RESUMO
This article presents that acrylate copolymers are the potential candidate against the adsorption of bovine serum albumin (BSA). A series of copolymers poly(methyl methacrylate) (pMMA), poly(3-sulfopropyl methacrylate-co-methyl methacrylate) p(SPMA-co-MMA), and poly(dimethylaminoethyl methacrylate-co-methyl methacrylate) p(DMAEMA-co-MMA) were synthesized via free radical polymerization. These amphiphilic copolymers are thermally stable with a glass transition temperature (Tg) 50-120 °C and observed the impact of surface charge on amphiphilic copolymers to control interactions with the bovine serum albumin (BSA). These copolymers pMD1 and pMS1 have surface charges, - 56.6 and - 72.6 mV at pH 7.4 in PBS buffer solution that controls the adsorption capacity of bovine serum albumin (BSA) on polymers surface. Atomic force microscopy (AFM) analysis showed minimum roughness of 0.324 nm and 0.474 nm for pMS1 and pMD1. Kinetic studies for BSA adsorption on these amphiphilic copolymers showed the best fitting of the pseudo-first-order model that showed physisorption and attained at 25 °C and pH 7.4 within 24 h.
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Polímeros , Soroalbumina Bovina , Cinética , Polimetil Metacrilato , Acrilatos , MetacrilatosRESUMO
OBJECTIVE: This study was aimed at including 2.5 wt.% of carbon nanoparticles (CNPs) and graphene oxide NPs (GNPs) in a control adhesive (CA) and then investigate the effect of this inclusion on their mechanical properties and its adhesion to root dentin. MATERIALS AND METHODS: Scanning electron microscopy and energy dispersive X-ray (SEM-EDX) mapping were conducted to investigate the structural features and elemental distribution of CNPs and GNPs, respectively. These NPs were further characterized by Raman spectroscopy. The adhesives were characterized by evaluating their push-out bond strength (PBS), rheological properties, degree of conversion (DC) investigation, and failure type analysis. RESULTS: The SEM micrographs revealed that the CNPs were irregular and hexagonal, whereas the GNPs were flake-shaped. EDX analysis showed that carbon (C), oxygen (O), and zirconia (Zr) were found in the CNPs, while the GNPs were composed of C and O. The Raman spectra for CNPs and GNPs revealed their characteristic bands (CNPs-D band: 1334 cm-1, GNPs-D band: 1341 cm-1, CNPs-G band: 1650 cm-1, and GNPs-G band: 1607 cm-1). The testing verified that the highest bond strength to root dentin were detected for GNP-reinforced adhesive (33.20 ± 3.55 MPa), trailed closely by CNP-reinforced adhesive (30.48 ± 3.10 MPa), while, the CA displayed lowest values (25.11 ± 3.60 MPa). The inter-group comparisons of the NP-reinforced adhesives with the CA revealed statistically significant results (p < 0.01). Failures of adhesive nature were most common in within the adhesives and root dentin. The rheological assessment results demonstrated a reduced viscosity for all the adhesives observed at advanced angular frequencies. All the adhesives verified suitable dentin interaction shown by hybrid layer and appropriate resin tag development. A reduced DC was perceived for both NP-reinforced adhesives, compared to the CA. CONCLUSION: The present study's findings have demonstrated that 2.5% GNP adhesive revealed the highest, suitable root dentin interaction, and acceptable rheological properties. Nevertheless, a reduced DC was observed (matched with the CA). Prospective studies probing the influence of diverse concentrations of filler NPs on the adhesive's mechanical properties to root dentin are recommended.
