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The preparation method of pedicel glucoside

A technique for the concentration of pedicel glucoside, which is applied in the field of preparation of pelican glucoside, can solve the problems of complex process, complicated method, and low yield, and achieve the effect of simple process, easy process, and high yield

Active Publication Date: 2017-03-29
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional silica gel column separation method takes a long time, consumes a large amount of organic solvents, and has low yield, which is no longer suitable for modern industrial requirements; the method using high-efficiency countercurrent chromatography is not suitable for factory scale-up production; the method using macroporous resin has complex processes and low yield
Patent CN103351419 discloses a two-step method for simultaneously preparing pelicin and syringin. Bing coarse powder is extracted with ethanol under reflux, and recrystallization or column chromatography is used to purify pelicin to obtain Syringin and pelicin, the purity is 98%, but for the extraction and separation of pelicin, the yield loss is relatively large
[0006] To sum up, the existing methods for extracting and purifying catechin glucoside from Jiubing have problems such as complex methods, unsuitability for industrial scale-up, use of more toxic reagents, low yield, low efficiency, and high cost.

Method used

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  • The preparation method of pedicel glucoside
  • The preparation method of pedicel glucoside

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take 1 kg of the medicinal material of jiubing, add 14 times the amount (14 L) of ethanol aqueous solution with a volume fraction of 40%, reflux extraction twice, the extraction time is 90 min, filter, collect the extracts twice, and combine the filtrates to obtain the jiubing extract.

[0021] Heat and concentrate the ethanol extract, recover the ethanol until it has no alcohol smell, and obtain the extract, add twice the amount of water (2L) and ethyl acetate (2L) of the medicinal materials, stir and mix, and let it stand at room temperature overnight (12h), white The flaky precipitate was precipitated in the water layer and filtered to obtain a white residue.

[0022] The filter residue was dried under normal pressure to obtain 31.0 g of pedicel glucoside product with a yield of 3.1%.

[0023] With pedicel glucoside reference substance (National Inspection Institute, batch number 11868-201001) as the external standard, use the HPLC method to detect the pedicel glucos...

Embodiment 2

[0025] Take 1kg of the medicinal material of jiubing, add 8 times the amount (8L) of 30% ethanol aqueous solution for reflux extraction twice, the extraction time is 90min, filter, collect the extracts twice, and combine the filtrates to obtain the jiubing extract.

[0026] Heat and concentrate the ethanol extract, recover the ethanol until it has no alcohol smell, and obtain the extract, add twice the amount of water (2L) and ethyl acetate (2L) of the medicinal materials, stir and mix, and let it stand at room temperature overnight (12h), white The flaky precipitate was precipitated in the water layer and filtered to obtain a white residue.

[0027] The filter residue was dried under normal pressure to obtain 27.8 g of pedicel glucoside product with a yield of 2.8%. With pedicel glucoside reference substance (National Inspection Institute, batch number 11868-201001) as the external standard, use the HPLC method to detect the pedicel glucoside product, and the chromatographic ...

Embodiment 3

[0029] Take 1 kg of the medicinal material of jiubing, add 14 times the amount (14 L) of ethanol aqueous solution with a volume fraction of 40%, reflux extraction twice, the extraction time is 90 min, filter, collect the extracts twice, and combine the filtrates to obtain the jiubing extract.

[0030] Heat and concentrate the ethanol extract, recover the ethanol until it has no alcohol smell, and obtain the extract, add water (1L) and ethyl acetate (1L) equal to the amount of the medicinal material, stir and mix, and let it stand overnight at room temperature (12h), white The flaky precipitate was precipitated in the water layer and filtered to obtain a white residue.

[0031] The filter residue was dried under normal pressure to obtain 35.7 g of pedicel glucoside product with a yield of 3.6%.

[0032] With pedicel glucoside reference substance (National Inspection Institute, batch number 11868-201001) as the external standard, use the HPLC method to detect the pedicel glucosi...

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Abstract

The invention relates to a preparation method of pedunculoside. The method includes the following steps of using the traditional Chinese medicinal material ovateleaf holly bark as the raw material, conducting heating reflux extraction through a 20%-70% ethyl alcohol aqueous solution, concentrating filtrate till no alcohol smell exists to obtain extract, dissolving and evenly mixing the extract in a 30%-70% ethyl acetate aqueous solution, standing overnight, conducting filtering to obtain filter residues, and drying the filter residues to obtain pedunculoside. Compared with the prior art, the method has the advantages of being simple in process, short in period, low in cost, high in product productivity and purity, suitable for large-scale industrialized production, and the like.

Description

technical field [0001] The invention relates to the separation technology of effective components of traditional Chinese medicinal materials, in particular to a simple method for preparing pedicel glucoside from jiubing. Background technique [0002] Jiubiying is the dry bark of Ilex rotunda Thunb., which was first recorded in "Lingnan Herbal Collection", and is now included in "Pharmacopoeia of the People's Republic of China" (2015 edition one), which is the first part of Lingnan Thunb in my country. Commonly used Chinese herbal medicine. The medicinal material is bitter and cool in nature, and has the effects of clearing away heat and detoxification, promoting dampness and relieving pain. It is often used to treat summer-heat-damp fever, sore throat, damp-heat diarrhea, abdominal distension and pain, rheumatic arthralgia, eczema, boils, and bruises. Jubiying contains many chemical components such as syringin, pelicin, and bibingacid. Among them, pedicel glucoside is rich ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J63/00C07H15/256C07H1/08
CPCC07H1/08C07H15/256C07J63/008
Inventor 王永刚严曾豪苏敏敏潘文俊彭维
Owner SUN YAT SEN UNIV
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