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Method of preparing high-purity chlorogenic acid from burdock roots

A technology of chlorogenic acid and burdock root, which is applied in the field of extraction of high-purity chlorogenic acid, can solve the problems of low preparation amount, long preparation time, and many types of solvents in the system, and achieve improved solubility, short preparation time, and reduced production cost effect

Active Publication Date: 2017-07-04
SHANDONG AGRICULTURAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This scheme overcomes the problems of low preparation amount, long preparation time and many types of solvents required in the previous purification method, greatly improving production efficiency and reducing production cost

Method used

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  • Method of preparing high-purity chlorogenic acid from burdock roots
  • Method of preparing high-purity chlorogenic acid from burdock roots
  • Method of preparing high-purity chlorogenic acid from burdock roots

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A method for preparing high-purity chlorogenic acid from burdock root, comprising the following steps:

[0032] (1) Preparation of burdock root extract

[0033] Grind the dried slices of burdock root through a 40-mesh sieve, take a 100g sample, perform ultrasonic extraction three times with 0.1mol / L sodium hydroxide according to the ratio of solid to liquid 1:10, the time is 1.5h, 1h and 0.5h respectively, and combine the extracts ; Adjust pH to 11-12 with 0.1mol / L hydrochloric acid.

[0034] (2) Purification and enrichment

[0035] Take the burdock root extract and apply it to the diethylamine anion exchange resin chromatography column, the loading rate is 3BV / h, first use distilled water to elute at 5BV / h for 2h, and then use 0.1mol / L sodium hydroxide solution to 3BV / h was eluted for 1h, 500mL was received as a unit, and the eluents were combined; the pH was adjusted to 4-5 with 1mol / L hydrochloric acid, and an equal volume of ethyl acetate was extracted three times...

Embodiment 2

[0043] The similarities between this example and Example 1 will not be repeated, the difference is: a method for preparing high-purity chlorogenic acid from burdock root, step (3) adopts Tongtian TBE-3000C high-speed countercurrent chromatography for separation and purification For chlorogenic acid, pour ethyl acetate, methanol and water in a volume ratio of 4:0.1:4, that is, ethyl acetate 1000mL, methanol 200mL and water 1000mL into a separatory funnel, oscillate evenly, and stand still for 30 minutes for later use. Take the upper phase as the stationary phase and the lower phase as the mobile phase.

[0044] Collection of the target compound: After detecting the collected fractions, it was found that the target compound (chlorogenic acid) elutes between 25 and 43 minutes of high-speed countercurrent chromatography.

[0045] The purity of the target compound was measured by collecting the fractions between 28 and 37 minutes of high-speed countercurrent chromatography. After r...

Embodiment 3

[0047] The similarities between this embodiment and Embodiment 1 will not be repeated, and the difference is:

[0048] (1) Preparation of crude extract of burdock root:

[0049] Dry and crush the discarded outer skin of burdock root after processing through a 40-mesh sieve, sample 50 g, and ultrasonically extract with 500 mL of 1 mol / L potassium hydroxide solution for 1 h; repeat the extraction once, combine the extracts, and adjust the pH with 1 mol / L hydrochloric acid to 3-4, extracted three times with equal volume of ethyl acetate, concentrated and dried under reduced pressure to obtain 2.1 g of burdock root extract;

[0050] (2) High-speed countercurrent chromatographic separation:

[0051] Take ethyl acetate, methanol and water according to the ratio of 5:0.5:4, take 240 mg of the crude ethyl acetate extract of burdock root prepared in (1), dissolve them in 5 mL of the dissolution system composed of the upper and lower phases, and dissolve them by ultrasonic . Separati...

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Abstract

A method of separating and purifying chlorogenic acid from burdock roots includes the steps of: 1) preparation of extract liquid of burdock roots: crushing dried burdock roots and soaking the burdock roots in an alkaline solution for 30 min, and performing ultrasonic or microwave extraction to obtain an extract liquid and regulating the pH of the extract liquid to 11-12; 2) purification and enrichment: feeding the extract liquid to an anion exchange column, wherein the pack in the anion exchange column is weak-alkaline anion resin, and successively eluting the anion exchange column with distilled water to remove impurities, such as saccharides, and eluting the anion exchange column with an alkaline solution, regulating the pH value of an eluate to 2-5 with an acidic solution, isovolumetrically extracting the eluate with ethyl acetate for three times, mixing the ethyl acetate phases, and performing pressure reduced concentration and drying to obtain a burdock root extract; and 3) separating and purifying the chlorogenic acid through high-speed countercurrent chromatography. In the method, with the alkaline solution as an extraction solvent, solubility of the chlorogenic acid is greatly increased; the method is free of organic solvents for extraction and enrichment and is free of an immobilized carrier for separation process and is free of dead adsorption. The method has simple processes, is quick and high-effective, has good repeatability and is high in purity of the target compound.

Description

technical field [0001] The invention relates to a method for extracting, enriching and separating effective components from food, in particular to an extraction method for preparing high-purity chlorogenic acid from burdock root. Background technique [0002] Burdock (Arctiumlappa L.) is a biennial herbaceous plant of Compositae. It is used for both medicine and food. It was introduced from China to Japan and improved into a high-quality vegetable. It is widely planted in Fengxian County, Peixian County, Jiangsu Province, and Cangshan Mountain, Shandong Province. Burdock root is the main edible part of burdock, which has excellent health care value. It is recorded in "Compendium of Materia Medica" that it can "pass the twelve meridians, remove the evil spirits of the five internal organs", "long-term use, lighten the body and resist aging". Medical research has proved that burdock root has the effects of invigorating the spleen and stomach, clearing away heat and detoxificat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/732C07C67/28C07C67/48C07C67/56
CPCC07C67/28C07C67/48C07C67/56C07C69/732
Inventor 乔旭光郑振佳邱志常李宁阳赵瑞璇李蒙
Owner SHANDONG AGRICULTURAL UNIVERSITY
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