Assuntos
Colagem Dentária , Nanopartículas , Adesivos/química , Metacrilatos/química , Carbono , Espectroscopia de Infravermelho com Transformada de Fourier , Estudos Prospectivos , Microscopia Eletrônica de Varredura , Dentina , Teste de Materiais , Adesivos Dentinários/química , Cimentos de Resina/química , Resistência à TraçãoRESUMO
INTRODUCTION: The number of published biofilm studies and novel ways for studying them has risen dramatically in recent years, ow-ing to the broad application of biofilms in medicine. Some bacteria develop biofilms that are highly resistant to antimicrobial agents, resulting in persistent infections. This necessitates the development of alternative methods for combating biofilms. In this regard, the application of cationic polymers is a good candidate for realization of this strategy. AIM: The aim of our study was to investigate the potential of a newly synthesized covalently attached star copolymer of N,N'-dimeth-ylaminoethyl methacrylate and hydroxyl-bearing oligo(ethylene glycol) methacrylate [P(DMAEMA-co-HOEGMA)] to silica surfaces and its quaternized version [P(QDMAEMA-co-HOEGMA)] for destruction of biofilms formed by Bacillus subtilis or Pseudomonas aeruginosa. MATERIALS AND METHODS: Model strains representing different genera and taxonomic groups were selected for the study. The anti-biofilm activities of two different newly synthesized cationic polymers were investigated by observation (live/dead staining) of the viability of bacterial cells within the biofilm. RESULTS: The results obtained by the live/dead labeling of bacterial biofilms show a substantial decrease in the viability of population in the presence of cationic polymers, better expressed at B. subtilis. CONCLUSIONS: The studied two immobilized on silica wafers newly synthesized star copolymers exhibited potential for anti-biofilm effects. The results demonstrated combined potential for reducing the viability of bacterial cells within the biofilms and probably for loosening the biofilm matrix. The effect was better expressed in B. subtilis.
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Biofilmes , Metacrilatos , Metacrilatos/farmacologia , Polímeros/farmacologia , Dióxido de SilícioRESUMO
In this study, magnetic poly(ethylene glycol dimethacrylate-N-methacryloyl-(L)-glutamic acid) (mPEGDMA-MAGA) particles were prepared by the dispersion polymerization in order to purify thrombin effectively. mPEGDMA-MAGA particles were synthesized by adding different ratios of magnetite (Fe3O4) to the medium in addition to the monomer phases EGDMA and MAGA. The characterization studies of mPEGDMA-MAGA particles were used by fourier transform infrared spectroscopy, zeta size measurement, scanning electron microscopy and electron spin resonance. mPEGDMA-MAGA particles were used in thrombin adsorption studies from aqueous thrombin solutions in both batch and magnetically stabilized fluidized bed (MSFB) system. Maximum adsorption capacity in pH 7.4 phosphate buffer solution is 964 IU/g polymer and 134 IU/g polymer in MSFB system and batch system, respectively. The developed magnetic affinity particles enabled the separation of thrombin from different patient serum samples in one step. It has also been observed that magnetic particles can be used repeatedly without significant reduction in adsorption capacity.
Assuntos
Ácido Glutâmico , Trombina , Humanos , Concentração de Íons de Hidrogênio , Metacrilatos/química , Polietilenoglicóis , Adsorção , Fenômenos MagnéticosRESUMO
In this work, two compounds belonging to the BODIPY family, and previously investigated for their photosensitizing properties, have been bound to the amino-pendant groups of three random copolymers, with different amounts of methyl methacrylate (MMA) and 2-(dimethylamino)ethyl methacrylate (DMAEMA) in the backbone. The P(MMA-ran-DMAEMA) copolymers have inherently bactericidal activity, due to the amino groups of DMAEMA and to the quaternized nitrogens bounded to BODIPY. Systems consisting of filter paper discs coated with copolymers conjugated to BODIPY were tested on two model microorganisms, Escherichia coli (E. coli) and Staphylococcus aureus (S. aureus). On solid medium, irradiation with green light induced an antimicrobial effect, visible as a clear inhibition area around the coated disks. The system based on the copolymer with 43% DMAEMA and circa 0.70 wt/wt% of BODIPY was the most efficient in both bacterial species, and a selectivity for the Gram-positive model was observed, independently of the conjugated BODIPY. A residual antimicrobial activity was also observed after dark incubation, attributed to the inherently bactericidal properties of copolymers.
