a 100,,m id fused-silica capillary, and the prepared monolithic column was subsequently modified based on a ring opening reaction of epoxide groups with 1,M,lysine in solution (pH,8.0) at 75°C for 10,h to produce a lysine chemically bonded stationary phases in capillary column. The ring opening reaction conditions were optimized so that the column could generate substantial EOF. Due to the zwitterionic functional groups of the lysine covalently bonded on the polymer monolithic rod, the prepared column can generate cathodic and anodic EOF by varying the pH values of running buffer during CEC separation. EOF reached the maximum of ,2.0×10,8,m2v,1s,1 and 2.6×10,8,m2v,1s,1 with pH of the running buffer of 2.25 and 10, respectively. As a consequence, neutral compounds, ionic solutes such as phenols, aromatic acids, anilines, and basic pharmaceuticals were all successfully separated on the column by CEC. Hydrophobic interaction is responsible for separation of neutral analytes. In addition, the electrostatic and hydrophobic interaction and the electrophoretic migration play a significant role in separation of the ionic or ionizable analytes. [source] Poly(methacrylic acid-ethylene glycol dimethacrylate) monolith in-tube solid-phase microextraction applied to simultaneous analysis of some amphetamine derivatives in urine by capillary zone electrophoresisELECTROPHORESIS, Issue 16 2005Fang Wei Abstract A method based on in-tube solid-phase microextraction and capillary zone electrophoresis (CZE) was proposed for simultaneously determining four amphetamines (amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine, and 3,4-methylenedioxymethamphetamine) in urine. A poly(methacrylic acid-ethylene glycol dimethacrylate) monolithic capillary column, which can provide sufficient extraction efficiency, was introduced for the extraction of amphetamines from urine samples. The hydrophobic main chains and acidic pendant groups of the monolithic column make it a superior material for extraction of basic analytes from aqueous matrix. After extraction, the samples were analyzed by CZE. The best separation was achieved using a buffer composed of 0.1,M disodium hydrogen phosphate (adjusted to pH,4.5 with 1,M hydrochloric acid) and 20% methanol v/v, with a temperature and voltage of 25°C and 20,kV, respectively. By applying electrokinetic injection with field-amplified sample stacking, detection limits of 25,34,µg/L were achieved. Excellent method of reproducibility was found over a linear range of 0.1,5,mg/L. Determination of these analytes from abusers' urine sample was also demonstrated. [source] On-line concentration of peptides and proteins with the hyphenation of polymer monolithic immobilized metal affinity chromatography and capillary electrophoresisELECTROPHORESIS, Issue 11 2005Lingyi Zhang Abstract An iminodiacetic acid (IDA)-type adsorbent is prepared at the one end of a capillary by covalently bonding IDA to the monolithic rods of macroporous poly(glycidyl methacrylate,co -ethylene dimethacrylate). Cu(II) is later introduced to the support via the interaction with IDA. By this means, polymer monolithic immobilized metal affinity chromatography (IMAC) materials are prepared. With such a column, IMAC for on-line concentration and capillary electrophoresis (CE) for the subsequent analysis are hyphenated for the analysis of peptides and proteins. The reproducibility of such a column has been proved good with relative standard deviations (RSDs) of dead time of less than 5% for injection-to-injection and 12% for column-to-column (n = 3). Through application on the analysis of standard peptides and real protein samples, such a technique has shown promising in proteome study. [source] Macroporous monolithic chiral stationary phases for capillary electrochromatography: New chiral monomer derived from cinchona alkaloid with enhanced enantioselectivityELECTROPHORESIS, Issue 17 2003Michael Lämmerhofer Abstract A new chiral monomer derived from cinchona alkaloid, namely O -9-(tert -butylcarbamoyl)-11-[2-(methacryloyloxy)ethylthio]-10,11-dihydroquinine 1, was employed for the preparation of enantioselective monolithic capillary columns by an in situ copolymerization with 2-hydroxyethyl methacrylate 2 (HEMA), ethylene dimethacrylate 3 (EDMA) in the presence of cyclohexanol and 1-dodecanol as porogens (UV or thermal initiation of azobisisobutyronitrile (AIBN) as radical initiator). The porous properties and the electrochromatographic behavior of the new chiral monoliths were comparatively evaluated with previously described analogs obtained from O -9-[2-(methacryloyloxy)ethylcarbamoyl]-10,11-dihydroquinidine 4 as chiral monomer. Despite close structural and physicochemical similarities of the both chiral monomers, the pore distribution profiles of the resulting monoliths were shifted typically towards larger pore diameters with the new monomer 1. Once more, it was confirmed that a low cross-linking (10 wt% related to total monomers) and a pore diameter of about 1 ,m in the dry state provides the best electrochromatographic efficiency as a result of lower resistance to mass transfer (smaller C-term contribution to peak broadening) and more homogeneous flow profile (smaller A-term). Most importantly, as expected the new poly(1 - co -HEMA- co -EDMA) monoliths showed enhanced enantioselectivities and in addition faster separations as compared to poly(4 - co -HEMA- co -EDMA) analogs, which represents a significant improvement. Further, the elution order was reversed owing to the pseudoenantiomeric behavior of quinine- and quinidine-derived monomers. Fluorescence-labeled 9-fluorenylmethoxycarbonyl (FMOC), dansyl (DNS), 7-dimethylaminosulfonyl-1,3,2-benzoxadiazol-4-yl (DBD), carbazole-9-carbonyl (CC) amino acids could be separated with resolution values between 2 and 4 (with efficiencies typically between 100,000 and 200,000 plates/m) and fluorescence detection (variable wavelength fluorescence detector in-line with UV) yielding routinely a gain in detection sensitivities up to two orders of magnitude without specific optimization of the conditions with regards to fluorescence efficiency. [source] Smart Hydrogels Co-switched by Hydrogen Bonds and ,,, Stacking for Continuously Regulated Controlled-Release SystemADVANCED FUNCTIONAL MATERIALS, Issue 4 2010Fang Li Abstract A series of hydrogels with continuously regulatable release behavior can be achieved by incorporating hydrogen bonding and ,,, stacking co-switches in polymers. A poly(nitrophenyl methacrylate- co -methacrylic acid) hydrogel (NPMAAHG) for control over drug release is fabricated by copolymerizing 4-nitrophenyl methacrylate and methacrylic acid using ethylene glycol dimethacrylate as a crosslinker. The carboxylic acid groups and nitrylphenyl groups form hydrogen bonds and ,,, stacking interactions, respectively, which act as switches to control the release of guest molecules from the polymers. As revealed by the simulated gastrointestinal tract drug release experiments, the as-synthesized NPMAAHG hydrogels can be regulated to release only 4.7% of drugs after 3,h in a simulated stomach and nearly 92.6% within 43,h in the whole digestive tract. The relation between the release kinetics and structures and the mechanism of the smart release control are analyzed in terms of diffusion exponent, swelling interface number, drug diffusion coefficient, and velocity of the swelling interface in detail. The results reveal that the release of guest molecules from the hydrogels can be continuously regulated for systemic administration by controlling the ratio of the hydrophilic hydrogen bonds and the hydrophobic ,,, stacking switches. [source] CdS-Nanoparticle/Polymer Composite Shells Grown on Silica Nanospheres by Atom-Transfer Radical Polymerization,ADVANCED FUNCTIONAL MATERIALS, Issue 3 2005T. Cui Abstract In this paper we describe the combined use of surface-initiated atom transfer radical polymerization (ATRP) and a gas/solid reaction in the direct preparation of CdS-nanoparticle/block-copolymer composite shells on silica nanospheres. The block copolymer, consisting of poly(cadmium dimethacrylate) (PCDMA) and poly(methyl methacrylate) (PMMA), is obtained by repeatedly performing the surface-initiated ATRP procedures in N,N -dimethylformamide (DMF) solution at room temperature, using cadmium dimethacrylate (CDMA) and methyl methacrylate (MMA) as the monomers. CdS nanoparticles with an average size of about 3,nm are generated in