Application of chromatography technology in the separation of active alkaloids from Hypecoum leptocarpum and their inhibitory effect on fatty acid synthase

A method that involved the combination of pH‐zone‐refining counter‐current chromatography and semipreparative reversed‐phase liquid chromatography has been established for the preparative separation of alkaloids from Hypecoum leptocarpum. From 1.2 g of crude sample, 31 mg N‐feruloyltyramine, 27 mg oxohydrastinine, 47 mg hydroprotopine, 25 mg leptopidine, and 18 mg hypecocarpine have been obtained. The structure of the new compound, hypecocarpine, is confirmed based on the analysis of spectroscopic data, including NMR, UV, and IR spectroscopy and positive electrospray ionization mass spectrometry. The known chemical structures were characterized on the basis of ¹H and ¹³C NMR spectroscopy. The purities of the five alkaloids are all over 92.7% as determined by high‐performance liquid chromatography. The alkaloids’ cytotoxicity in breast cancer cells is assessed by using a Cell Counting Kit assay and their inhibitory effect on fatty acid synthase expression is assessed by a Western blot assay. These results suggest that leptopidine could suppress growth and induce cytotoxicity in breast cancer cells and that the cytotoxicity of leptopidine may be related to its inhibitory effect on fatty acid synthase expression.     

A Robust Metal-Organic Framework with Scalable Synthesis and Optimal Adsorption and Desorption for Energy-Efficient Ethylene Purification

Adsorptive separation is an energy-efficient alternative, but its advancement has been hindered by the challenge of industrially potential adsorbents development. Herein, a novel ultra-microporous metal-organic framework ZU-901 is designed that satisfies the basic criteria raised by ethylene/ethane (C₂H₄/C₂H₆) pressure swing adsorption (PSA). ZU-901 exhibits an “S” shaped C₂H₄ curve with high sorbent selection parameter (65) and could be mildly regenerated. Through green aqueous-phase synthesis, ZU-901 is easily scalable with 99 % yield, and it is stable in water, acid, basic solutions and cycling breakthrough experiments. Polymer-grade C₂H₄ (99.51 %) could be obtained via a simulating two-bed PSA process, and the corresponding energy consumption is only 1/10 of that of simulating cryogenic distillation. Our work has demonstrated the great potential of pore engineering in designing porous materials with desired adsorption and desorption behavior to implement an efficient PSA process.     

Hyperterpenoids A and B: Two pairs of unprecedented 6/6/4/6/6 polycyclic cyclobutane meroterpenoids with potent neuroprotective and anti-inflammatory activities from Hypericum beanii

Hyperterpenoid A (1) and B (2), two pairs of enantiomers, with an unprecedented 6/6/4/6/6 polycyclic skeleton, along with one known compoud hypermonone A (3) were isolated from Hypericum beanii. The racemate (±)-1 and (±)-2 were successfully separated into the two optically pure enantiomers (ee ≥ 99%) using a preparative HPLC system. Their absolute configurations were elucidated by extensive spectroscopic analyses and single-crystal X-ray diffraction method. The related plausible biogenetic pathways were presented. Compound 1-3 showed significant neuroprotective activity and potential anti-inflammatory activity. The result that (+)-2 and (-)-2 presented different anti-inflammatory properties, may lead us to new discovery of structure activity relationship between racemates, enantiomers, and diastereomers, as well as further research regarding the binding of drugs to target proteins.     

Water-in-salt widens the electrochemical stability window: Thermodynamic and kinetic factors

Originating from the 1.23 V potential window of pure water, the narrow electrochemical stability window (ESW) has always been the most stubborn problem for aqueous battery systems. However, the water-in-salt system magically widens the ESW of aqueous electrolyte from 1.23 V to above 3 V by the super-concentrated LiTFSI solution. The mechanisms of widening aqueous battery ESW have been a crucial topic, in which the significant factors, including unique solid–electrolyte interface, solvation structure, and others, have been highlighted. Here, we specify the concept of ESW in detail and review the influence factors of ESW in the water-in-salt system from both thermodynamic and kinetic perspectives to explore the importance of each factor.     

磨削粗糙表面法向接触刚度研究

为更加准确地描述机械磨削表面的接触刚度,本文在现有统计分析理论的基础上,提出了一种新的粗糙表面接触模型。模型针对接触表面微凸体形貌,将原有的球体假设采用cos函数曲线回转体代替,在假设形貌的基础上重新解算了微凸体弹塑性变形的临界压入深度,推导出了接触区域真实接触压力与接触刚度关系表达式。通过数值仿真方法得到了不同塑性指数下平均距离、接触刚度与接触压力之间的变化关系。对比结果显示,随着塑性指数的增大,本文模型的平均距离与球形模型的平均距离之间的差值逐渐增大。在接触刚度方面,本文模型相比球形模型更加贴近实验结果,并且随着塑性指数的增加,球形模型与本文模型之间的差值越来越大。本文模型结果与实验数据的相对偏差能够控制在5%以内,从而验证了本文模型的正确性,为更加准确地描述磨削表面零件的接触行为提供理论基础。     

Fatigue damage evolution in silicon films for micromechanical applications

In this paper we examine the conditions for surface topography evolution and crack growth/fracture during the cyclic actuation of polysilicon microelectromechanical systems (MEMS) structures. The surface topography evolution that occurs during cyclic fatigue is shown to be stressassisted and may be predicted by linear perturbation analyses. The conditions for crack growth (due to pre-existing or nucleated cracks) are also examined within the framework of linear elastic fracture mechanics. Within this framework, we consider pre-existing cracks in the topical SiO₂ layer that forms on the Si substrate in the absence of passivation. The thickening of the SiO₂ that is normally observed during cyclic actuation of Si MEMS structures is shown to increase the possibility of stable crack growth by stress corrosion cracking prior to the onset of unstable crack growth in the SiO₂ and Si layers. Finally, the implications of the results are discussed for the prediction of fatigue damage in silicon MEMS structures.     

抗磨可靠性寿命的加速试验与预测

在工程实际中，对新机器零件的抗磨可靠性寿命进行评估或预测非常重要，但是，由于磨损是一种受多因素制约的随机过程，目前在实验室广泛采用的模拟磨损试验，不仅周期较长，而且预测误差也比较大。因此，提出了一种在保持磨损机相似的前提下合理选用高ＰＶ值的抗磨可靠性寿命加速试验的新方法。