ABSTRACT
Objectives: To study the ability of theaflavin-3,3'-digallate (TF3)/ethanol solution to crosslink demineralized dentin collagen, resist collagenase digestion, and explore the potential mechanism. Methods: Fully demineralized dentin blocks were prepared using human third molars that were caries-free. Then, these blocks were randomly allocated into 14 separate groups (n = 6), namely, control, ethanol, 5% glutaraldehyde (GA), 12.5, 25, 50, and 100 mg/ml TF3/ethanol solution groups. Each group was further divided into two subgroups based on crosslinking time: 30 and 60 s. The efficacy and mechanism of TF3's interaction with dentin type I collagen were predicted through molecular docking. The cross-linking, anti-enzymatic degradation, and biomechanical properties were studied by weight loss, hydroxyproline release, scanning/transmission electron microscopy (SEM/TEM), in situ zymography, surface hardness, thermogravimetric analysis, and swelling ratio. Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), and Raman spectroscopy were utilized to explore its mechanisms. Statistical analysis was performed using one and two-way analysis of variance and Tukey's test. Results: TF3/ethanol solution could effectively crosslink demineralized dentin collagen and improve its resistance to collagenase digestion and biomechanical properties (p < 0.05), showing concentration and time dependence. The effect of 25 and 50 mg/ml TF3/ethanol solution was similar to that of 5% GA, whereas the 100 mg/mL TF3/ethanol solution exhibited better performance (p < 0.05). TF3 and dentin type I collagen are mainly cross-linked by hydrogen bonds, and there may be covalent and hydrophobic interactions. Conclusion: TF3 has the capability to efficiently cross-link demineralized dentin collagen, enhancing its resistance to collagenase enzymatic hydrolysis and biomechanical properties within clinically acceptable timeframes (30 s/60 s). Additionally, it exhibits promise in enhancing the longevity of dentin adhesion.
ABSTRACT
The temperature and strain fields monitoring during the preparation process of buoyancy materials, as well as the health status after molding, are important for mastering the mechanical properties of buoyancy materials and ensuring the safety of operators and equipment. This paper proposes a short and high-density femtosecond fiber Bragg grating (fs-FBG) array based on different temperature coefficients fibers. By optimizing the parameters of femtosecond laser point-by-point writing technology, high-performance fs-FBG arrays with millimeter level gating length and millimeter level spatial resolution were prepared on two types of fibers. These were successfully embedded in buoyancy materials to achieve in-situ online monitoring of the curing process and after molding. The experimental results show that the fs-FBG array sensor has good anti-chirp performance and achieves online monitoring of millimeter-level spatial resolution. Intelligent buoyancy materials can provide real-time feedback on the health status of equipment in harsh underwater environments. The system can achieve temperature monitoring with an accuracy of 0.56 °C and deformation monitoring with sub-millimeter accuracy; the error is in the order of micrometers, which is of great significance in the field of deep-sea exploration.
ABSTRACT
A high-throughput sample pre-treatment method combined with high-performance liquid chromatography (HPLC) was developed to analyze phthalates (PAEs) in food and food contact package samples. Thin film microextraction (TFME) in 96-blade format was used to pre-treat 96 samples simultaneously. Octadecyl groups functionalized fibrous mesoporous silica nanospheres, namely C18-FMSNs, were synthesized and used as TFME coating material. The coating was fabricated by spraying a slurry of C18-FMSNs and polyacrylontrile (PAN) mixture with a commercial portable spraypen. The prepared C18-FMSNs/PAN coatings exhibited good reproducibility, repeatability and reusability. The optimized TFME conditions for PAEs consisted of extraction at pH 4.0 for 50 min, and desorption by methanol/acetonitrile (25/75, V/V) for 40 min. The pretreatment time for each sample was approximately 1.3 min. This TFME-HPLC method showed good linearity for eight PAEs within the concentration range of 0.5-1000 ng mL-1, with the coefficients higher than 0.9972. The limits of detection and quantification were 0.096-0.26 ng mL-1 and 0.32-0.86 ng mL-1, respectively. The intra-day and inter-day RSD % were below 6.6 % and 8.4 %, respectively, indicating good precision. The PAEs analysis in real samples showed that dibutyl phthalate (DBP) of 2.3 ± 0.3 ng mL-1 and di-(2-ethylhexyl) phthalate (DEHP) of 5.5 ± 0.8 ng mL-1 in boxed milk, dimethyl phthalate (DMP) of 12.6 ± 0.8 ng mL-1, DBP of 3.2 ± 0.4 ng mL-1and DEHP of 14.3 ± 0.7 ng mL-1 in the simulated water migration of plastic box, as well as DMP of 19.0 ± 0.6 ng mL-1, DBP of 25.6 ± 0.9 ng mL-1 and DEHP of 49.5 ± 2.8 ng mL-1 in the simulated ethanol migration of plastic box were determined, respectively. In addition, the detection of PAEs in all the real samples showed good recovery ranging from 85.6 to 110 % and lower RSDs % (<7.2 %).