situ by exposing the silica nanospheres coated with block-copolymer shells to H2S gas. These synthetic core,shell nanospheres were characterized using transmission electron microscopy (TEM), dynamic light scattering (DLS), thermogravimetric analysis (TGA), diffuse reflectance UV-vis spectroscopy, X-ray photoelectron spectroscopy (XPS), and powder X-ray diffraction (XRD). These composite nanospheres exhibit strong red photoluminescence in the solid state at room temperature. [source] Preparation and Characteristics of Esculin-Imprinted PolymersHELVETICA CHIMICA ACTA, Issue 6 2007Guo-Song Wang Abstract Four molecularly imprinted polymers (MIPs) were prepared in MeOH with esculin (=6,7-dihydroxycoumarin 6-(, - D -glucopyranoside)=6-(, - D -glucopyranosyloxy)-7-hydroxy-2H -1-benzopyran-2-one) as the imprinted molecule, methacrylic acid (=2-methylprop-2-enoic acid; MAA), acrylamide (=prop-2-enamide; AM), 4-vinylpyridine (=4-ethenylpyridine; 4-VP), or 2-vinylpyridine (=2-ethenylpyridine; 2-VP) as the functional monomer, respectively, as well as ethylene glycol dimethacrylate (=2-methylprop-2-enoic acid ethane-1,2-diyl ester; EGDMA) as the cross-linking agent. The interaction between the template and the functional monomers was investigated by fluorescence and UV spectrophotometry, respectively, which revealed the presence of esculin/monomer complexes in the stoichiometric ratio 1,:,2 in the pre-polymerization mixture. The resultant polymers were studied in equilibrium binding experiments to evaluate the recognition ability and the binding capacity towards esculin. The results showed that MIP1, prepared with MAA as the functional monomer, exhibited advantageous characteristics of high binding capacity, optimal imprinting effect, and good selectivity towards esculin. The Scatchard analysis indicated that there are two types of binding sites in MIP1, and its binding parameters including the apparent maximum numbers of binding sites and the dissociation constants were calculated. Finally, by packing an SPE column (SPE=solid-phase extraction) with MIP1, the esculin was separated and enriched successfully by this sorbent from samples of Cortex fraxini, and the average recovery was up to 74.7%. [source] Bioreactors Based on Monolith-Supported Ionic Liquid Phase for Enzyme Catalysis in Supercritical Carbon DioxideADVANCED SYNTHESIS & CATALYSIS (PREVIOUSLY: JOURNAL FUER PRAKTISCHE CHEMIE), Issue 7 2007Pedro Lozano Abstract Bioreactors with covalently supported ionic liquid phases (SILP) were prepared as polymeric monoliths based on styrene,divinylbenzene or 2-hydroxyethyl methacrylate,ethylene dimethacrylate, and with imidazolium units loadings ranging from 54.7 to 39.8,% wt IL per gram of polymer. The SILPs were able to absorb Candida antarctica lipase B (CALB), leading to highly efficient and robust heterogeneous biocatalysts. The bioreactors were prepared as macroporous monolithic mini-flow systems and tested for the continuous flow synthesis of citronellyl propionate in supercritical carbon dioxide (scCO2) by transesterification. The catalytic activity of these mini-flow-bioreactors remained practically unchanged for seven operational cycles of 5,h each in different supercritical conditions. The best results were obtained when the most hydrophobic monolith, M-SILP- 8 -CALB, was assayed at 80,°C and 10,MPa, reaching a total turnover number (TON) of 35.8×104 mol product/mol enzyme. The results substantially exceeded those obtained for packed-bed reactors with supported silica-CALB-Si-4 catalyst under the same experimental conditions. [source] Molecular imprinted solid-phase extraction of huperzine A from Huperzia SerrataJOURNAL OF APPLIED POLYMER SCIENCE, Issue 5 2009Guosong Wang Abstract On the basis of the non-covalent interaction between template and monomer, porous molecularly imprinted polymers (MIPs) were synthesized by a thermal-initiated polymerization method using huperzine A as template, acrylamide, or methacrylic acid as function monomer, ethylene glycol dimethacrylate as cross-linking agent. The interaction between template and functional monomers was studied by UV spectrophotometry, which showed a formation of huperzine A-monomer complexes with stoichiometric ratio of 1 : 2 in