Separation of cannabinoids on three different mixed‐mode columns containing carbon/nanodiamond/amine‐polymer superficially porous particles

Three mixed‐mode high‐performance liquid chromatography columns packed with superficially porous carbon/nanodiamond/amine‐polymer particles were used to separate mixtures of cannabinoids. Columns evaluated included: (i) reversed phase (C₁₈), weak anion exchange, 4.6 × 33 mm, 3.6 μm, and 4.6 × 100 mm, 3.6 μm, (ii) reversed phase, strong anion exchange (quaternary amine), 4.6×33 mm, 3.6 μm, and (iii) hydrophilic interaction liquid chromatography, 4.6 × 150 mm, 3.6 μm. Different selectivities were achieved under various mobile phase and stationary phase conditions. Efficiencies and peak capacities were as high as 54 000 N/m and 56, respectively. The reversed phase mixed‐mode column (C₁₈) retained tetrahydrocannabinolic acid strongly under acidic conditions and weakly under basic conditions. Tetrahydrocannabinolic acid was retained strongly on the reversed phase, strong anion exchange mixed‐mode column under basic polar organic mobile phase conditions. The hydrophilic interaction liquid chromatography column retained polar cannabinoids better than the (more) neutral ones under basic conditions. A longer reversed phase (C₁₈) mixed‐mode column (4.6 × 100 mm) showed better resolution for analytes (and a contaminant) than a shorter column. Fast separations were achieved in less than 5 min and sometimes 2 min. A real world sample (bubble hash extract) was also analyzed by gradient elution.     

Silica‐supported polymeric monolithic column with a mixed mode of hydrophilic and strong cation‐exchange interactions for microcolumn liquid chromatography

A novel sulfonic acid group containing hydrophilic strong cation‐exchange monolith was prepared by in situ coating 5 μm bare silica particles with the copolymers of glycidyl methacrylate and pentaerythritol triacrylate and further sulfonating the prepared polymer matrix with Na₂SO₃ inside a 150 μm id capillary. The preparation conditions were investigated, and the method was described in detail. The prepared column was characterized by comparing with its counterparts reported previously in terms of matrix morphology, preparation reproducibility, permeability, swelling–shrinking behavior, mechanical stability, hydrophilicity, binding capacity, and column efficiency. The swelling–shrinking behavior of the present column in solvents of different polarities was negligible, the hydrophobicity could be suppressed at the acetonitrile concentrations higher than 40% v/v, and the binding capacities were 256 μequiv/mL and 20.1 mg/mL for Cu²⁺ and lysozyme, respectively. The minimum theoretical plate heights were 8, 10, and 13 μm, and the values of the C term in van Deemter equation were 9, 12, and 35 ms for the test analytes of Na⁺, thiourea, and cytidine 5ʹ‐monophosphate, respectively. This column exhibited an excellent performance in the separations of monovalent inorganic cations, uncharged polar, and charged polar compounds.     

Unexpected Factors Affecting the Kinetics of Guest Molecule Release from Investigation of Binary Chemical Systems Trapped in a Single Void of Mesoporous Silica Particles

In this work, we present results for loading of well-defined binary systems (cocrystal, solid solution) and untreated materials (physical mixtures) into the voids of MCM-41 mesoporous silica particles employing three different filling methods. The applied techniques belong to the group of “wet methods” (diffusion supported loading – DiSupLo ) and “solvent-free methods” (mechanical ball-mill loading – MeLo , thermal solvent free – TSF ). As probes for testing the guest1-guest2 interactions inside the MCM-41 pores we employed the benzoic acid ( BA ), perfluorobenzoic acid ( PFBA ), and 4-fluorobenzoic acid ( 4-FBA ). The guests intermolecular contacts and phase changes were monitored employing magic angle spinning (MAS) NMR Spectroscopy techniques and powder X-ray diffraction (PXRD). Since mesoporous silica materials are commonly used in drug delivery system research, special attention has been paid to factors affecting guest release kinetics. It has been proven that not only the content and composition of binary systems, but also the loading technique have a strong impact on the rate of guests release. Innovative methods of visualizing differences in release kinetics are presented.     

