Method for extracting kaempferitrin from prunus cerasifera leaves

A technology of kaempferol and purple leaf plum is applied in the field of natural product chemistry to achieve the effects of large processing capacity and low extraction cost

Inactive Publication Date: 2013-01-16
WUHAN POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The original species is produced in southwestern Asia, and now our country is widely planted and rich in resources, and its leaves are rich in kaempferol, but there is no economical method for extracting and separating kaempferol from the leaves of purple leaf plum

Method used

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  • Method for extracting kaempferitrin from prunus cerasifera leaves
  • Method for extracting kaempferitrin from prunus cerasifera leaves
  • Method for extracting kaempferitrin from prunus cerasifera leaves

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1. Weigh 200g of dried purple-leaf plum leaves and crush them. Put the 40-mesh sieve into a 5000ml beaker, add 2000ml of 70% (V / V) ethanol aqueous solution, seal it with plastic wrap, and place it at room temperature for 12 hours. Min speed stirring 2h, filter, collect the filtrate.

[0023] Add 1000ml of 70% (V / V) ethanol water solution to the filter cake, stir at 600r / min for 20min, and then filter. The filter cake is treated once more according to the above method, and the above three filtrates are combined to obtain the extract.

[0024] 2. Concentrate the extract solution in a water bath at 59°C under reduced pressure to 500ml, place it at 2°C for 12 hours, centrifuge (4000r / min, 30min) to remove most of the fat-soluble substances to obtain a centrifuge solution, and distill the centrifuge solution with distilled water Dilute to 2000ml.

[0025] 3. Chromatography on a macroporous resin column at a flow rate of 3ml / min (HPD400A macroporous adsorption resin from Zhe...

Embodiment 2

[0035] Steps 1 and 2 are the same as in Example 1.

[0036] 3. Chromatography on a macroporous resin column at a flow rate of 4ml / min (HPD400A macroporous adsorption resin from Zhengzhou Qinshi Technology Co., Ltd., with a specific surface area of ​​500-550m 2 / g, the polarity is medium polarity, the glass column model is Φ3.0*L100cm), at the same flow rate, wash the column with 3000ml distilled water.

[0037] 4. Use 30% (V / V) ethanol aqueous solution to wash kaempferol from the column at a flow rate of 5ml / min, and collect the fraction between 550 and 1250ml behind the column.

[0038] 5. The distillate was crystallized at 3°C ​​for 8 days, and filtered after crystallization to obtain the crude crystalline product and mother liquor.

[0039] 6. The crude product of the crystalline substance was washed with water and vacuum-dried at room temperature to obtain the kaempferi product (qualified and quantified by HPLC external standard method, its content ≥ 98%). Step 3, repeat...

Embodiment 3

[0042] Steps 1 and 2 are the same as in Example 1.

[0043] 3. Chromatography on a macroporous resin column at a flow rate of 5ml / min (HPD400A macroporous adsorption resin from Zhengzhou Qinshi Technology Co., Ltd., with a specific surface area of ​​500-550m 2 / g, the polarity is medium polarity, the glass column model is Φ3.0*L100cm), at the same flow rate, wash the column with 3000ml distilled water.

[0044]4. Use 30% (V / V) ethanol aqueous solution to wash kaempferol from the column at a flow rate of 5ml / min, and collect the fraction between 550 and 1250ml behind the column.

[0045] 5. The distillate was crystallized at 0°C for 7 days, and filtered after crystallization to obtain the crude crystalline product and mother liquor.

[0046] 6. The crude product of the crystalline substance was washed with water and vacuum-dried at room temperature to obtain the kaempferi product (qualified and quantified by HPLC external standard method, its content ≥ 98%). Step 3, repeating...

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Abstract

The invention discloses a method for extracting kaempferitrin from prunus cerasifera leaves. The method includes using an ethanol water solution to extract the prunus cerasifera leaves, concentrating the prunus cerasifera leaves under reduced pressure, stewing a concentrated solution at the temperature of 2-5 DEG C for 12-24 hours, and performing centrifugal separation to remove precipitation matters; distilling a centrifuged liquid by using distilled water, adding a macroporous resin column for primary separation, eluting most of coloring matters by using distilled water, then eluting the coloring matters by using the ethanol water solution with volume by volume concentration of 20%-33%, and collecting effective post-column fraction liquids; placing the effective fraction liquids at the temperature of -6-5 DEG C for 6-8 days for crystallization, and performing filtering after crystallization to obtain coarse crystallized products and mother solutions; and subjecting the coarse crystallized products to washing and vacuum drying at room temperatures to obtain kaempferitrin products, wherein the specific surface area of macroporous resins with medium polarity is 500-800m<2> / g. According to the method, a large dose of columns are added for primary separation and crystallization for further purification so that kaempferitrin crystals with large yield and high purity can be obtained, throughput of a single batch is large, and extracting costs are low.

Description

technical field [0001] The invention belongs to the technical field of natural product chemistry, and in particular relates to a method for extracting kaempferol from the leaves of purple-leaved plums. Background technique [0002] Kaempferol, alias: kaempferol-3,7-O-L-dirhamnoside, the English name is Kaempferitrin; Kaempferol 3,7-L-dirhamnoside, molecular formula: C 27 h 30 o 14 , molecular weight: 578.57, CAS No. 482-38-2, according to literature reports, this substance can lower blood sugar, resist fatigue, clear away heat and detoxify, reduce swelling and relieve pain. Pharmacological effects such as oxidants. The extraction of kaempferen mainly uses the dried root of Bupleurum chinense DC or Bupleurum scorzonerifolium Willd. as the raw material. The corresponding products were obtained after chromatographic separation and freeze-drying. Since there is no better crystallization and purification method for kaempferrin at present, in the chromatographic separation, c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07H1/08
Inventor 吴波
Owner WUHAN POLYTECHNIC UNIVERSITY
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