Assuntos
Anti-Infecciosos , Fotoquimioterapia , Escherichia coli , Metilmetacrilato , Staphylococcus aureus , Anti-Infecciosos/farmacologia , Metacrilatos/farmacologia , Polímeros/farmacologia , Antibacterianos/farmacologia , Fármacos Fotossensibilizantes/farmacologiaRESUMO
Due to the questionable durability of dental restorations, there is a need to increase the lifetime of composite restoration. The present study used diethylene glycol monomethacrylate/4,4'-methylenebis(cyclohexyl isocyanate) (DEGMMA/CHMDI), diethylene glycol monomethacrylate/isophorone diisocyanate (DEGMMA/IPDI) monomers, and bis(2,6-diisopropylphenyl)carbodiimide (CHINOX SA-1) as modifiers of a polymer matrix (40 wt% urethane dimethacrylate (UDMA), 40 wt% bisphenol A ethoxylateddimethacrylate (bis-EMA), and 20 wt% triethyleneglycol dimethacrylate (TEGDMA)). Flexural strength (FS), diametral tensile strength (DTS), hardness (HV), sorption, and solubility were determined. To assess hydrolytic stability, the materials were tested before and after two aging methods (I-7500 cycles, 5 °C and 55 °C, water and 7 days, 60 °C, 0.1 M NaOH; II-5 days, 55 °C, water and 7 days, 60 °C, 0.1 M NaOH). The aging protocol resulted in no noticeable change (median values were the same as or higher than the control value) or a decrease in the DTS value from 4 to 28%, and a decrease in the FS value by 2 to 14%. The hardness values after aging were more than 60% lower than those of the controls. The used additives did not improve the initial (control) properties of the composite material. The addition of CHINOX SA-1 improved the hydrolytic stability of composites based on UDMA/bis-EMA/TEGDMA monomers, which could potentially extend the service life of the modified material. Extended studies are needed to confirm the possible use of CHINOX SA-1 as an antihydrolysis agent in dental composites.
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Metacrilatos , Ácidos Polimetacrílicos , Bis-Fenol A-Glicidil Metacrilato , Hidróxido de Sódio , Teste de Materiais , Resinas Compostas , Polietilenoglicóis , Poliuretanos , ÁguaRESUMO
A novel drug delivery system designed for intraocular injection, gelatin methacryloyl (GelMA), has attracted much attention due to its sustained-release character and low cytotoxicity. We aimed to explore the sustained drug effect of GelMA hydrogels coupled with triamcinolone acetonide (TA) after injection into the vitreous cavity. The GelMA hydrogel formulations were characterized using scanning electron microscopy, swelling measurements, biodegradation, and release studies. The biological safety effect of GelMA on human retinal pigment epithelial cells and retinal conditions was verified by in vitro and in vivo experiments. The hydrogel exhibited a low swelling ratio, resistance to enzymatic degradation, and excellent biocompatibility. The swelling properties and in vitro biodegradation characteristics were related to the gel concentration. Rapid gel formation was observed after injection, and the in vitro release study confirmed that TA-hydrogels have slower and more prolonged release kinetics than TA suspensions. In vivo fundus imaging, optical coherence tomography measurements of retinal and choroid thickness, and immunohistochemistry did not reveal any apparent abnormalities of retinal or anterior chamber angle, and ERG indicated that the hydrogel had no impact on retinal function. The GelMA hydrogel implantable intraocular device exhibited an extended duration, in situ polymerization, and support cell viability, making it an attractive, safe, and well-controlled platform for treating the posterior segment diseases of the eye.