Size-controlled flow synthesis of metal-organic frameworks crystals monitored by in-situ ultraviolet-visible absorption spectroscopy

Size-controlled flow synthesis of nanoporous particles are of considerable interest for future industrial applications,however,is facing challenges due to lack of in-situ method for size-characterization in fluidic environment.We present that ultraviolet-visible(UV-vis) absorption spectroscopy can be integrated into a flow-synthesis system which was produced by femtosecond laser micro machining.The shift of the absorption peak position of the ex-situ and in-situ UV-vis spectra correlates to variation of size of porous metal-organic frameworks crystals.ZIF-67 crystals with a size in the range from 200 nm to1025 nm are fabricated with the assistance of tri-ethylamine under monitoring of in-situ UV-vis spectra.The ZIF-67 crystals are converted into nanoporous carbons particles with controlled sizes.These materials show size-dependent performance in Na-ion battery and size-independent performance in metal/H_2 O seawater battery.     

Janus 粒子在环境检测领域中的应用

Janus 粒子,也称为阴阳结构粒子或两面性非对称粒子,是指表面上具有两种或两种以上不同化学组成或性质的不对称粒子。目前,Janus 粒子因其独特的结构和功能已经逐渐成为生物医药、催化、材料以及防污等领域中的新型功能材料。在环境检测领域,Janus材料亦因其特殊的光学、磁学及电学性能,为提高检测灵敏度、选择性和稳定性等提供了新的研究方向。基于此,本文主要讨论了Janus材料在环境检测方面的特点、优势和相关应用。最后,本文基于本课题组的研究经验以及工作中所面临的问题,对本领域的发展和未来的研究方向提出了展望,以期对本领域的未来发展提供指导。     

Self-Crosslinked Ellipsoidal Poly(Tannic Acid) Particles for Bio-Medical Applications

Self-crosslinking of Tannic acid (TA) was accomplished to obtain poly(tannic acid) (p(TA)) particles in single step, surfactant free media using sodium periodate (NaIO₄) as an oxidizing agent. Almost monodisperse p(TA) particles with 981 ± 76 nm sizes and −22 ± 4 mV zeta potential value with ellipsoidal shape was obtained. Only slight degradation of p(TA) particles with 6.8 ± 0.2% was observed at pH 7.4 in PBS up to 15 days because of the irreversible covalent formation between TA units, suggesting that hydrolytic degradation is independent from the used amounts of oxidation agents. p(TA) particles were found to be non-hemolytic up to 0.5 mg/mL concentration and found not to affect blood clotting mechanism up to 2 mg/mL concentration. Antioxidant activity of p(TA) particles was investigated by total phenol content (TPC), ferric reducing antioxidant potential (FRAP), trolox equivalent antioxidant capacity (TEAC), total flavanoid content (TFC), and Fe (II) chelating activity. p(TA) particles showed strong antioxidant capability in comparison to TA molecules, except FRAP assay. The antibacterial activity of p(TA) particles was investigated by micro-dilution technique on E. coli as Gram‑negative and S. aureus as Gram-positive bacteria and found that p(TA) particles are more effective on S. aureus with over 50% inhibition at 20 mg/mL concentration attained.     

Concerted effect of boron and porosity on shear thickening behavior of hybrid mesoporous silica dispersions

In the present work, the influence of porosity and boron on shear thickening behavior of hybrid mesoporous silica has been studied. Three different levels of boron modification were performed by varying the molar composition of boric acid viz., 1.5 mmol, 2.5 mmol, and 3.5 mmol in a co-condensation approach. The incorporation of boron in mesoporous silica network was confirmed by various techniques such as Fourier transform infra-red (FTIR), and ¹¹B solid- state nuclear magnetic resonance (NMR) spectroscopy. The morphology and particle size were confirmed by using scanning and transmission electron microscopy. To evaluate the effect of boron and porosity on the shear thickening behavior, dispersions were prepared from mesoporous boron- modified silica (MSiB), control mesoporous silica (MSi), non-porous boron-modified silica (SiB), and control non-porous silica (Si) in polyethylene glycol. The shear thickening behavior was studied using steady shear rheology. The dispersion prepared from different loadings of synthesized MSiB containing 1.5 mmol boron showed more than 16 times increase in viscosity (657.7 Pa.s) compared to that of MSi (39.2 Pa.s) at a fairly low volume fraction (φ = 0.15) of silica. It is expected that the highly ordered mesoporous architecture of hybrid silica has improved the interaction between the particle and the dispersing medium through hydrogen bonding. The porous morphology of the hybrid mesoporous silica as well as the incorporation of boron in the silica network favors the formation of a frictional contact network, and a transition from continuous shear thickening (CST) to discontinuous shear thickening (DST) behavior was observed. Therefore, silica prepared via incorporation of boron as well as porosity can be material of interest in variety of applications, for example, soft body armors, sporting goods, and shear thickening electrolytes for high impact resistant batteries.     

