Method for preparing kaempferol

A technology for kaempferol and filtrate is applied in the field of recrystallization and purification of kaempferol, and in the field of enzymatic hydrolysis.

Inactive Publication Date: 2010-06-30
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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[0011] There are few literatures about the e

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  • Method for preparing kaempferol

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Embodiment 1

[0029] Grind 10kg of raw materials (2.4% equivalent content of kaempferol and its derivatives), add 80L and add 1% sodium hydroxide, stir and heat in a boiling water bath for 1.5 hours, cool, filter; add phosphoric acid to the filtrate to adjust the pH to 5, add 50g Cellulase, heat up to 40°C in a stirring heating device, stabilize for 15 hours and hydrolyze to obtain 84L hydrolyzate; heat and concentrate the hydrolyzate to 8L, add ethyl acetate to stir and extract, take the ester phase and recover ethyl acetate under reduced pressure to obtain 487g extract; the extract uses 2L 95% methanol to finally obtain 213g of kaempferol finished product with a content of 92.1%.

Embodiment 2

[0031] Grind 10kg of raw materials (3.1% equivalent content of kaempferol and its derivatives), add 90L and add 1.5% sodium hydroxide, stir and heat in a boiling water bath for 1.7 hours, cool, filter; add phosphoric acid to the filtrate to adjust the pH to 6, add 75g Amylase, heat up to 45°C in a stirring heating device, stabilize for 18 hours and hydrolyze to obtain 95L hydrolyzate; heat and concentrate the hydrolyzate to 8L, add ethyl acetate to stir and extract, take the ester phase and recover ethyl acetate under reduced pressure to obtain 506g Extract: 2.5L 85% methanol was used for the extract to finally obtain 279g of kaempferol finished product with a content of 94.3%.

Embodiment 3

[0033] Grind 10kg of raw materials (the equivalent content of kaempferol and its derivatives is 2.7%), add 100L and add 1.5% sodium hydroxide, stir and heat in a boiling water bath for 2 hours, cool, filter; add acetic acid to the filtrate to adjust the pH to 7, add 100g β-glucosidase, heat up to 50°C in a stirring heating device, stabilize for 20 hours and hydrolyze to obtain 107L hydrolyzate; heat and concentrate the hydrolyzate to 7L, add ethyl acetate to stir and extract, take the ester phase and recover ethyl acetate under reduced pressure ester, to obtain 496g of medicinal extract; 3L of 80% methanol was used for the medicinal extract to finally obtain 246g of kaempferol finished product with a content of 96.5%.

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Abstract

The invention relates to a method for separating and purifying kaempferol, which is low in cost, high in yield, short in period and easy to industrialize. The method comprises the process steps of: pulverizing raw materials containing the kaempferol, then adding 1 to 2 percent sodium hydroxide solution into the raw materials for extraction, regulating a pH value to 5 to 7 for enzymolysis, extracting enzymolysis liquid by using ethyl acetate, and after decompressing and concentrating the extraction liquid, performing three times of recrystallization by using methyl alcohol to prepare products. The kaempferol prepared by adopting the method is simple in process, high in utilization rate of the raw materials and high in purity.

Description

Technical field: [0001] The invention relates to an extraction and purification process of kaempferol, in particular to a method for purifying kaempferol by enzymolysis and recrystallization. Background technique: [0002] Kaempferol [0003] Alias: kaempferol-3, kaempferol, kaempferol, tetrahydroxyflavone, thymosin III. [0004] English name: Kaempferol [0005] CAS number: 520-18-3 [0006] Structural formula: [0007] [0008] Molecular formula and molecular weight: C 15 h 10 o 6 ;286.23 [0009] Physical properties: Kaempferol belongs to flavonols, yellow needle crystal, melting point 276°C-278°C, sensitive to light and air. Kaempferol is slightly soluble in water, soluble in hot ethanol, ether and alkali. [0010] Pharmacological action: Antibacterial, has inhibitory effect on Staphylococcus aureus, Pseudomonas aeruginosa, typhoid bacillus and Shigella. Cough, treatment of bronchitis. Inhibits enzymes, inhibits eye aldose reductase, and is beneficial to th...

Claims

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Application Information

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IPC IPC(8): C07D311/30C07D311/40C12P17/06
Inventor 刘东锋张翼杨成东
Owner NANJING ZELANG MEDICAL TECH
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