the pre-polymerized systems. The resultant MIP particles were tested in the equilibrium binding experiment to analyze their adsorption ability to huperzine A, and were characterized by Fourier Transform Infrared (FTIR) study. The recognition properties of MIP were estimated in solid-phase extraction by selecting four compounds (isolated from the Chinese herb Huperzia serrata) as substrates, and were compared with and prior to those of the NIP. High affinity and adsorption of MIP1 which was prepared in chloroform with huperzine A as imprinted molecule, and acrylamide (AM) as functional monomer, made an attractive application of MIP1 in separation processes. In final, using MIP1 solid-phase extraction micro-column, huperzine A was enriched and separated from the real extraction sample of Huperzia serrata. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009 [source] Synthesis, characterization, and antimicrobial properties of novel quaternary amine methacrylate copolymersJOURNAL OF APPLIED POLYMER SCIENCE, Issue 5 2008Supriya Punyani Abstract A novel amine methacrylate monomer trimethylolpropane trimethacrylate,piperazine,ethyleneglycol dimethacrylate (TMPTMA-PPZ-EGDMA) was synthesized by amination of trimethylolpropane trimethacrylate (TMPTMA) with excess of piperazine (PPZ) followed by reaction with ethyleneglycol dimethacrylate (EGDMA). Copolymerization of TMPTMA-PPZ-EGDMA with 2-hydroxyethyl methacrylate (HEMA) was carried out by free radical polymerization using ammonium persulfate (APS) and N,N,N,,N,-tetramethyl ethylenediamine (TEMED) as a redox initiator. The copolymers obtained were then quaternized with 1-iodooctane. The monomers were characterized by FTIR and 1H NMR spectral studies. The molecular weights and polydispersity values of the monomers were determined with gel permeation chromatography. Quaternized copolymers containing more than 20% amine methacrylate monomer showed microporosity in the range of 9.9,10.4 ,m. The antibacterial activity of the quaternized copolymers against Escherichia coli and Staphylococcus aureus was studied using UV,vis spectrophotometer and scanning electron microscopy. Quaternized copolymers showed broad-spectrum contact-killing antibacterial properties without releasing any active agent as checked by iodide selective ion meter. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008 [source] Water sorption kinetics in light-cured poly-HEMA and poly(HEMA- co -TEGDMA); determination of the self-diffusion coefficient by new iterative methodsJOURNAL OF APPLIED POLYMER SCIENCE, Issue 4 2007Irini D. Sideridou Abstract The present investigation is concerned with the determination of self-diffusion coefficient (D) of water in methacrylate-based biomaterials following Fickian sorption by two new methods: the Iterative and the Graphical methods. The D value is traditionally determined by means of the initial slope of the corresponding sorption curve and the so-called Stefan's approximation. The proposed methods using equations without approximations and data resulting from the whole sorption range reach to accurate values of D, even when the sorption curve does not present an initial linear portion. In addition to D, the Graphical method allows the extrapolation of the mass of the sorbed water at equilibrium (M,), even when the equilibrium specimen's mass fluctuates around its limited value (m,). The test of the proposed procedures by means of ideal and Monte Carlo simulated data revealed that these methods are fairly applicable. The obtained D values compared with those determined by means of the Stephan's method revealed that the proposed methods provide more accurate results. Finally, the proposed methods were successfully applied to the experimental determination of the diffusion coefficient of water (50°C) in the homopolymer of 2-hydroxyethyl methacrylate (HEMA) and in the copolymer of HEMA with triethylene glycol dimethacrylate (98/2 mol/mol). These polymers were prepared by light curing (, = 470 nm) at room temperature in presence of camphorquinone and N,N -dimethylaminoethyl methacrylate as initiator. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007 [source] Biporous polymeric beads fabricated by double emulsification for high-speed protein chromatographyJOURNAL OF APPLIED POLYMER SCIENCE, Issue 1 2007Guo-Yong Sun Abstract Rigid biporous beads (BiPB) were fabricated by double emulsification. An aqueous suspension of superfine calcium carbonate granules and organic solvent were used as porogenic agents to create superpores and micropores, respectively. The polymerization of monomers, glycidyl methacrylate, and ethylene glycol dimethacrylate was initiated with benzoin ethyl ether by ultraviolet irradiation. Modified with diethylamine (DEA), the BiPB were derivatized into an anion-exchange medium (which is denoted as DEA,BiPB). The DEA,BiPB with an average diameter of 46.3 ,m was characterized to possess two types of pores, that is, micropores (20,200 nm) and superpores (500,5300 nm). Flow hydrodynamic experiments showed that the DEA,BiPB column had a smaller backpressure than that of the conventional microporous beads column at a given flow rate. The static adsorption capacity of the DEA,BiPB was close to that of the DEA,MiPB for bovine serum albumin. However, frontal analysis demonstrated that the dynamic binding capacity of the DEA,BiPB column was two times higher than that of the DEA,MiPB at a flow rate of 1800 cm/h. Moreover, the purification of the molecular chaperone GroEL was carried out with the DEA,BiPB column at two flow rates (150 and 1500 cm/h). This showed that the GroEL purification was nearly the same at the two flow rates tested. These results indicate that the DEA,BiPB column is promising for high-speed protein chromatography. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 103: 17,23, 2007 [source] Effect of monomer composition on crystal growth by resin containing bioglassJOURNAL OF BIOMEDICAL MATERIALS RESEARCH, Issue 1 2010Masanori Hashimoto Abstract This study evaluated the effect of resin monomer composition on crystal growth at the interface between the resin/bioglass composites and water. Light-cured resin that contained 2-bis[4(2-hydroxy-3-methacryloyloxy-propyloxy)-phenyl], 2-hydroxyethyl methacrylate, and triethylene glycol dimethacrylate with different compositions were used. Resin/bioglass composites were prepared with 40 mass% bioglass and 60 mass% resin. The resin/bioglass composites were stored in deionized distilled water for 24 h (control group) or 3,12 months (experimental groups). After water storage, the disk surfaces were examined by light- and scanning electron microscopy. Chemical states of the crystals were analyzed by laser-Raman spectroscopy and micro-X-ray diffractometry. The microscopic analysis showed crystal on the resin disks surface after six months of water storage for hydrophilic resins. However, there was no crystal formation in the control and the experimental groups of specimens of hydrophobic resins. Raman analysis showed the chemical states of the crystals formed on the resin matrix and bioglass to be different. The micro-X-ray analysis of crystals on resin disks identified them to be calcium carbonate. This crystal formation occurred in water instead of simulated body fluid. In conclusion, the resin monomer compositions affected the ability to induce crystal growth on the surfaces of disks containing bioglass. © 2010 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 2010 [source] Solubility, salivary sorption and degree of conversion of dimethacrylate-based polymeric matrixesJOURNAL OF BIOMEDICAL MATERIALS RESEARCH, Issue 2 2008Luana Gonēalves Abstract This study investigated the relationship between the solubility, salivary sorption, and degree of conversion of dimethacrylate-based polymeric matrixes. Six polymeric matrixes produced by mixing bis-GMA, TEGDMA and UDMA dimethacrylate monomers were studied. Photoactivation was induced by camphoroquinone/ethyl N,N-dimethyl-4-aminobenzoate. The specimens were light-cured using an irradiance of 850 mW/cm2 for 20 s. The solubility and sorption (,g/mm3) were measured after immersion in artificial saliva (neutral pH) for 7 days. The degree of conversion (%) was obtained by using a FT-IR spectrometer equipped with an attenuated total reflectance crystal (ATR). The degree of conversion varied from 39.15 ± 6.30 to 65.57± 4.80, and was influenced by the viscosity of the monomers present in the