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Hidrogéis , Triancinolona Acetonida , Humanos , Hidrogéis/química , Gelatina/química , Metacrilatos , Injeções Intraoculares , Engenharia TecidualRESUMO
The visualization of organs and tissues using 31P magnetic resonance (MR) imaging represents an immense challenge. This is largely due to the lack of sensitive biocompatible probes required to deliver a high-intensity MR signal that can be distinguished from the natural biological background. Synthetic water-soluble phosphorus-containing polymers appear to be suitable materials for this purpose due to their adjustable chain architecture, low toxicity, and favorable pharmacokinetics. In this work, we carried out a controlled synthesis, and compared the MR properties, of several probes consisting of highly hydrophilic phosphopolymers differing in composition, structure, and molecular weight. Based on our phantom experiments, all probes with a molecular weight of ~3-400 kg·mol-1, including linear polymers based on poly(2-methacryloyloxyethyl phosphorylcholine) (PMPC), poly(ethyl ethylenephosphate) (PEEP), and poly[bis(2-(2-(2-methoxyethoxy)ethoxy)ethoxy)]phosphazene (PMEEEP) as well as star-shaped copolymers composed of PMPC arms grafted onto poly(amidoamine) dendrimer (PAMAM-g-PMPC) or cyclotriphosphazene-derived cores (CTP-g-PMPC), were readily detected using a 4.7 T MR scanner. The highest signal-to-noise ratio was achieved by the linear polymers PMPC (210) and PMEEEP (62) followed by the star polymers CTP-g-PMPC (56) and PAMAM-g-PMPC (44). The 31P T1 and T2 relaxation times for these phosphopolymers were also favorable, ranging between 1078 and 2368 and 30 and 171 ms, respectively. We contend that select phosphopolymers are suitable for use as sensitive 31P MR probes for biomedical applications.
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Fósforo , Polímeros , Polímeros/química , Metacrilatos/química , Micelas , Fosforilcolina/química , Espectroscopia de Ressonância Magnética , Materiais Biocompatíveis/química , Ácidos Polimetacrílicos/química , Propriedades de SuperfícieRESUMO
Silk methacrylate (SilMA) has been studied extensively due to its ability to modify Silk fibroin (SF) by increasing the water solubility and enhancing the mechanical properties of SF hydrogels. However, SilMA hydrogels are generally soft with weak mechanical properties. In order to enhance the mechanical properties of hydrogel scaffolds, we used liquid nitrogen to modify SilMA to obtain a novel N2-SilMA/gelatin-methacryloyl (GelMA) composite hydrogel. N2-SilMA was successfully detected by Fourier transform infrared (FTIR) spectroscopy and 1H nuclear magnetic resonance. Scanning electron microscope showed that the composite hydrogel still had certain arrangement characteristics of SF and dense pores which met the necessary conditions for the cell scaffold. The mechanical tests showed that the mechanical properties of SilMA were greatly enhanced after modification at ultra-low temperature. We evaluated its cytocompatibility and biocompatibility, and the results showed that the composite scaffold promoted the growth of cells. Different types of composite hydrogels were injected into ICR mice and the results showed a stable scaffold structure in vivo, suggesting their ability to promote angiogenesis. In conclusion, the N2-SilMA/GelMA composite hydrogel had better mechanical properties, excellent cytocompatibility, and biological properties compared to the other groups.
Assuntos
Fibroínas , Engenharia Tecidual , Animais , Camundongos , Engenharia Tecidual/métodos , Seda/química , Gelatina/química , Hidrogéis/química , Estudos de Viabilidade , Camundongos Endogâmicos ICR , Tecidos Suporte/química , Fibroínas/química , MetacrilatosRESUMO
In this paper, macroporous antimicrobial polymeric gels (MAPGs) functionalized with active quaternary ammonium cations attached to varying hydrocarbon chain lengths have been fabricated. Apart from the change in the alkyl chain length attached to the quaternary ammonium cation, the amount of crosslinker was also varied during the fabrication of the macroporous gels. The prepared gels were characterized using Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, field emission scanning electron microscopy (FE-SEM) and swelling studies. In addition, the mechanical properties of the fabricated macroporous gels were studied using compression and tensile testing. The antimicrobial activity of the gels has been determined for Gram-negative bacteria (Escherichia coli, Pseudomonas aeruginosa) as well as Gram-positive bacteria (Bacillus subtilis, Staphylococcus aureus). Antimicrobial activity, as well as the mechanical properties of the macroporous gels, was found to be influenced by the alkyl chain length attached to the quaternary ammonium cations as well as by the amount of crosslinker used for the fabrication of the gel. In addition, on increasing the alkyl chain length from C4 (butyl) to C8 (octyl), the effectiveness of the polymeric gels increased. It was observed that the gels derived using a tertiary amine (NMe2) containing monomer showed relatively low antimicrobial activity as compared to the gels obtained using quaternized monomers (C4 (butyl), C6 (hexyl), and C8 (octyl)). The gels based on the quaternized C8 monomer displayed the highest antimicrobial activity and mechanical stability as compared to the gels based on the C4 and C6 monomers.
