Three anthraquinones-emodin, chrysophanol, and physcion-were successfully purified from the dichloromethane extract of the Chinese medicinal herb Rumex japonicus by high-speed counter-current chromatography (HSCCC). The extract was separated with nhexane-ethanol-water (18:22:3, v/v/v) as the two-phase solvent system and yielded 3.4 mg of emodin, 24.1 mg of chrysophanol, and 2.0 mg of physcion from 500 mg of sample with purities of 99.2 %, 98.8% and 98.2%, respectively. The HSCCC fractions were analyzed by high-performance liquid chromatography (HPLC) and the chemical structures of the three anthraquinones were confirmed by 1 H-NMR and 13 C-NMR analysis. This is the first time these anthraquinones have been obtained from R. japonicus by HSCCC.
Lignocellulosic biomass is mainly composed of polysaccharides and lignin. The complexity and diversity of the plant cell wall polymers makes it difficult to isolate the components in pure form for characterization. Many current approaches to analyzing the structure of lignocellulose, which involve sequential extraction and characterization of the resulting fractions, are time-consuming and laborintensive. The present study describes a new and facile system for rationally derivatizing and dissolving coarsely ground plant cell wall materials. Using ionic liquids (EmimAc) and dichloroacetyl chloride as a solvent/reagent produced mildly acetylated whole cell walls without significant degradation. The acetylated products were soluble in DMSO-d 6 from which they can be characterized by solution-state two-dimensional nuclear magnetic resonance (2D NMR) spectrometry. A distinct advantage of the procedure is that it realizes the dissolution of whole lignocellulosic materials without requiring harsh ball milling, thereby allowing the acquisition of high-resolution 2D NMR spectra to revealing structural details of the main components (lignin and polysaccharides). The method is therefore beneficial to understanding the composition and structure of biomass aimed at its improved utilization.
Nanozymes have developed rapidly as substitutes for natural enzymes. However, the toxic synthesis and the use of expensive materials seriously restrict their large-scale applications. To solve these issues, Fe 3+ -doped aminated lignin (Fe-AL) peroxidase-mimicking nanozymes were innovatively synthesized. The active center FeN x was introduced to alkali lignin by amination via Mannich or epoxidation methods before Fe 3+ -doping. The Fe-AL nanozymes could achieve accurate colorimetric detection of H 2 O 2 in 10−100 mM and could be reused over 30 times with only a negligible decrease in catalytic activity. Besides, the color-developing systems could even maintain the blue color over 72 h, which showed great promise in designing cheap and portable H 2 O 2 sensors. This work not only can promote the development of lignin-based nanomaterials but also provide a new way for the synthesis of nanozymes from natural macromolecules.
In this study, a sn-1, 3 extracellular lipases from Aspergillus niger GZUF36 (PEXANL1) was expressed in Pichia pastoris, characterized, and the predicted structural model was analyzed. The optimized culture conditions of P. pastoris showed that the highest lipase activity of 66.5 ± 1.4 U/mL (P < 0.05) could be attained with 1% methanol and 96 h induction time. The purified PEXANL1 exhibited the highest activity at pH 4.0 and 40°C temperature, and its original activity remained unaltered in the majority of the organic solvents (20% v/v concentration). Triton X-100, Tween 20, Tween 80, and SDS at a concentration of 0.01% (w/v) enhanced, and all the metal ions tested inhibited activity of purified PEXANL. The results of ultrasound-assisted PEXANL1 catalyzed synthesis of 1,3-diaglycerides showed that the content of 1,3-diglycerides was rapidly increased to 36.90% with 25 min of ultrasound duration (P < 0.05) and later decreased to 19.93% with 35 min of ultrasound duration. The modeled structure of PEXANL1 by comparative modeling showed α/β hydrolase fold. Structural superposition and molecular docking results validated that Ser162, His274, and Asp217 residues of PEXANL1 were involved in the catalysis. Small-angle X-ray scattering analysis indicated the monomer properties of PEXANL1 in solution. The ab initio model of PEXANL1 overlapped with its modeling structure. This work presents a reliable structural model of A. niger lipase based on homology modeling and small-angle X-ray scattering. Besides, the data from this study will benefit the rational design of suitable crystalline lipase variants in the future.
Chloride corrosion test was carried out in 4% NaCl solution to study the chloride corrosion resistance of rubber concrete. Rubber concrete was prepared by using 20 mesh, 1∼3 mm, and 3∼6 mm rubber particles instead of sand by 5%, 10%, 15%, and 20% of the cementitious material mass. The P-wave velocity and compressive strength of rubber concrete were measured. The microstructure of rubber concrete corroded by chloride was analyzed by SEM. The micromorphology was compared with the macrofailure characteristics under uniaxial compression. The results show that the rubber concrete was still in the early stage of erosion. With the increase of immersion time at the age of 110 days, the P-wave velocity and compressive strength of concrete were generally on the rise. Furthermore, during the period of erosion, the mechanical properties of rubber concrete increased with the increase of rubber particle size and decreased with the increase of the content. Therefore, when the rubber particle size was 3∼6 mm and the content was 5%, the antierosion performance was the best. This study has a certain guiding significance for the chloride corrosion resistance of rubber concrete.
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