polymeric matrixes. The solubility of polymeric matrixes varied between 13.64 ± 0.39 and 25.08 ± 0.83, and was strongly influenced by the degree of conversion (Pearson, r = ,0.9587, p < 0.01). No correlation was found between salivary sorption and the degree of conversion (p = 0.3918). Salivary sorption was only dependent on the chemical and physical structures of the monomers presented in the polymeric matrixes. © 2007 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 2008 [source] Sorption kinetics of ethanol/water solution by dimethacrylate-based dental resins and resin compositesJOURNAL OF BIOMEDICAL MATERIALS RESEARCH, Issue 1 2007Irini D. Sideridou Abstract In the present investigation the sorption,desorption kinetics of 75 vol % ethanol/water solution by dimethacrylate-based dental resins and resin composites was studied in detail. The resins examined were made by light-curing of bisphenol A glycol dimethacrylate (Bis-GMA), triethylene glycol dimethacrylate (TEGDMA), urethane dimethacrylate (UDMA), bisphenol A ethoxylated dimethacrylate (Bis-EMA), and mixtures of these monomers. The resin composites were prepared from two commercial light-cured restorative materials (Z100 MP and Filtek Z250), the resin matrix of which is based on copolymers of the above-mentioned monomers. Ethanol/water sorption/desorption was examined in both equilibrium and dynamic conditions in two adjacent sorption,desorption cycles. For all the materials studied, it was found that the amount of ethanol/water sorbed or desorbed was always larger than the corresponding one reported in literature in case of water immersion. It was also observed that the chemical structure of the monomers used for the preparation of the resins directly affects the amount of solvent sorbed or desorbed, as well as sorption kinetics, while desorption rate was nearly unaffected. In the case of composites studied, it seems that the sorption/desorption process is not influenced much by the presence of filler. Furthermore, diffusion coefficients calculated for the resins were larger than those of the composites and were always higher during desorption than during sorption. Finally, an interesting finding concerning the rate of ethanol/water sorption was that all resins and composites followed Fickian diffusion kinetics during almost the whole sorption curve; however, during desorption the experimental data were overestimated by the theoretical model. Instead, it was found that a dual diffusion,relaxation model was able to accurately predict experimental data during the whole desorption curve. Kinetic relaxation parameters, together with diffusion coefficients, are reported for all resins and composites. © 2006 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 2006 [source] Biocompatibility investigation and urea removal from blood by urease-immobilized HEMA incorporated poly(ethyleneglycol dimethacrylate) microbeadsJOURNAL OF BIOMEDICAL MATERIALS RESEARCH, Issue 1 2003F. Ayhan Abstract The biocompatibility of modified and urease-immobilized poly(ethyleneglycol dimethacrylate/2-hydroxyethylmetacrylate) [poly(EGDMA/HEMA)] microbeads was tested through blood compatibility tests. Twelve percent HEMA incorporated nonporous particles of 105,125 ,m were used in the research. Hydroxyl groups on microbeads were chemically modified by following a three-step procedure that is composed of activation, spacer-arm incorporation (hexamethylene diamine) and, finally, glutaraldehyde bounding. Enzyme urease was immobilized on microbead surfaces, and adsorption of blood proteins in serum and plasma, blood coagulation time, and leukocyte and platelet adhesion were tested. Incubation of 1.5 cc of biological fluid with 100 mg of urease-immobilized poly(EGDMA/HEMA) microbeads at room temperature shows that protein adsorption on surfaces occurs, but protein content after treatment was in the range of healthy people. Adsorbed albumin and total globulin amounts per gram of microbeads is much greater than fibrinogen. Immobilization of urease reduced the protein adsorption and blood coagulation times compared with those of modified microbeads. Prothrombin time (PT) was not altered much, whereas poly(EGDMA/HEMA) microbeads induced a significant increase