Assuntos
Compostos de Amônio , Anti-Infecciosos , Antibacterianos/farmacologia , Antibacterianos/química , Polímeros/química , Anti-Infecciosos/química , Metacrilatos/química , CátionsRESUMO
Potential estrogenic effects and changes in fertility are some of the health problems associated with bisphenol A (BPA) derivatives used to produce some polymers, including dental materials that contain Bis-GMA. Those issues drove this study proposing the synthesis of methacrylate resveratrol and phenolphthalein monomers that, combined with diluent monomers, generate copolymers. Their key characteristics were determined and analyzed on the chemical structure-property perspective considering monomer planarity and flexibility based on molecular dynamic simulations. METHODS: Methacrylate resveratrol ((E)-5-(4-(methacryloyloxy)styryl)-1,3-phenylenebis(2-methylacrylate)), EMPM) and methacrylate phenolphthalein ((3-oxo-1,3-dihydroisobenzofuran-1,1-diyl)bis(4,1-phenylene)bis(2-methylacrylate)), DIFPM) were synthesized through the reaction of precursors with methacryloyl chloride. After monomers purification and spectroscopic characterization (FTIR and NMR), the following copolymers were produced: DIFPM/TEGDMA and Bis-GMA/TEGDMA, EMPM/HEMA and Bis-GMA/HEMA. Microhardness, degree of conversion, water sorption and contact angle data were statistically analyzed through one-way ANOVA and Tukey's test (p ≤ 0.05). RESULTS: The DIFPM molecular structure's reduced flexibility proved to be an important factor to inhibit TEGDMA cyclization. In turn, the EMPM molecule's high planarity modified the spatial organization of the HEMA copolymer, altering the water diffusion and, therefore, the water sorption when compared to Bis-GMA copolymers. CONCLUSION: The scientific findings contribute to better understand the effect of monomer chemical structures, molecular geometry, and planarity on some physicochemical properties of copolymers. Knowledge that can contribute to the design of new monomers to replace Bis-GMA.
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Metacrilatos , Fenolftaleína , Bis-Fenol A-Glicidil Metacrilato/química , Resveratrol , Metacrilatos/química , Ácidos Polimetacrílicos/química , Polietilenoglicóis/química , Polímeros/química , Água/química , Resinas Compostas/química , Teste de Materiais , Materiais DentáriosAssuntos
Antineoplásicos , Carcinoma Pulmonar de Células não Pequenas , Neoplasias Pulmonares , Humanos , Carcinoma Pulmonar de Células não Pequenas/tratamento farmacológico , Gefitinibe/uso terapêutico , Neoplasias Pulmonares/tratamento farmacológico , Metacrilatos/uso terapêutico , Antineoplásicos/uso terapêuticoRESUMO
BACKGROUND: To evaluate the release of bisphenol-A glycidyl methacrylate (BisGMA), triethylene glycol dimethacrylate (TEGDMA), bisphenol A (BPA), and phthalates of the composite resin used in the bonding of spurs applied in the treatment of children with anterior open bite and its effects on human keratinocytes. METHODOLOGY: Saliva samples of 22 children were collected before spur attachment (baseline) and 30 minutes (min) and 24 hours (h) after spur bonding. Analysis was performed using high-performance liquid chromatography (HPLC) coupled to tandem mass spectrometry (HPLC-MS/MS) and gas chromatography coupled to mass spectrometry (GC-MS). Standardized resin increments were added to three different dilutions of the cell culture medium. Keratinocytes (HaCaT) were cultivated in the conditioned media and evaluated for cell viability (MTT) and cell scratch assay. RESULTS: The levels of BisGMA (1.74±0.27 µg/mL), TEGDMA (2.29±0.36 µg/mL), and BPA (3.264±0.88 µg/L) in the saliva after 30 min, in comparison to baseline (0±0 µg/mL, 0±0 µg/mL, and 1.15±0.21 µg/L, respectively), presented higher numbers. After 24 h, the levels of the monomers were similar to the baseline. Phthalates showed no significant difference among groups. HaCat cells showed increased viability and reduced cell migration over time after exposure to methacrylate-based resin composites. CONCLUSION: Resin composites, used to attach spurs in children with anterior open bite during orthodontic treatment, release monomers after polymerization and can influence the behavior of human keratinocytes, even at very low concentrations. Orthodontists should be aware of the risks of the resinous compounds release and preventive procedures should be held to reduce patient exposure.
