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Method for preparing hyperoside and isoquercitrin simultaneously from dogbane leaves

A technology of isoquercitrin and hyperoside, which is applied in the fields of chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve problems such as unsuitable for large-scale production, low product yield, complicated process, etc. Achieve the effect of fast adsorption speed, large adsorption capacity and simple operation method

Active Publication Date: 2013-02-13
YANTAI INST OF COASTAL ZONE RES CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the method simultaneously prepares hyperoside and isorhamnetin-3-O-galactoside, the method also has the disadvantages of small amount of treatment and low efficiency.
Chinese patent 200610054268.9 discloses the "preparation method of hyperin and hypericin in Hypericum perforatum", using Hypericum perforatum as raw material, using CTAB reverse micellar extraction to obtain hyperin and hypericin, the process is complicated , low product yield, not suitable for large-scale production

Method used

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  • Method for preparing hyperoside and isoquercitrin simultaneously from dogbane leaves
  • Method for preparing hyperoside and isoquercitrin simultaneously from dogbane leaves
  • Method for preparing hyperoside and isoquercitrin simultaneously from dogbane leaves

Examples

Experimental program
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Effect test

Embodiment 1

[0036] (1) Extraction: take 500g of Apocynum basil leaves, dry and pulverize them, add 5L of methanol with a volume fraction of 70%, heat and reflux for extraction 3 times, each time for 2 hours, combine the extracts, filter the extracts, concentrate under reduced pressure and recover the organic solvent to obtain Extract, add water to dissolve the extract, extract 3 times with an equal volume of petroleum ether after dissolving, dilute the water phase after extraction to a concentration of 10g / L, and mix well to obtain the intermediate product A. Its high-performance liquid chromatogram is as follows: figure 1 .

[0037](2) Separation of macroporous resins: Pass the intermediate product A at a flow rate of 3BV / h through AB-8 resin columns filled with 3-stage serial series treated according to conventional methods, and dynamically adsorb to saturation, wherein each series of macroporous adsorption resins The diameter-to-height ratio of the column is 1:8. Rinse the series adso...

Embodiment 2

[0043] (1) Extraction: dry and pulverize 1Kg of apocynum leaves, add 15L of 85% methanol, heat and reflux 3 times, 3 hours each time, combine the extracts, filter the extracts, concentrate under reduced pressure and recover the organic solvent to obtain extracts, extracts Add water to dissolve, extract 4 times with an equal volume of petroleum ether, dilute the aqueous phase to a concentration of 8g / L, and mix well to obtain the intermediate product A.

[0044] (2) Separation of macroporous resin: pass the intermediate product A at a flow rate of 3BV / h through a resin column filled with a combination of AB-8 and X-5 treated in a conventional manner in four stages in series, and dynamically adsorb to saturation. The diameter-to-height ratio of the macroporous adsorption resin columns connected in series is 1:10. Rinse the combined resin column of AB-8 and X-5 with distilled water at a flow rate of 7BV / h, and elute until no impurities flow out. Rinse the tandem resin column wit...

Embodiment 3

[0048] (1) Extraction: 5Kg of apocynum leaves were dried and pulverized, added 50L of 85% methanol, extracted 3 times by ultrasound, 1 hour each time, combined the extracts, filtered the extracts, concentrated under reduced pressure and recovered organic solvents to obtain extracts, extracts Add water to dissolve, extract 4 times with an equal volume of petroleum ether, dilute the water phase to a concentration of 10g / L, and mix thoroughly to obtain the intermediate product A.

[0049] (2) Separation of macroporous resins: Pass the intermediate product A at a flow rate of 5BV / h through AB-8 resin columns filled with 5 stages in series treated according to conventional methods, and dynamically adsorb to saturation, in which each series of macroporous adsorption resins The diameter-to-height ratio of the column is 1:6. Rinse the AB-8 macroporous resin series adsorption column with distilled water at a flow rate of 10BV / h, and elute until no impurities flow out. Rinse the tandem...

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Abstract

The method relates to a method for preparing hyperoside and isoquercitrin simultaneously from dogbane leaves. The method includes subjecting the dogbane leaves which serve as a raw material to heating reflux or ultrasonic extraction, and obtaining an extract after decompressing concentration; adding water to the extract for dissolution, and removing pigment and fat soluble impurities through petroleum ether; performing aqueous phase dilution, preforming dynamic adsorption until saturation through at least three serially connected macroporous adsorption resin columns, feeding an eluting solution for elution, then performing elution through the eluting solution until no hyperoside and isoquercitrin flowing out, and collecting the effluent liquid; and performing compressing concentration on the effluent liquid, performing recrystallization in methanol, enabling the liquid to pass through a medium-pressure gradient eluting system filled with C18 reverse phase silica gel, and obtaining the hyperoside and the isoquercitrin simultaneously whose purities reach 90%-98%. According to the method, the sample throughput is large, the operation is simple, high-purity hyperoside and isoquercitrin are prepared simultaneously, and not only the cost is low, but also the method is suitable for large-scale preparation.

Description

technical field [0001] The invention relates to modern separation and purification technology of traditional Chinese medicine, in particular to a method for simultaneously preparing hyperin and isoquercitrin from Apocynum apocynum leaves Background technique [0002] Apocynum venetum leaves are the dried leaves of Apocynum venetum, a perennial herb of the Apocynaceae family. It has the effects of calming the liver and calming the nerves, clearing heat and diuresis, and has a long history of medicinal and tea drinking. Modern pharmacological research shows that apocynum leaves can be used to treat diseases such as hypertension, hyperlipidemia, coronary heart disease, asthma, bronchitis, etc., and have good effects. [0003] Hyperin and isoquercitrin are the main active ingredients in Apocynum venetifolia. Hyperin, also known as quercetin-3-O-β-D-galactopyranoside, belongs to flavonol glycosides, the aglycon is quercetin, the sugar group is galactopyranose, and quercetin The...

Claims

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Application Information

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IPC IPC(8): C07H1/08C07H17/07
Inventor 夏传海孔娜娜方圣涛凌浩
Owner YANTAI INST OF COASTAL ZONE RES CHINESE ACAD OF SCI
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