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磺酸功能化离子液体催化制备薯蓣皂苷元研究

投稿时间：2023-10-23 点此下载全文

引用本文：黄凤玉,李东洋,谢彩侠,张娟,刘富岗,王飞燕,王庆婷.磺酸功能化离子液体催化制备薯蓣皂苷元研究[J].中国现代中药,2024,26(5):839-847

DOI：10.13313/j.issn.1673-4890.20231023002

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作者中文名	作者英文名	单位中文名	单位英文名	E-Mail
黄凤玉	HUANG Feng-yu	河南中医药大学药学院，河南郑州 450046 河南省中药质量控制与评价工程技术研究中心，河南郑州 450046	School of Pharmacy, Henan University of Chinese Medicine, Zhengzhou 450046, China Henan Engineering and Technology Research Center for Quality Control and Evaluation of TCM, Zhengzhou 450046, China
李东洋	LI Dong-yang	河南中医药大学药学院，河南郑州 450046 河南省中药质量控制与评价工程技术研究中心，河南郑州 450046	School of Pharmacy, Henan University of Chinese Medicine, Zhengzhou 450046, China Henan Engineering and Technology Research Center for Quality Control and Evaluation of TCM, Zhengzhou 450046, China
谢彩侠	XIE Cai-xia	河南中医药大学药学院，河南郑州 450046 河南省中药质量控制与评价工程技术研究中心，河南郑州 450046	School of Pharmacy, Henan University of Chinese Medicine, Zhengzhou 450046, China Henan Engineering and Technology Research Center for Quality Control and Evaluation of TCM, Zhengzhou 450046, China
张娟*	ZHANG Juan	河南中医药大学药学院，河南郑州 450046 河南省中药质量控制与评价工程技术研究中心，河南郑州 450046	School of Pharmacy, Henan University of Chinese Medicine, Zhengzhou 450046, China Henan Engineering and Technology Research Center for Quality Control and Evaluation of TCM, Zhengzhou 450046, China
刘富岗*	LIU Fu-gang	河南中医药大学药学院，河南郑州 450046	School of Pharmacy, Henan University of Chinese Medicine, Zhengzhou 450046, China
王飞燕	WANG Fei-yan	河南中医药大学药学院，河南郑州 450046 河南省中药质量控制与评价工程技术研究中心，河南郑州 450046	School of Pharmacy, Henan University of Chinese Medicine, Zhengzhou 450046, China Henan Engineering and Technology Research Center for Quality Control and Evaluation of TCM, Zhengzhou 450046, China
王庆婷	WANG Qing-ting	河南中医药大学药学院，河南郑州 450046 河南省中药质量控制与评价工程技术研究中心，河南郑州 450046	School of Pharmacy, Henan University of Chinese Medicine, Zhengzhou 450046, China Henan Engineering and Technology Research Center for Quality Control and Evaluation of TCM, Zhengzhou 450046, China

基金项目:河南省高等学校重点科研计划项目（23A360003）

中文摘要:目的探索磺酸功能化离子液体1-磺丁基-3-甲基咪唑三氟甲烷磺酸盐（[BHSO₃MIm]CF₃SO₃）作为催化剂在薯蓣皂苷元制备中的应用。方法以盾叶薯蓣提取粗皂苷为原料、[BHSO₃MIm]CF₃SO₃为催化剂，水解制备薯蓣皂苷元。通过单因素试验对反应温度、反应时间、离子液体用量、溶剂体积进行考察，采用响应面分析方法进一步优化反应条件，确定最佳反应条件。进行12次循环实验，考察该离子液体循环使用性能。结果最佳反应条件为反应温度100 ℃、反应时间5.17 h、离子液体用量2.56 g、水溶剂体积6 mL，在该条件下薯蓣皂苷元产率为12.99%。该离子液体循环6次时，循环效率为82.70%，循环10次时循环效率降至58.12%。结论在薯蓣皂苷元制备过程中，[BHSO₃MIm]CF₃SO₃作为酸催化剂，表现出了水解效率高、性能稳定、易于回收、循环使用性能良好等优势，具备较强的应用前景。

中文关键词:磺酸功能化离子液体 1-磺丁基-3-甲基咪唑三氟甲烷磺酸盐薯蓣皂苷元响应面分析

Study on Catalytic Preparation of Diosgenin by Sulfonic Acid-Functionalized Ionic Liquid

Abstract:Objective To explore the application of the sulfonic acid-functionalized ionic liquid [BHSO₃MIm]CF₃SO₃ as a catalyst in the preparation of diosgenin.Methods Crude saponins extracted from Dioscorea zingiberensis were used as raw materials. With [BHSO₃MIm]CF₃SO₃ as a catalyst, diosgenin was prepared by hydrolysis. The reaction temperature, reaction time, amount of ionic liquid, and volume of solvent were investigated by single factor test. The reaction conditions were further optimized by response surface analysis to determine the optimal reaction conditions. The recycling performance of the ionic liquid was investigated by 12 cycles of experiments.Results The optimal reaction condition was as follows: reaction temperature at 100 °C, reaction time of 5.17 h, ionic liquid amount of 2.56 g, and solvent of 6 mL. Under these condition, the yield of diosgenin was 12.99%. When the ionic liquid was tested six times, the cycling efficiency was still as high as 82.70% and decreased to 58.12% when the ionic liquid was tested 10 times.Conclusion In the preparation process of diosgenin, [BHSO₃MIm]CF₃SO₃, as an acid catalyst, has the advantages of high hydrolysis efficiency, stable performance, easy recovery, and good recycling performance, and it has a strong application prospect.

keywords:sulfonic acid-functionalized ionic liquid [BHSO₃MIm]CF₃SO₃ diosgenin response surface analysis

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