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Method for simultaneously preparing chlorogenic acid and luteoloside from honeysuckle flower

A technology of luteolin and chlorogenic acid, which is applied to chemical instruments and methods, preparation of carboxylic acid esters, preparation of sugar derivatives, etc., can solve the problems of complex process, cumbersome separation steps, high equipment cost, etc. low cost effect

Inactive Publication Date: 2011-03-16
NORTHWEST A & F UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0007] If using traditional methods (polyamide pretreatment combined with sephadex LH-20 gel chromatography purification method and preparative high-performance countercurrent chromatography (HSCCC) method) from honeysuckle Chlorogenic acid is separated and purified. Although chlorogenic acid with higher purity can be obtained, such methods often have disadvantages such as cumbersome separation steps, complicated process, and high equipment cost. Therefore, this method is difficult to be used in industrial production.
At the same time, there is no research report on the preparation of luteolin. Luteolin is a flavonoid glycoside compound. The common method for separating and preparing flavonoid glycosides is generally alkali extraction and acid precipitation, and the content of luteolin in honeysuckle is generally 0.1 %, it is obviously not suitable to use the conventional alkali extraction and acid precipitation method

Method used

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  • Method for simultaneously preparing chlorogenic acid and luteoloside from honeysuckle flower
  • Method for simultaneously preparing chlorogenic acid and luteoloside from honeysuckle flower
  • Method for simultaneously preparing chlorogenic acid and luteoloside from honeysuckle flower

Examples

Experimental program
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Effect test

Embodiment 1

[0034]Take 500 g of honeysuckle dry powder, add 10 L of ethanol with a mass fraction of 60%, ultrasonically extract 3 times, each time for 30 minutes, combine the extracts, filter the extracts and remove the filter residue, concentrate the filtrate to a brown-red viscous extract; Dissolve the extract in 6 deionized water for 3 times, filter, and pass the filtrate through a D101 macroporous resin column at a flow rate of 3 times the column volume / hour, absorb for 10 hours, and elute with deionized water for 3 hours at a flow rate of 4 times the column volume / hour , and then eluted with 10% ethanol with a mass fraction of pH=6, 20% ethanol with a mass fraction of 20% ethanol at a flow rate of 2 times column volume / hour for 3 h, and then eluted with 30% ethanol with a mass fraction of pH=6, The mass fraction of 40% ethanol was eluted at a flow rate of 2 times column volume / hour for 4 hours, and finally 95% mass fraction of ethanol was used for elution at a flow rate of 5 times col...

Embodiment 2

[0038] Take 500 g of honeysuckle dry powder, add 15 L of ethanol with a mass fraction of 70%, ultrasonically extract 3 times, each time for 30 minutes, combine the extracts, filter the extracts and remove the filter residue, concentrate the filtrate to brown-red viscous extract, use pH = 6 deionized water to dissolve the extract for 3 times, filtered, and the filtrate passed through the D101 macroporous resin column at a flow rate of 3 times column volume / hour, adsorbed for 9 hours, and eluted with deionized water at a flow rate of 4 times column volume / hour for 2.5 h, then elute with 10% ethanol with a mass fraction of pH=6 and 20% ethanol with a mass fraction of 20% at a flow rate of 3 times column volume / hour for 3 h, and then use 30% ethanol with a mass fraction of pH=6 and 40% ethanol at a flow rate of 2.5 column volumes / hour for 4 hours, and finally 95% ethanol at a flow rate of 5 column volumes / hour for 4 hours.

[0039] The ethanol eluate with a mass fraction of 10% an...

Embodiment 3

[0042] Refer to attached figure 1 , take 800g of honeysuckle dry powder, add 12L of ethanol with a mass fraction of 65%, ultrasonically extract 3 times, each time for 30min, combine the extract, remove the filter residue after filtering the extract, concentrate the filtrate to brown-red viscous extract, use pH =6 deionized water to dissolve the extract for 3 times, filter, and the filtrate passes through a D101 type macroporous resin column at a flow rate of 3 times column volume / hour, absorb for 11 hours, and elute with deionized water at a flow rate of 4 times column volume / hour 3h, then elute with 10% ethanol with a mass fraction of pH=6 and 20% ethanol with a mass fraction of 20% at a flow rate of 3 times column volume / hour for 4h, and then use 30% ethanol with a mass fraction of pH=6 and 40% ethanol at a flow rate of 3 column volumes / hour for 3 hours, and finally with 95% ethanol at a flow rate of 5 column volumes / hour for 4 hours.

[0043] The ethanol eluate with a mas...

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Abstract

The invention discloses a method for simultaneously preparing chlorogenic acid and luteoloside from honeysuckle flower, which comprises the following steps of: extracting by using ethanol, enriching by using D101 macroporous resin, separating and purifying by using a silicagel column and a polyamide column, recrystallizing and the like. In the method, the chlorogenic acid and the luteoloside are extracted from the honeysuckle flower by a hot ethanol solvent extraction method; the aims of enriching the chlorogenic acid and the luteoloside and separating the chlorogenic acid from the luteoloside are fulfilled by regulating the concentration and pH value of eluent used by the macroporous resin; and the chlorogenic acid and the luteoloside are subjected to silicagel column chromatography, polyamide column chromatography and recrystallization respectively to form the chlorogenic acid and the luteoloside with the purity of over 95 percent.

Description

technical field [0001] The invention belongs to the field of preparation of biochemical articles, and relates to a method for simultaneously preparing chlorogenic acid and luteolin from honeysuckle. Background technique [0002] Honeysuckle (Chinese honeysuckle, Flos Lonicerae ) for Honeysuckle ( Caprifoliaceae ) Honeysuckle ( Lonicera ) plant honeysuckle ( Lonicera.japonica Thunb .) is a commonly used traditional Chinese medicine, which has the functions of clearing away heat and detoxification, cooling wind to dissipate heat, anti-virus, protecting liver and gallbladder, and is a green natural product with the same source of medicine and food. [0003] The main components of honeysuckle are organic acids, flavonoids, volatile oils, triterpene glycosides, iridoid glycosides, and ceramide compounds. Among them, chlorogenic acid is a polar organic acid, which is easily soluble in polar solvents such as water, ethanol, acetone, methanol, etc., and luteolin is a flavonoi...

Claims

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Application Information

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IPC IPC(8): C07C69/732C07C67/56C07H17/07C07H1/08
Inventor 张树军李娜高鹏吴进张继文王俊儒
Owner NORTHWEST A & F UNIV
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