Physicochemical Interaction of ZnO Fine Particles with 5‐Mono‐(4‐carboxyphenyl)‐10,15,20‐Triphenylporphyrin

This study deals with an investigation on the preparation and physicochemical interactions of ZnO nanoparticles with acid functionalized porphyrin [5‐mono‐(4‐carboxyphenyl)‐10,15,20‐triphenylporphyrin (CPTPP)] for photovoltaic applications in a detailed manner. Zinc acetate and sodium hydroxide were used as the starting materials for the synthesis of ZnO nanoparticles at 60 °C in an alcoholic medium. The freshly prepared fine particles were then functionalized with CPTPP. Both the virgin and pregnant ZnO particles were characterized by using UV‐Visible spectrophotometry (UV), fluorescence emission (PL), Fourier transform infrared spectroscopy (FTIR), X‐ray diffraction (XRD) and scanning electron microscopy (SEM). The band gap energy obtained for ZnO particles, having a value of 3.47 eV, shows significant quantum confinement effect and enhanced photophysical activity. FTIR analysis of the doped ZnO nanostructures showed the presences of some chemical species. SEM analysis revealed a clear change in the surface morphologies of undoped ZnO. The average crystallite size of nanoparticles, calculated from XRD peaks, was found in the nano regime. The lattice parameters calculated for ZnO nanocrystals were also found in good agreement with those given in the literature. From the enhancement in the red shift of the UV‐Vis spectra, it is concluded that hybridization of acid functionalized porphyrin can cause a significant expansion in the total absorption region of ZnO semiconductor for photovoltaic applications.     

准东高碱煤气化过程中碱金属迁移与结渣特性实验研究

利用循环流化床对天池木垒高碱煤进行了气化实验研究,获得了天池木垒高碱煤在循环流化床上的结渣特性及碱金属迁移规律,并对实验中出现的床内颗粒聚团现象进行了分析。结果表明,不同存在形态的碱金属在煤气化过程中的迁移规律不同,水溶钠和醋酸铵溶钠在煤气化过程中以气态形式析出,不溶钠主要存在半焦中;随着气化温度升高,底渣和煤气中钠含量增加,飞灰中钠含量减少;尾部管道温度降低过程中,煤气中钠的冷凝速率明显高于钾;天池木垒高碱煤气化过程中容易引起床内颗粒聚团,床温越高,颗粒聚团现象越明显,床温波动越大;碱金属与灰分中矿物成分及床料中SiO₂反应生成黏性低温共熔物是导致颗粒聚团的关键。     

Detection of p53 Gene by Using Genomagnetic Assay Combined with Carbon Nanotube Modified Disposable Sensor Technology

Electrochemical monitoring of DNA hybridization related to p53 gene sequence was investigated using genomagnetic assay combined with single walled carbon nanotube (SWCNT) modified pencil graphite electrodes (PGEs). The hybridization was performed either at magnetic beads (MB) surface or in solution. The enhanced guanine signal was obtained using SWCNT‐PGEs compared to one obtained by unmodified PGEs. The selectivity of genomagnetic assay was tested under optimum conditions. The DLs were calculated as 0.88 µM and 0.11 µM for hybridization performed at MB surface and solution, respectively. This selective, practical and cost effective genomagnetic assay combined with SWCNT‐PGEs is reported herein for the first time.