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A kind of preparation method of pedicel glucoside

The technology of leucanthin and extract is applied in the field of preparation of leucanthoside, can solve the problems of complex operation, large loss, low relative yield and the like, and achieves the effects of simple operation, high yield and short cycle

Active Publication Date: 2021-06-15
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods still have some disadvantages, such as low yield, complicated operation, and expensive
The method disclosed in patent CN102643322A for simultaneously preparing phylloside and syringin also obtained a good purification effect, but multiple recrystallizations and methods such as preparation of liquid were used, and the equipment was expensive and the operation was complicated
Patent CN103351419A discloses a two-step method for simultaneously preparing pelicin and syringin. The coarse powder of the medicinal material is extracted with ethanol solution and then purified by recrystallization or column chromatography. The purity of the obtained pelicin is up to 98%, but the purification process is relatively complicated and the loss is large, it involves the use of a preparative liquid phase, and the use of organic solvents such as methanol and acetone is more toxic
Patent CN105646638A discloses a simple preparation method for pedicel glucoside, but the relative yield is low, the loss of pedicel glucoside is large, and organic reagents such as ethyl acetate are used, which is highly toxic

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Weigh 1 kg of Jiubingying medicinal material, add 8 times the amount of 30% ethanol solution, place it on a constant temperature water bath at 90°C for extraction under reflux for 4 hours, filter, and discard the filter residue. Concentrate the extract until there is no alcohol smell, add water to 6 times the amount, and place it overnight at 4°C to precipitate a solid. After filtering, dry the solid at 105°C for 5 hours to obtain 25.63 grams of the first part of the product. Set aside the filtrate.

[0018] Divide into four parts in parallel and put them on four columns containing 300 grams of polyamide respectively. After soaking the above-mentioned polyamide in pure water for 24 hours, put it into the column by wet method, and wash them with 3 times the column volume of pure water respectively. , discarded. Then use three times the amount of 10% ethanol solution, 20% ethanol solution, 30% ethanol solution and 40% ethanol solution to elute. The effluent was collecte...

Embodiment 2

[0022] Weigh 1 kg of Jiubing medicinal material, add 16 times the amount of 60% ethanol solution, place it on a constant temperature water bath at 90°C for extraction under reflux for 2 hours, filter, and discard the filter residue. Concentrate the extract until there is no alcohol smell, add water to 6 times the amount, and place it overnight at 4°C to precipitate a solid. After filtering, dry the solid at 105°C for 5 hours to obtain 20.56 grams of the first part of the product. Set aside the filtrate.

[0023] Divide into four parts in parallel and put them on four columns containing 300 grams of polyamide respectively. After soaking the above-mentioned polyamide in pure water for 24 hours, put it into the column by wet method, and wash them with 3 times the column volume of pure water respectively. , discarded. Then eluted with 7 times the amount of 10% ethanol solution, 20% ethanol solution, 30% ethanol solution and 40% ethanol solution respectively. The effluent was col...

Embodiment 3

[0027] Weigh 1 kg of Jiubingying medicinal material, add 8 times the amount of 20% ethanol solution, place it on a constant temperature water bath at 90°C for extraction under reflux for 4 hours, filter, and discard the filter residue. Concentrate the extract until it has no alcohol taste, add water to 6 times the amount, and after standing, a small amount of solid precipitates out, and heats and dries to gelatinize syrup. Trial was unsuccessful.

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PUM

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Abstract

The invention relates to a preparation method of pedicel glucoside. In the method, the raw material of jiubing is heated and refluxed in ethanol aqueous solution to extract, water precipitates, the filtrate is adsorbed on a polyamide column, washed with water to remove impurities, eluted with ethanol solution, and recrystallized with 30-60% ethanol to obtain the product. Compared with the prior art, the method of the invention can obviously improve the yield and purity of long products. As determined by the HPLC external standard method, the purity of the obtained pedicel glucoside product reaches more than 95%. Moreover, the operation is simple, without special and toxic solvents, environmental protection, low cost, short cycle, and is beneficial to industrialized production.

Description

technical field [0001] The invention relates to a separation technology of effective components of Chinese medicinal materials, in particular to a preparation method of pedicel glucoside. Background technique [0002] Iron holly (Ilex rotunda Thunb) is an evergreen shrub or tree belonging to the Ilex family, and is widely planted as a landscape or economic crop in southern China. Jiubing is the dry bark of Ilex holly, which is a traditional Chinese medicine. It can clear away heat and detoxify, promote dampness and relieve pain. It can be used to treat colds, pharyngitis, acute gastroenteritis, dysentery, tonsillitis and cardiovascular diseases. It has a good inhibitory effect on aerobic and anaerobic bacteria. Modern pharmacology shows that the water decoction of Jiubing has inhibitory effect on Staphylococcus aureus, hemolytic streptococcus and other bacteria, and can treat various infectious diseases. Pelicin glucoside is a pentacyclic triterpene saponin compound that m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J63/00
CPCC07J63/008
Inventor 王永刚王伟玥苏薇薇姚宏亮
Owner SUN YAT SEN UNIV