JOURNAL OF NANOPARTICLE RESEARCH
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2023
·Vol. 25
·期 7
·1-15
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IF 2.5
Fan Mingxuan,Tang Lingqian,Wang Yihan,Feng Lu,Zhou Hong
In this work, thiol-functionalized silica SiO 2 -Pr-SH (Pr = −(CH 2 ) 3 ) was synthesized by self-hydrolysis of 3-mercaptopropyltrimethoxysilane (MPTMS) with the average particle sizes up to 1.9 μm. Then sulfonic acid-functionalized SiO 2 -PrSPr-SO 3 H was prepared by the 1,3-Propanesultone grafted onto SiO 2 -Pr-SH and used as solid acid catalysts for alcoholysis of total saponins in Dioscorea zingiberensis C. H. Wright (DZW) to the production of diosgenin. The as-prepared solid acid was fully characterized with FT-IR, Raman, TGA, BET, FESEM, EDS, elemental mapping, XPS, and XRD, respectively. The solid acid quantity, solvent dosage, extraction temperature, and time were studied by single-factor experiments. The maximum yield of diosgenin was calculated to be 16.73% relative to 0.1 g total saponins, which was higher than the sulfuric acid hydrolysis method. Importantly, it is an efficient alcoholysis approach for the production of diosgenin from total saponins and the prepared solid acid can be recycled in the reaction medium. The possible alcoholysis products and reaction mechanism were proposed on the basis of LC-MS results. This work not only provides a new solid acid for the production of diosgenin from DZW but also gives a beneficial synthetic reference for the preparation of high-activity SO 3 H-functionalized catalysts based on the organosilane. Graphical abstract SO 3 H-functionalized silica as an efficient solid acid catalyst for the production of diosgenin from Dioscorea zingiberensis C. H. Wright
研究领域:
化学工程
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植物化学
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药物合成
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高影响因子
CATALYSIS LETTERS
·
2022
·Vol. 153
·期 4
·1096-1108
·
IF 2.936
Tang Lingqian,Fan Mingxuan,Pan Zhiquan,Cheng Qingrong,Feng Lu,Wu Hanjun,Zhou Hong
Low-molecular weight solid acid, [(DETA-(SO 3 H) 2 ], was synthesized and fully characterized by FTIR, XRD, TGA, XPS, 1 H-NMR and elemental analysis. The prepared solid acid exhibited high strong acid density (7.6 mmol H + /g), much higher than most of other solid acids. The solid acid was used for the extraction of diosgenin from the saponins in Dioscorea zingiberensis C. H. Wright. Diosgenin is a very medical intermediate for the synthesis of various kinds of steroidal drugs. To improve the diosgenin yield, the optimal conditions of the extraction reaction were investigated by single-factor experiments. Under the optimized conditions, the diosgenin yield catalyzed by the solid acid was much higher than those obtained by the catalysis of other solid acids or conventional sulfuric acid. Importantly, no waste liquid was discharged in the approach as the reaction medium can be recycled. The alcoholysis approach for the production of diosgenin has a great potential application in the industry. Graphical Abstract A novel low-molecular weight solid acid was synthesized and fully characterized. The solid acid showed excellent catalytic activity for the catalytic alcoholysis of saponins from D. zingiberensis C. H. Wright (DZW), the catalyst can be recycled and the whole extraction process is green and efficient.
研究领域:
化学工程
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植物化学
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医药工业
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高影响因子
CHEMICAL ENGINEERING JOURNAL
·
2024
·
IF 13.3
Yongxian Niu,Xi zhang,Wenbing Yu,Han Yin,Rui Lu,Zhenggang Liu,Fang Lu
Herein, a renewable system consisted of tartaric acid and isopropanol was developed to produce diosgenin efficiently from Dioscorea zingiberensis rhizomes. The yield of diosgenin reached 4.15% comparable to the highest value reported in previous researches. The combination of experiment and DFT calculation revealed that the acid-alcohol system could regulate the hydrogen bond interaction of each component in the rhizomes to disassemble the connection network and promote the release of saponin. Meanwhile, the intramolecular hydrogen bond of tartaric acid and the steric hindrance effect of isopropanol could prevent the esterification reaction and maintain the strong acidity of the system for the high yield of diosgenin. The scale-up experiment with a 100-fold feeding capacity was also conducted successfully. Furthermore, the technological process integrated with purification of diosgenin, recovery of organic acid and solvent and upgrading of residual solid to porous carbon materials has been established systematically to verify the prospective of industrialization.