Assuntos
Mordida Aberta , Saliva , Criança , Humanos , Saliva/química , Espectrometria de Massas em Tandem , Ácidos Polimetacrílicos/química , Resinas Compostas/química , Bis-Fenol A-Glicidil Metacrilato/química , Metacrilatos/química , Polietilenoglicóis/química , Teste de MateriaisRESUMO
High elution and diffusion of 2-hydroxylethyl methacrylate (HEMA) and camphorquinone (CQ) through dentinal tubules may induce pulp injury and postoperative sensitivity. We aimed to investigate the melatonin protective effect in HEMA- and CQ-treated human dental pulp cells (hDPCs) as well as its relevance in a mechanism for postoperative sensitivity in diabetic patients. hDPCs were exposed to HEMA (5 mM) and/or CQ (1 mM) in the absence and presence of melatonin (MEL) (0.1 mM and 1 mM). Heme oxygenase-1 (HMOX1), NADPH oxidase-4 (NOX4), BCL-2-associated X-protein (BAX), B-cell lymphoma-2 (BCL-2) and caspase-3 (CASP3) gene expression levels, and superoxide dismutase (SOD) activity were measured in hDPCs while inducible nitric oxide synthase (iNOS) and melatonin protein expression were measured in human dental pulp as well, by RT-PCR, by ELISA, and spectrophotometrically. Bioinformatic analyses were performed by using the ShinyGO (v.0.75) application. Type 2 diabetic patients showed a higher incidence of postoperative sensitivity and lower melatonin and higher iNOS content in dental pulp tissue compared with non-diabetic patients. Melatonin, when co-added in hDPC culture, reverses HEMA and CQ cytotoxic effects via anti-apoptotic and anti-inflammatory/antioxidant iNOS-related effects. Enrichment analyses showed that genes/proteins, altered by HEMA and CQ and normalized by melatonin, are the most prominently overrepresented in type 2 diabetes mellitus pathways and that they share subcellular localization in different oligomeric protein complexes consisting of anti- and pro-apoptotic regulators. This is the first evidence of the ability of melatonin to counteract iNOS-mediated inflammatory and stress effects in HEMA- and CQ-treated hDPCs, which could be of significance for the modulation of presently observed immediate postoperative sensitivity after composite restoration in type 2 diabetic patients.
