An enhanced analytical strategy integrating offline two-dimensional liquid chromatography with high-resolution accurate mass spectrometry and molecular networking: Comprehensive characterization of HuangLian JieDu Decoction as a case study

Comprehensive ingredient research is of great significance for understanding the effective material basis of herbal medicines, but due to the diversity and complexity of their phytochemicals, such research is challenging. Here, a multifaceted strategy was proposed to analyze and identify the composition of HuangLian JieDu Decoction based on offline two-dimensional liquid chromatography combined with ultraviolet detection and high-resolution mass spectrometry. Multiple components were separated by two-dimensional liquid chromatography, which consisted of hydrophilic interaction chromatography and reversed-phase liquid chromatography, and then further characterized by high-resolution mass spectrometry with a full mass spectrometry/precursor ion list/data-dependent secondary scan data acquisition method. For data processing, database screening and molecular networking were used to identify the components in HuangLian JieDu Decoction. The offline two-dimensional liquid chromatography combined with ultraviolet detection and a high-resolution mass spectrometry system showed good orthogonality of 76.35% and a high peak capacity of 5175, effectively separating multiple components. Finally, 527 compounds, including 164 alkaloids, 133 terpenoids, 88 flavonoids, 60 phenylpropanoids, 38 organic acids, and 44 other compounds, were characterized. This integrated approach is suitable for the comprehensive characterization of herbal medicines and other complex chemical systems.     

Fabrication of Mesoporous CoS2 Nanotube Arrays as the Counter Electrodes of Dye‐Sensitized Solar Cells

Mesoporous cobalt sulfide nanotube arrays on FTO‐coated glass were synthesized by combining three simple technologies: the selective etching of ZnO sacrificial templates, mesoporous Co₃O₄ formation from cobalt‐chelated chitosan, and ion‐exchange reaction (IER). The mesoporous Co₃O₄ nanotubes composed of the Co₃O₄ nanoparticles possess a high surface area and are taken advantage for further removal of templates and IER. The morphologies and crystal structures of the CoS₂ nanotube arrays were characterized by SEM, TEM, and XRD analyses. Their electrocatalytic properties were determined by electrochemical analyses including cyclic voltammetry measurements and Tafel polarization. The DSSCs assembled with a CoS₂ counter electrode achieved a power conversion efficiency of 6.13 %, which was comparable to that of the DSSC with the Pt counter electrode (6.04 %). This indicates that the mesoporous CoS₂ nanotube array can be a low‐cost and efficient alternative for the reduction of electrolytes in DSSCs.     

测试转台温控箱的计算机控制

本文针对测试转台温控箱系统的大滞后特性，设计了一种带Ｓｍｉｔｈ预估器的ＰＩ校正器，并采用了基于８０９８单片机的计算机控制实现。仿真和实验均表明，文中的控制算法能够有效克服纯大滞后对控制系统稳定性的影响，具有良好的鲁棒性及控制性能，而且实现简单，可靠性好。     

Orientation degree dependence of magnetic properties of Co doped ZnO thin films by sol–gel process

Co-doped ZnO films were successfully fabricated on Si substrates by sol–gel process. The effects of Co concentration and preheating temperature on the structure and magnetic properties of the Zn_1−x Co _x O films were systematically studied. The results revealed that the films were highly c-axis oriented and contained no impurity phase. With preheating temperature increasing, the orientation degree of the films decreased. When the Co concentration and oxygen vacancy of the films are almost changeless, the enhancement of ferromagnetism in films originates from the orientation degree of the films increasing.     

Photoluminescence and laser properties of mesostructured SBA-15 monolith doped with coumarin 151

Large, flawless and transparent silica monoliths were prepared at room temperature by solvent evaporation method and loaded with dye. The composites containing dye molecules were characterized by X-ray diffraction, transmission electron microscopy, Uv–vis and photoluminescence spectra. A red-shift in photoluminescence spectrum was observed from the composite monolith compared with that of laser dye in C₂H₅OH solution. The property of laser narrowing has been shown when the composites are pumped at _p = 355 nm by nitrogen laser.     