Subject(s)
Diethylhexyl Phthalate , Nanospheres , Phthalic Acids , Silicon Dioxide , Reproducibility of Results , Phthalic Acids/analysis , Dibutyl Phthalate , Esters/analysisABSTRACT
In recent years, biopolymer aerogels as thermal insulation materials have received widespread attention due to natural abundance, cost-efficiency, and environment-friendly. However, the flammability and low strength hinder its practical application. Hollow glass microspheres (HGMs) as an inorganic thermal insulation filler have been filled in biopolymer aerogels to improve flame retardancy. However, the structure formed by HGMs embedded porous network of biopolymer aerogel has rarely been investigated, which not only reduce thermal conductivity through high porosity, but also adjust the filling volume of HGMs and achieve uniform distribution through chemical cross-linking. Herein, a biopolymer aerogel composite was assembled by chitosan aerogel (CSA) and different volume of HGMs by chemical cross-linking, freeze-drying, and silylation modification processes. When the filling volume fraction of HGMs reached 40 %, a skeleton structure was initially formed. The composites with HGMs volume of 40 %-60 % exhibited low density, high porosity, low thermal conductivity, good mechanical property, and excellent flame retardancy. According to GB 8624-2012 standard for classification, the composite with 60 % HGMs achieved class A1 non-combustible.
Subject(s)
Chitosan , Flame Retardants , Microspheres , Porosity , ExcipientsABSTRACT
The modification before the stabilization process could tune the exothermic behavior and the structural evolution of PAN fibers during stabilization. In this study, we demonstrate that a rapid thermal pretreatment in nitrogen can effectively mitigate the exothermic behavior of PAN fibers, such as decreasing the initial temperature, broadening the exothermal peak, and decreasing the nominal heat release during heating the fibers in air. The color of fibers has shown gradual changes from white to light yellow, yellow and brown during thermal pretreatment in nitrogen with the increase of pretreating temperature and time. The differential scanning calorimetry (DSC), Fourier Transform Infrared Spectrometer (FTIR), X-ray diffraction (XRD), and Thermogravimetric Analysis (TG) characterization have been applied to analyze the thermal properties, chemical and physical structural difference between PAN, and thermally pretreated PAN fibers. The thermal pretreatment of PAN fibers in nitrogen could induce cyclization, dehydrogenation, and cross-linking reactions, in which the cyclization play an important role on improving the cyclization index of stabilized PAN fibers. Meanwhile, the pretreatment can result in noticeable changes of the aggregation structure of PAN fibers, as indicated by the increase of crystallinity and crystalline size. These structural modifications can benefit the main cyclization reaction during stabilization and enhance the carbon yield in resultant carbon fibers. The rapid thermal pretreatment in nitrogen could increase efficiency of modification on PAN fibers, and that could save much time and energy. It is beneficial to manufacture low-cost carbon fibers and to spread the applications of carbon fibers.
ABSTRACT
The synthesis of a directly linked zinc chlorin dimer was first achieved by a facile and efficient oxidative coupling of zinc chlorin monomers with phenyliodine bis(trifluoroacetate) (PIFA). The reaction shows high regioselectivity at the 20-position near the hydrogenated pyrrole ring producing selective dichlorin in 74% yield.
Subject(s)
Fluoroacetates , Metalloporphyrins/chemistry , Pyrroles/chemical synthesis , Zinc/chemistry , Iodobenzenes , Molecular Structure , Oxidative Coupling , Pyrroles/chemistry , Stereoisomerism , Trifluoroacetic Acid/chemistryABSTRACT
An efficient and metal-free oxidative method was reported for synthesis of triply linked diporphyrins with 2.5 equiv of phenyliodine bis(trifluoroacetate) (PIFA). This reaction showed high selectivity for Zn(II) porphyrins and had been successfully applied in the synthesis of a novel triply-singly interlacedly linked porphyrin array with lower energy gap.