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Robinin preparation method

A technology of locust glycoside and locust flower, applied in the field of preparation of locust glucoside, which can solve the problems of low product purity and easy destruction of glycoside structure, and achieve the effect of high content, high purity and good crystal form

Inactive Publication Date: 2012-05-30
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This invention needs to be adjusted with acid and lye, which easily destroys the structure of glycosides, and the resulting product has low purity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Take 5kg of dried Robinia pseudoacacia flower medicinal material, crush it to 20 mesh, reflux extract with 30L 95% ethanol solution for 3h, extract twice, filter while hot, combine the extract, concentrate the extract under reduced pressure to syrupy state, add 950ml of hot water to dissolve, then add 5g of activated carbon, stirred and decolorized, filtered to obtain decolorized solution, adsorbed on a 5LHZ816 macroporous resin column on the decolorized solution, controlled the flow rate of the upper column to 1 / 2BV / h, first washed with 10L water to remove impurities, and the flow rate was 3BV / h, and then sequentially used 15L30% , 12L 50% and 18L 85% ethanol solution elution, the elution flow rate is 2.5BV / h, collect 85% ethanol eluent, recover under reduced pressure until there is no alcohol smell, separate out, filter to obtain 61g of crude glycoside, the above crude glycoside is dissolved with pyridine, Add water dropwise until turbidity appears, let the crystals st...

Embodiment 2

[0021] Take 5kg of dried Robinia pseudoacacia medicinal material, crush it to 20 mesh, reflux extract with 50L of 90% ethanol solution for 1.5h, extract 4 times, filter while hot, combine the extract, concentrate the extract under reduced pressure to syrupy state, add 800ml of hot water to dissolve, and then Add 8g of activated carbon, stir for decolorization, and filter to obtain a decolorization solution. The decolorization solution is adsorbed on a 5LADS-7 macroporous resin column, and the flow rate of the upper column is controlled to be 1 / 3BV / h. Elute with 12L 25%, 12L 40% and 15L 75% ethanol solution, the elution flow rate is 2.5BV / h, collect the 75% ethanol eluate, recover under reduced pressure until there is no alcohol smell, precipitate, filter to obtain 59.5g of crude glycoside, the above crude glycoside Dissolve it with pyridine, add water dropwise until it becomes turbid, let the crystals stand, filter out the crystals, and dry to obtain 55.2 g of acaciaside produc...

Embodiment 3

[0023] Take 5kg of dried Robinia pseudoacacia flower medicinal material, crush it to 20 mesh, reflux extract with 35L 99% ethanol solution for 1 hour, extract 3 times, filter while hot, combine the extract, concentrate the extract under reduced pressure to syrupy state, add 900ml of hot water to dissolve, then add 8g activated carbon, stirred for decolorization, filtered to obtain decolorization solution, adsorbed on 5LADS-7 macroporous resin column on the decolorization solution, controlled the flow rate of the upper column to 1 / 2BV / h, first washed with 12L water to remove impurities, the flow rate was 3BV / h, and then used 15L 30%, 15L 45% and 15L 80% ethanol solutions were eluted, the elution flow rate was 2.5BV / h, the 80% ethanol eluate was collected, recovered under reduced pressure until there was no alcohol smell, precipitated, filtered to obtain 69.3g of crude glycosides, the above crude glycosides were used Pyridine was dissolved, and water was added dropwise until turb...

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PUM

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Abstract

The invention relates to a robinin preparation method. The process steps of the robinin preparation method include that robinia pseudoacacia flowers are used as raw materials, and are extracted and concentrated by the aid of backflow of from 90 to 99% of alcohol, dissolved by hot water, and added with activated carbon to realize decolorization, enriched macroporous resin is injected to decoloring liquid, water and alcohol liquor is used for elution, the decoloring liquid is collected, rough robinin is obtained by means of decompression alcohol-free precipitation, and recrystalization is realized by the aid of pyridine and water. Robinin can be produced by the method, process is simple, an end product is good in crystal form and high in purity, and the product of the process meets requirements of food and medicine.

Description

Technical field: [0001] The invention relates to a method for preparing acacinin, in particular to a process for preparing high-purity acacinin by using a macroporous resin. Background technique: [0002] Robinia pseudoacacia is the flower of the legume plant Robinia pseudoacacia, Robinia pseudoacacia, also known as acacia and Huteng. Robinia pseudoacacia is used as medicine, which has the functions of eliminating carbuncle, treating hemorrhoids, invigorating stomach and clearing intestines, etc. The content of acacia glycoside in Robinia pseudoacacia is 0.5%-5%. [0003] Locustside, acaciatin-7-rhamnoglucoside, also known as locustside, is soluble in hot water and hot ethanol, but almost insoluble in ether. Animal experiments have shown diuretic, strong, anti-inflammatory effects. Clinically used to treat acute and chronic nephritis, uremia, renal hypertension, cystitis and other urinary system diseases. [0004] Existing techniques for extracting and purifying acaciasid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07H1/08
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司
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