of activated partial thromboplastin time (APTT). The platelet and leukocyte adhesion slightly increased with the modification of poly(EGDMA/HEMA) and decreased with the introduction of urease. When blood samples were treated with urease-immobilized microbeads, BUN values of patients were lowered to almost acceptable amounts. © 2002 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater 64B: 13,18, 2003 [source] Poly(glutamic acid) poly(ethylene glycol) hydrogels prepared by photoinduced polymerization: Synthesis, characterization, and preliminary release studies of protein drugsJOURNAL OF BIOMEDICAL MATERIALS RESEARCH, Issue 1 2002Zhiqiang Yang Abstract A class of new biodegradable hydrogels based on poly(ethylene glycol) methacrylate-graft-poly(glutamic acid) and poly(ethylene glycol) dimethacrylate was synthesized by photoinduced polymerization. Because all the polymeric constituents were highly hydrophilic, crosslinking could be performed in aqueous solutions. This type of crosslinked hydrogel was prepared by modifying a select number of acidic side-groups on poly(glutamic acid) with poly(ethylene glycol) methacrylate. These modified chains were then crosslinked in the presence of poly(ethylene glycol) dimethacrylate under a photoinduced polymerization at a wavelength of 365 nm. Swelling experiments were conducted to study the crosslinking density, pH-responsive behavior, and degradation of the hydrogel. Results showed that the degree of swelling of this type of hydrogels increased as the crosslinker concentration (or density) was reduced. Because of the presence of acidic side chains on poly(glutamic acid), swelling behavior was found to be pH-responsive, increasing at high pH in response to the increase in the amount of ionized acidic side chains. The degradation rate of these hydrogels also varied with pH. More rapid degradation was observed under stronger alkaline conditions because of the hydrolysis of the ester bonds between the crosslinker and the polymer backbone. Practically useful degradation rates could be achieved for such hydrogels under physiological conditions. Drug release rates from these hydrogels were found to be proportional to the protein molecular weight and the crosslinker density; increasing at lower protein molecular weight or crosslinker density. The preliminary findings presented in this article suggest that this class of biodegradable hydrogels could be an attractive avenue for drug delivery applications. The specific photoinduced crosslinking chemistry used would permit hydrogels to be synthesized in existence of the entrapped macromolecular drugs including peptides, proteins, and cells. In addition, the rapid feature of this polymerization procedure along with the ability to perform hydrogel synthesis and drug loading in an aqueous environment would offer great advantages in retaining drug activity during hydrogel synthesis. © 2002 Wiley Periodicals, Inc. J Biomed Mater Res 62: 14,21, 2002 [source] CHROMATOGRAPHIC SEPARATION AT A PREPARATIVE SCALE OF EGG WHITE OVALBUMIN AND ITS APPLICATION IN THE ELABORATION OF YOGURT MOUSSEJOURNAL OF FOOD PROCESS ENGINEERING, Issue 1 2006B. PAREDES ABSTRACT Egg white contains high-quality proteins. Some processes using eggs produce egg white as by-product. These egg white proteins may be recovered for use as additive in food products. In the first part of this study, a new polymeric material was developed and used in the chromatographic separation of ovalbumin at preparative scale. Ovalbumin is the major component of egg white and thus, it has the greatest weight in terms of its functional effects. An application of the purified ovalbumin was subsequently studied in the elaboration of yogurt mousse. The results obtained showed that the poly(glycidil methacrylate-co-ethylene dimethacrylate) resin that was manufactured enabled the separation of ovalbumin with good efficiency. This study also showed that the formulation obtained from the yogurt mousse with ovalbumin had a greater yield in volume than the commercial product used as a benchmark, improving the majority of its organoleptic qualities without appreciably affecting its stability and organoleptic properties. [source] | |||||||||||||||||||||||||||||||