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Method for refining chlorogenic acid from honeysuckle crude extract

A technology for crude honeysuckle extract and honeysuckle extract, which is applied in the field of extracting chlorogenic acid and achieves the effects of large processing capacity, continuous and simple operation, and shortening of preparation time.

Active Publication Date: 2015-03-18
YANTAI INST OF COASTAL ZONE RES CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the method of preparing high-purity chlorogenic acid by medium-pressure liquid chromatography is the first report

Method used

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  • Method for refining chlorogenic acid from honeysuckle crude extract
  • Method for refining chlorogenic acid from honeysuckle crude extract
  • Method for refining chlorogenic acid from honeysuckle crude extract

Examples

Experimental program
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Effect test

Embodiment 1

[0034] (1) D3520 type macroporous resin column impurity removal process

[0035] 100g of honeysuckle extract was dissolved in 1000mL deionized water, and after fully stirring, it was prepared into an aqueous solution of honeysuckle extract (the HPLC figure of chlorogenic acid in the aqueous solution is shown in figure 1 As shown), the above aqueous solution is passed through a D3520 macroporous resin column at a flow rate of 5BV / h to remove impurities such as flavonoids and sugars, and the effluent is collected. The HPLC diagram of chlorogenic acid in the effluent is shown in figure 2 shown.

[0036] (2) ADS-F8 macroporous resin column enrichment and purification process

[0037] Pass the effluent collected in step (1) directly through the ADS-F8 macroporous resin column at a flow rate of 5BV / h. After the dynamic adsorption is saturated, rinse the above macroporous resin column with deionized water at a flow rate of 2BV / h until the The liquid is colorless, and then eluted w...

Embodiment 2

[0043] (1) D4006 type macroporous resin column impurity removal process

[0044] Dissolve 500g of honeysuckle extract with 5000mL of deionized water, and after fully stirring, prepare an aqueous solution of honeysuckle extract, pass the above aqueous solution through a D4006 macroporous resin column at a flow rate of 3BV / h to remove impurities such as flavonoids and sugars, and collect the effluent liquid.

[0045] (2) Enrichment and purification process of NKA macroporous resin column

[0046] Pass the effluent collected in step (1) directly through the NKA macroporous resin column at a flow rate of 3BV / h. After the dynamic adsorption is saturated, rinse the above macroporous resin column with deionized water at a flow rate of 4BV / h until the effluent color, and then eluted with 50% ethanol aqueous solution at a flow rate of 8BV / h, collected the eluate until no chlorogenic acid was detected by HPLC, and finally concentrated the collected eluate under reduced pressure to obta...

Embodiment 3

[0052] (1) H103 macroporous resin column impurity removal process

[0053]Dissolve 1000g of honeysuckle extract with 10000mL of deionized water, and after fully stirring, prepare an aqueous solution of honeysuckle extract, pass the above aqueous solution through a H103 macroporous resin column at a flow rate of 4BV / h to remove impurities such as flavonoids and sugars, and collect the effluent liquid.

[0054] (2) S-8 macroporous resin column enrichment and purification process

[0055] Pass the effluent collected in step (1) directly through the S-8 macroporous resin column at a flow rate of 4BV / h. After the dynamic adsorption is saturated, rinse the above macroporous resin column with deionized water at a flow rate of 6BV / h until the The liquid is colorless, and then eluted with 60% ethanol aqueous solution at a flow rate of 7BV / h, collects the eluate until no chlorogenic acid is detected by HPLC, and finally concentrates the collected eluate under reduced pressure to obtain...

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Abstract

The invention relates to a method for extracting chlorogenic acid, and in particular relates to a method for refining chlorogenic acid from a honeysuckle crude extract. The method specifically comprises the following processes: a process of removing impurities by adopting a macroporous resin column A, a macroporous resin column B enrichment and purification process and a middle-pressure liquid chromatography (MPLC) refining process. The method comprises the following steps: by adopting a honeysuckle crude extract as a raw material, fully dissolving the raw material by using deionized water to prepare an aqueous solution of the honeysuckle crude extract, removing the impurities of the aqueous solution by virtue of macroporous resin column A adsorption, enabling an effluent liquid to directly pass through a macroporous resin column B, performing dynamic adsorption and saturation, feeding an impurity washing liquid to wash the impurities until the effluent liquid is colorless, eluting macroporous resin B by using an eluent until high performance liquid chromatography (HPLC) detects that no chlorogenic acid flows out, collecting the eluent, performing reduced pressure concentration on the eluent, and performing gradient elution by virtue of the MPLC provided with a C18 reverse phase silica gel column to prepare a chlorogenic acid product with the purity of more than 98%. According to the method disclosed by the invention, a process of preparing high-purity chlorogenic acid by using the MPLC is proposed for the first time; and the method is large in sample treatment quantity and simple to operate, and is suitable for large-scale preparation.

Description

technical field [0001] The invention relates to a method for extracting chlorogenic acid, in particular to a method for refining chlorogenic acid from crude honeysuckle extracts. Background technique [0002] Honeysuckle, also known as honeysuckle, is a perennial semi-evergreen winding woody vine of the Lonicera family. Honeysuckle is a dry flower bud or a flower that just opened, and it is widely distributed in the three northeastern provinces of my country, Guangdong, Hainan, Shandong, and the Himalayas. Honeysuckle is sweet and cold, clearing away heat without injuring the stomach. Its fragrance can dispel pathogenic factors and disperse wind and heat. [0003] Chlorogenic acid is the characteristic active ingredient of honeysuckle, which has the functions of antibacterial, antiviral and antifungal, and enhancing the body's defense function. The refining methods of chlorogenic acid in traditional Chinese medicine preparations mainly include organic solvent extraction, r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/732C07C67/56
CPCC07C67/56C07C2601/14C07C69/732
Inventor 夏传海孙鹏程王建华孔娜娜
Owner YANTAI INST OF COASTAL ZONE RES CHINESE ACAD OF SCI
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