研究领域:
植物化学
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药物化学
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高影响因子
BIORESOURCE TECHNOLOGY
·
2026
·
IF 8.2
Wenbing Yu,Lishan Chen,Han Yin,Rui Lu,Zhenggang Liu,Fang Lu
Diosgenin represents a key precursor in the synthesis of steroidal pharmaceuticals, yet its conventional production relies on strong acid hydrolysis, which generates substantial acidic wastewater and poses serious environmental concerns. To circumvent these issues, a sustainable strategy for precise engineering of acid site in biochar catalysts derived from Dioscorea zingiberensis residues is presented. The carbon supports were prepared by direct calcination of the biomass residues across a controlled temperature range without exogenous additives, allowing tailored specific surface parameters. Subsequent sulfonation introduced sulfonic acid groups as the primary active sites, along with carboxylic acid groups and other weak acid species. A linear correlation was identified between the specific surface area and total acid site density, enabling rational regulation of acidic properties. Alcoholysis of saponins catalyzed by C-800-SO 3 H (derived from calcination at 800 °C with subsequent sulfonation) enabled a diosgenin yield of 23.26% based on crude saponins, equivalent to 4.39% relative to the raw rhizome mass. Catalytic performance correlated strongly with sulfonic acid density, indicating that sulfonic acid groups dominate the catalytic conversion. The catalyst also retained considerable activity over five reuse cycles. This work establishes a rational and eco-compatible route for designing high-performance solid acid catalysts from biomass waste, demonstrating promising potential for green production of pharmaceutical intermediates.
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PubMed
高影响因子
Journal of Cleaner Production
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2020
·
IF 7.246
Bowei Shen,XueJun Yu,Farong Zhang,Wenxiu Jiang,Hui Yuan,Zhiquan Pan,Hong Zhou
A new method of the catalytic alcoholysis of Dioscorea zingiberensis C. H. Wright into diosgenin by magnetic solid acid in a Teflon-lined stainless-steel autoclave for the first time. The magnetic solid acid, Fe 3 O 4 @SiO 2 –SO 3 H, was prepared by the connecting the –SO 3 H groups on the surface of SiO 2 encapsulated Fe 3 O 4 microspheres . The synthesized catalysts were systematically analyzed by Fourier transform infrared (FT-IR) spectroscopy, thermogravimetric analyzer (TGA), X-ray diffraction (XRD), vibrating sample magnetometry (VSM), temperature programmed desorption of ammonia (NH 3 -TPD), scanning electron microscope (SEM), transmission electron microscope (TEM) and transmission electron microscope-mapping(TEM-mapping). To obtain the best conditions for the alcoholysis of Dioscorea zingiberensis C. H. Wright, single factor test was first utilized to determine the range of optimal conditions and optimized by response surface method . A three-level-three-factor Box-Behnken design was adopted to illustrate the effect of solid acid mass, solvent volume, reaction time and temperature on the yield of diosgenin. The optimum conditions obtained by response surface methodology were: 0.42 g Fe 3 O 4 @SiO 2 –SO 3 H, 4.38 mL solvent of ethanol, the reaction temperature at 100 °C and 6.09 h reaction time. At the optimal conditions, this method can reach the highest yield 2.64% from Dioscorea zingiberensis C. H. Wright. The yield of the new method was 21.66% higher than conventional sulfuric acid hydrolysis based on the analysis results of UV and HPLC. Importantly, the catalysts and solvents used in the alcoholysis process by the solid acid can be recovered, which is green and environmentally friendly, indicating that the catalytic alcoholysis with magnetic solid acid under hydrothermal conditions had a broad application prospect in diosgenin production.
研究领域:
植物化学
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药物化学
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绿色化学
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高影响因子
危险品化学品经营许可证（带存储）