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Method for large-scale preparation of wedelolactone chemical reference substance

A technology of wedelide and lactone chemistry, which is applied in the field of large-scale preparation of wedelide chemical reference substances, can solve the problems that the output of reference substances cannot meet the needs of practical applications, cannot be scaled up for industrial scale production, and the steps are cumbersome, etc., and achieve Easy to prepare materials in batches, easy to process, and improve the effect of separation efficiency

Inactive Publication Date: 2014-09-17
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, most of the reports on the preparation of wedelolide from Eclipta chinensis are laboratory-scale, and the steps are cumbersome, such as Zhang Jinsheng et al. 95% methanol percolation extraction, methanol dissolving to remove impurities or ethyl acetate extraction to remove impurities, silica gel column separation to obtain wedelolide, and the separation eluent uses toluene-acetone-acetic acid (6:8:1) or dichloromethane- Methanol-water (14:9:4 lower layer); Yuan Hongxia et al. (Chinese Journal of Experimental Formulas, 17 (16): 103-105, 2011) reported that 95% ethanol percolation extraction, ethyl acetate extraction, silica gel column Petroleum ether-ethyl acetate gradient separation, sephadex LH-20 purification to obtain wedelide; Wagner et al. (Ger.DE3525363, German patent) used methanol soaking extraction, ethyl acetate extraction, C18 reverse-phase HPLC gradient elution to prepare wedelide , Kokai et al. (JP83228353, Japanese patent) use water reflux extraction, butanol-water (1:1) countercurrent-countercurrent distribution, Sephadex LH-20, such documents may use benzene and dichloromethane containing more toxic elution Solvent, or Sephadex LH-20, C18 expensive separation packing, and almost all use very time-consuming percolation or immersion extraction, which cannot be scaled up for industrial scale production, and the output of reference substances cannot meet the needs of practical applications

Method used

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  • Method for large-scale preparation of wedelolactone chemical reference substance
  • Method for large-scale preparation of wedelolactone chemical reference substance
  • Method for large-scale preparation of wedelolactone chemical reference substance

Examples

Experimental program
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Effect test

Embodiment 1

[0028] 1) Ethyl acetate extraction:

[0029] Add 3kg of Eclipta alcohol extract (provided by Sichuan Academy of Traditional Chinese Medicine), add 15L of water, heat to dissolve at 40°C, add 4.5L of ethyl acetate for extraction, extract 3 times, combine extracts, concentrate under reduced pressure to 500ml, mix Add 500 grams of 100-200 mesh silica gel, mix well, dry in a fume hood, and grind for later use.

[0030] 2) Medium-pressure silica gel column chromatography purification:

[0031] Pick The stainless steel column is used as a medium-pressure chromatography column, and 1.5kg of 100-200 mesh silica gel is loaded as a separation silica gel, and the ethyl acetate extract sample powder is evenly loaded into the column head, and the packing is tight; Shanghai Tongtian TBP2H10 constant flow pump is used as a medium-pressure column. Pump, petroleum ether: ethyl acetate: acetic acid (7:3:1) mixed solvent as the eluent, the flow rate is controlled at 150ml / min, the pressure is...

Embodiment 2

[0036] 1) Ethyl acetate extraction:

[0037]40kg of Eclipta medicinal material, reflux extraction with 70% ethanol, 480L for the first time, 400L for the second time, each extraction for 1.5 hours, the two extractions were combined to obtain about 7kg of alcohol extract extract; add 35L of water, heat at 40°C Make it dissolve, add 10.5L ethyl acetate for extraction, extract 3 times, combine the extracts, concentrate under reduced pressure to 2L, mix in 2kg of 100-200 mesh silica gel, mix well, dry in a fume hood, and grind for later use.

[0038] 2) Purification by silica gel column chromatography under reduced pressure:

[0039] Pick The stainless steel column is used as a decompression chromatography column, and a 2.5L suction filter bottle is used as a collector; 4.2kg of 200-300 mesh silica gel is loaded as a separation silica gel, and the ethyl acetate extract powder is evenly loaded into the column head, and the packing is tight; Henan Gongyi Yuhua brand circulating v...

Embodiment 3

[0043] 1) Ethyl acetate extraction:

[0044] Add 1kg of Eclipta alcohol extract (provided by Sichuan Academy of Traditional Chinese Medicine), add 5L of water, heat to dissolve at 40°C, add 1.5L of ethyl acetate for extraction, extract 3 times, combine extracts, concentrate under reduced pressure to 200ml, mix Add 200 grams of 100-200 mesh silica gel, mix well, dry in a fume hood, and grind for later use.

[0045] 2) Medium-pressure silica gel column chromatography purification:

[0046] Pick The stainless steel column is used as a medium-pressure chromatography column, and 750 grams of 100-200 mesh silica gel is loaded as a separation silica gel, and the ethyl acetate extract powder is evenly loaded into the column head, and the packing is tight; Shanghai Tongtian TBP2H10 constant flow pump is used as the medium Pressure pump, petroleum ether: ethyl acetate: acetic acid (6:4:1) mixed solvent as the eluent, the flow rate is controlled at 100ml / min, the pressure is about 0.2...

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Abstract

The invention relates to a new technology for large-scale preparation of a wedelolactone chemical reference substance. Through wedelolactone stability and preparation process streamlining optimization, a self-made large medium-pressure or pressure reduced silica gel column is employed for chromatography purification to obtain the wedelolactone chemical reference substance with purity greater than 98% in batches, and the scale is up to the 10g grade.

Description

[0001] Technical Field The present invention relates to a new preparation process for the large-scale preparation of Wedelolactone (Wedelolactone) chemical reference substance. It mainly includes three steps of ethyl acetate extraction, self-made large-scale medium pressure or vacuum silica gel column chromatography purification, and recrystallization. Background technique [0002] Wedelolide is a coumarin compound, which has the functions of protecting the liver, anti-inflammation, and enhancing immunity. The Chinese Pharmacopoeia (2010 edition) listed it as a new quantitative index component of the traditional Chinese medicine Eclipta chinensis. There is a huge gap in practical application. In addition, The separation and purification steps of the reference substance are cumbersome, all of which lead to the high price of the reference substance (commercially available at 1000-1500 yuan, 20mg / bottle). Therefore, obtaining a large number of reference substances in batches can ...

Claims

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Application Information

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IPC IPC(8): C07D493/04
CPCC07D493/04
Inventor 肖红斌王莉彭杰程孟春
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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