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Diabetes Mellitus Tipo 2 , Melatonina , Humanos , Melatonina/farmacologia , Diabetes Mellitus Tipo 2/tratamento farmacológico , Metacrilatos/farmacologia , Óxido Nítrico Sintase Tipo II/genética , Óxido Nítrico Sintase Tipo II/metabolismo , Polpa Dentária/metabolismo , Antioxidantes , Proteínas Proto-Oncogênicas c-bcl-2/metabolismoRESUMO
Modern dentistry places great demands on the dental composites used for filling tooth cavities or treating cavitated tooth decay. The aim of the work was to modify the properties of composites by changing the initiators and co-initiators. This was achieved by using initiators based on a quinoxaline skeleton and co-initiators that are derivatives of acetic acid, which is an advantage of these photoinitiating systems due to the elimination of aromatic amines from the photocurable composition. The composites also differed in dental fillers. The effect of the compounds on the exothermicity of the photopolymerization process, the surface morphology of the obtained materials and the maximum compressive strength were determined. The photoinitiating capacity of the two-component systems was tested by the microcalorimetric method using the multifunctional monomer TMPTA, typical for dental filler compositions. The new photoinitiating systems show particularly good efficiency of free radical polymerization initiation, which occurs by the photoinduced intermolecular electron transfer (PET) mechanism. The comparison of the tested systems with camphorquinone, a photoinitiator traditionally used in dentistry, made it possible to observe a decrease in temperature during photopolymerization without a significant decrease in the polymerization rate or increase in photocuring time, as well as a better homogeneity of the surface of the obtained polymeric materials. This indicates that dye-acetic acid derivative systems may be useful in dental applications.
Assuntos
Resinas Compostas , Quinoxalinas , Resinas Compostas/química , Metacrilatos/química , Polímeros , Polimerização , Teste de Materiais , Materiais DentáriosRESUMO
Coenzyme Q10 (CoQ10) is a vital substance found throughout body. It helps convert food into energy and is eaten small amounts in foods. CoQ10 has gained great interest in recent years as a potential candidate for the treatment of various diseases. The content of CoQ10 in food samples is a crucial quality index for foods. Therefore, the development of sensitive separation and quantification method for determining the amount of CoQ10 in various samples, especially in foods, is an important issue, especially for food nutrition. In this study, a new, miniaturized monolithic column was developed and applied for the determination of CoQ10 in pistachio samples by nano-liquid chromatography (nano-LC). The monolithic column with a 50 µm i.d. was prepared by in situ polymerization using laurylmethacrylate (LMA) as the main monomer and ethylene dimethacrylate (EDMA) as the crosslinker. Methanol (MeOH) and polyethyleneglycol (PEG) were used as porogenic solvents. The final monolithic column was characterized by using scanning electron microscopy (SEM) and chromatographic analyses. The monolithic column with a 50 µm i.d. was applied to the analysis of CoQ10 in pistachio samples in nano-LC. This analytical method was validated by means of sensitivity, linearity, precision, recovery, and repeatability. The LOD and LOQ values were 0.05 and 0.48 µg/kg, respectively. The developed method using the monolithic column was optimized to achieve very sensitive analyses of CoQ10 content in the food samples. The applicability of the method was successfully demonstrated by the analysis of CoQ10 in pistachio samples.
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Pistacia , Cromatografia Líquida/métodos , Metacrilatos/química , Solventes , Microscopia Eletrônica de Varredura , Cromatografia Líquida de Alta PressãoRESUMO
Considering the poor hydrolytic stability of the most methacrylate-based functional monomers of self-etch dental adhesives in acidic and aqueous conditions, in this study allyl-based photo-polymerizable self-etch monomers was synthesized in order to improve the hydrolytic stability. The new self-etch monomers based on phosphonic acid functional groups were synthesized through a two-step procedure. First, phosphoric anhydride, poly-phosphoric acid, and polyethylene glycol were reacted to produce phosphate ester precursor (P-PEG-P). Next, allyl 2, 3-epoxypropyl ether was reacted with P-PEG-P to synthesize allyl self-etch monomer. Glycidyl methacrylate was also reacted with P-PEG-P to synthesize a methacrylate self-etch analogue monomer. The monomers were characterized using FTIR and 1H-NMR spectroscopy. The viscosities of monomers were measured using a rheometer. The degree photopolymerization conversion of monomers was measured using FTIR spectroscopy. The pH assay was performed by a digital pH-meter. The etching behavior of the monomers on human teeth was studied using scanning electron microscopy (SEM). Thermo-gravimetric analysis (TGA) was performed to evaluate the possible interaction of the monomers with tricalcium phosphate (TCP). The solubility of synthesized monomers was examined in ethanol, acetone, and water. The hydrolytic stability of cured resins in artificial saliva during 4 months was also surveyed. The synthesis of new self-etching monomers was successfully confirmed by spectroscopy analyses. The results represented appropriate viscosity of self-etching monomers around 1 (Pa s). The resin containing methacrylate monomer exhibited its degree of conversion is more than that of allyl monomer (p < 0.05). The allyl and methacrylate self-etch monomers exhibited pH values of 1.2 and 1.3, respectively. SEM micrograph verified that the synthesized monomers were able to suitable etching of the enamel human premolar teeth. The data obtained from TGA tests revealed that thermal stability of (TCP) containing monomers is enhanced. Also, the monomers exhibited an excellent solubility in polar solvents, but when they are mixed with TCP, they are not, anymore, dissolved in these solvents. Furthermore, the allyl monomer showed higher hydrolytic stability than the methacrylate monomer. The new photo-polymerizable acidic monomer based on allyl functionality showed enhanced hydrolytic stability compared to methacrylate-based monomer. It may be considered as a promising monomer for self-etch dental adhesives.
