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Two-step simultaneous preparation method for pedunculoside and syringin

A technology for hollyrin and syringin, which is applied in chemical instruments and methods, preparation of sugar derivatives, steroids, etc., can solve the problems of loss of syringin, high cost, long purification process, etc., and achieves high efficiency of the method. Reasonable, less reagent dosage, short purification cycle

Active Publication Date: 2013-10-16
陕西中药研究所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Patent CN101033245 discloses a preparation method and application of glucoside, which is to rescue Bing coarse powder and extract it with ethanol reflux to obtain glucoside with a purity of 98%, but syringin is lost
[0007] To sum up, in the process of extracting and separating pelicin and syringin, there are generally problems such as large loss of pelicin and lilac, long purification process, high toxicity of solvent residues, and high cost.

Method used

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  • Two-step simultaneous preparation method for pedunculoside and syringin
  • Two-step simultaneous preparation method for pedunculoside and syringin

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Two-step method for simultaneously preparing the method for pedicel glucoside and syringin, comprising the following steps:

[0031] 1) Take 1kg of dried jiubing medicinal material, add 12L of 40% ethanol aqueous solution, reflux extraction 3 times, each time for 1h, combine the extracts, concentrate under reduced pressure to recover ethanol, concentrate until the concentration of the extract is 0.25g / mL, after standing for 24 hours, filter, and collect the filter residue and filtrate respectively;

[0032] 2) Dry the filter residue under reduced pressure to obtain the crude pedicel glucoside. After dissolving the crude product in methanol, put it in a water bath at 60°C to make it reach a supersaturated solution, and then let it stand at room temperature for 48 hours until crystallization occurs. , the crystals are filtered and dried under reduced pressure to obtain 7.4g of product, which is detected by comparison with a standard test, see figure 2 , the product is ...

Embodiment 2

[0036] Two-step method for preparing the method for pedicel glucoside and syringin simultaneously, comprising the following steps:

[0037] 1) Take 2kg of dried jiubing medicinal materials, add 12L of 30% ethanol aqueous solution, reflux extraction 3 times, 1.5h each time, combine the extracts, concentrate under reduced pressure to recover ethanol, concentrate until the concentration of the extract is 0.20g / mL, after standing for 24h, filter, and collect the filter residue and filtrate respectively;

[0038] 2) Dry the filter residue under reduced pressure to obtain the crude catechin glucoside. After dissolving the crude product in methanol, put it in a water bath at 70°C to make it reach a supersaturated solution, and then let it stand at room temperature for 48 hours until crystallization occurs. , the crystals were filtered and dried under reduced pressure to obtain 13.1g of product with a purity of 98.1%;

[0039]3) The filtrate obtained in step 1) was separated by colu...

Embodiment 3

[0041] Two-step method for simultaneously preparing the method for pedicel glucoside and syringin, comprising the following steps:

[0042] 1) Take 2.5kg of dried jiubing medicinal materials, add 18L of ethanol aqueous solution with a volume fraction of 40%, reflux extraction 3 times, each time for 1h, combine the extracts, concentrate under reduced pressure to recover ethanol, and concentrate until the concentration of the extract is 0.10g / mL, after standing for 24h, filter, and collect the filter residue and filtrate respectively;

[0043] 2) Dry the filter residue under reduced pressure to obtain crude pedicel glucoside. After dissolving the crude product in methanol, put it in a water bath at 50°C to make it reach a supersaturated solution, and then let it stand at room temperature for 48 hours until crystallization occurs. , the crystals were filtered and dried under reduced pressure to obtain 16.2g of product with a purity of 98.4%;

[0044] 3) The filtrate obtained in...

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Abstract

The invention discloses a two-step simultaneous preparation method for pedunculoside and syringin and belongs to the technical field of natural product extraction and separation. The method comprises the following steps: adding 20-70% (volume fraction) of ethanol water into ovate leaf holly bark, performing reflux extraction, collecting an extracting solution, standing and filtering the extracting solution, and respectively collecting filtrate and residues; 2 drying the residues to obtain crude pedunculoside, and purifying the pedunculoside to obtain the pedunculoside; 3, performing column chromatography separation to the filtrate with macroreticular resin, taking an ethanol-water system as an eluting agent to conduct gradient elution, concentrating and drying elution components to obtain crude syringin, purifying the crude syringin to obtain the syringin. The method is simple and feasible, has a short separation time and high separating efficiency, the purity of the pedunculoside and the purity of syringin can both reach more than 98%, and the method is suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of extraction and separation of natural products, and in particular relates to a two-step method for simultaneously preparing pelicin and syringin. Background technique [0002] Jiubiying is the dry bark of Ilex rotunda Thunb., a plant of the Ilex family, which was first recorded in "Lingnan Collection of Medicines". Iron holly grows in sparse forests at the foot of the mountain or beside ditches and streams, and is distributed in Jiangsu, Anhui, Zhejiang, Jiangxi, Fujian, Taiwan, Hunan, Guangdong, Guangxi, and Yunnan. It is a commonly used herbal medicine in southern my country. It has the effects of clearing away heat and detoxification, promoting dampness and relieving pain. It is often used to treat heat-damp fever, sore throat, damp-heat diarrhea, abdominal distension and pain, rheumatic arthralgia, eczema, boils, and bruises. [0003] Among the active ingredients in Jiubiying, the contents of pelicin ...

Claims

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Application Information

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IPC IPC(8): C07J63/00C07H15/203C07H1/08
Inventor 张俏曹爱兰朱爱华史文静杜文娟
Owner 陕西中药研究所
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