Structure‐Based Design of Platinum(II) Complexes as c‐myc Oncogene Down‐Regulators and Luminescent Probes for G‐Quadruplex DNA

A series of platinum(II) complexes with tridentate ligands was synthesized and their interactions with G‐quadruplex DNA within the c‐myc gene promoter were evaluated. Complex 1 , which has a flat planar 2,6‐bis(benzimidazol‐2‐yl)pyridine (bzimpy) scaffold, was found to stabilize the c‐myc G‐quadruplex structure in a cell‐free system. An in silico G‐quadruplex DNA model has been constructed for structure‐based virtual screening to develop new Pt^II‐based complexes with superior inhibitory activities. By using complex 1 as the initial structure for hit‐to‐lead optimization, bzimpy and related 2,6‐bis(pyrazol‐3‐yl)pyridine (dPzPy) scaffolds containing amine side‐chains emerge as the top candidates. Six of the top‐scoring complexes were synthesized and their interactions with c‐myc G‐quadruplex DNA have been investigated. The results revealed that all of the complexes have the ability to stabilize the c‐myc G‐quadruplex. Complex 3 a ([Pt^II L2R ] ⁺ ; L2 =2,6‐bis[1‐(3‐piperidinepropyl)‐1H‐enzo[d]imidazol‐2‐yl]pyridine, R =Cl) displayed the strongest inhibition in a cell‐free system (IC₅₀=2.2 μM ) and was 3.3‐fold more potent than that of 1 . Complexes 3 a and 4 a ([Pt^II L3R ]⁺; L3 =2,6‐bis[1‐(3‐morpholinopropyl)‐1H‐pyrazol‐3‐yl]pyridine, R =Cl) were found to effectively inhibit c‐myc gene expression in human hepatocarcinoma cells with IC₅₀ values of ≈17 μM , whereas initial hit 1 displayed no significant effect on gene expression at concentrations up to 50 μM . Complexes 3 a and 4 a have a strong preference for G‐quadruplex DNA over duplex DNA, as revealed by competition dialysis experiments and absorption titration; 3 a and 4 a bind G‐quadruplex DNA with binding constants (K) of approximately 10⁶–10⁷ dm³ mol^?1, which are at least an order of magnitude higher than the K values for duplex DNA. NMR spectroscopic titration experiments and molecular modeling showed that 4 a binds c‐myc G‐quadruplex DNA through an external end‐stacking mode at the 3′‐terminal face of the G‐quadruplex. Intriguingly, binding of c‐myc G‐quadruplex DNA by 3 b is accompanied by an increase of up to 38‐fold in photoluminescence intensity at λ_max=622 nm.     

Enhanced electrochemiluminescence of luminol-O2 system at gold–hydrophobic ionic liquid|water interface

A hydrophobic thiol-functionalized ionic liquid (IL) was synthesized and immobilized tightly on a gold electrode surface via Au–S bond to construct a stable Au–IL|water interface. At the Au–IL|water interface, the electrochemiluminescence (ECL) of luminol-O₂ system was investigated. The ECL intensity of luminol-O₂ system at the Au–IL|water interface was much larger and more stable than that at Au|water interface. The enhanced ECL mechanism at the Au–IL|water interface was studied and discussed in details.     

Preparation, characterization and luminescence properties of porous Si3N4 ceramics with Eu2O3 as sintering additive

Porous Si₃N₄ ceramics with photoluminescence properties were prepared by pressureless sintering using α-Si₃N₄ powder as raw material and Eu₂O₃ as sintering additive. Chemical composition, phase formation, microstructure and photoluminescence properties of porous Si₃N₄ ceramics were studied by X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), scanning electron microscopy (SEM) and photoluminescence measurements (PL/PLE). The results show that single Eu₂O₃ additive promotes α→β transformation but not significant densification. A broad band emission center at 570 nm assigned to Eu²⁺ is observed, Eu³⁺ in Eu₂O₃ is (partially) converted to Eu²⁺ by reaction with Si₃N₄, which results in a lower β aspect ratio and β-content compared to the other Ln (Ln=lanthanide) oxide additives.