Assuntos
Adesivos , Colagem Dentária , Humanos , Polimerização , Metacrilatos/química , Solventes , Água , Cimentos Dentários , Teste de Materiais , Cimentos de Resina/química , Adesivos Dentinários/químicaRESUMO
Osteosarcoma (OS) is the most common form of primary malignant bone cancer in adolescents. Over the years, OS prognosis has greatly improved due to adjuvant and neoadjuvant (preoperative) chemotherapeutic treatment, increasing the chances of successful surgery and reducing the need for limb amputation. However, chemotherapeutic treatment to treat OS is limited by off-target toxicities and requires improved localization at the tumor site. Collagen, the main constituent of bone tissue, is extensively degraded and remodeled in OS, leading to an increased availability of denatured (monomeric) collagen. Collagen hybridizing peptides (CHPs) comprise a class of peptides rationally designed to selectively bind to denatured collagen. In this work, we have conjugated CHPs as targeting moieties to water-soluble N-(2-hydroxypropyl)methacrylamide (HPMA) copolymers to target OS tumors. We demonstrated increased accumulation of collagen-targeted HPMA copolymer-CHP conjugates compared to nontargeted HPMA copolymers, as well as increased retention compared to both nontargeted copolymers and CHPs, in a murine intratibial OS tumor model. Furthermore, we used microcomputed tomography analysis to evaluate the bone microarchitecture and correlated bone morphometric parameters (porosity, bone volume, and surface area) with maximum accumulation (Smax) and accumulation at 168 h postinjection (S168) of the copolymers at the tumor. Our results provide the foundation for the use of HPMA copolymer-CHP conjugates as targeted drug delivery systems in OS tumors.
Assuntos
Neoplasias Ósseas , Osteossarcoma , Camundongos , Humanos , Animais , Adolescente , Microtomografia por Raio-X , Sistemas de Liberação de Medicamentos/métodos , Metacrilatos , Peptídeos , Colágeno , PolímerosRESUMO
This review addresses the need for a framework to increase the consistency, objectivity and transparency in the regulatory assessment of respiratory sensitisers and associated uncertainties. Principal issues are considered and illustrated through a case study (with methyl methacrylate). In the absence of test methods validated for regulatory use, formal documentation of the weight-of-evidence for hazard classification both at the level of integration of individual studies within lines of evidence and across a broad range of data streams was agreed to be critical for such a framework. An integrated approach is proposed to include not only occupational studies and clinical evidence for the regulatory assessment of respiratory sensitisers, but also information on structure and physical and chemical factors, predictive approaches such as structure activity analysis and in vitro and in vivo mechanistic and toxicokinetic findings. A weight-of-evidence protocol, incorporating integration of these sources of data based on predefined considerations, would contribute to transparency and consistency in the outcome of the assessment. In those cases where a decision may need to be taken on the basis of occupational findings alone, conclusions should be based on transparent weighting of relevant data on the observed prevalence of occupational asthma in various studies taking into account all relevant information including the range and nature of workplace exposures to the substance of interest, co-exposure to other chemicals and study quality.