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Method for extracting chlorogenic acid and caffeic acid from coffee beans

A technology for coffee beans and chlorogenic acid, which is applied in the separation/purification of carboxylic acid esters, the separation/purification of carboxylic acid compounds, organic chemistry, etc. Convenience, improved filtration speed, low price effect

Active Publication Date: 2015-12-23
湖南楚宏生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, coffee bean acid water is used directly to extract chlorogenic acid, because coffee beans contain a lot of lipids, which will affect the extraction of chlorogenic acid and caffeic acid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Grind the dried coffee bean raw material to 10-20 mesh, weigh 100KG and add 600L ether for cold extraction for 3-4 hours; filter the coffee bean residue and ether-containing solution once with a ceramic membrane, and carry out the ether-containing solution at 40 Concentrate under reduced pressure at ~50°C, recover ether, and obtain 15kg of coffee bean fat; mix 70kg of coffee bean residue with 400L of acetone solution (made by mixing 320L of acetone with 80L of 0.001mol / L hydrochloric acid aqueous solution, etc.) and mix at room temperature Leaching, the time is 3-5 hours; the filtrate is obtained by filtering the ceramic membrane once, and the obtained filtrate is concentrated under reduced pressure, acetone is recovered, and 60L of extract Ⅰ is obtained; the extract Ⅰ is directly applied to NKA-9 macroporous adsorption resin for After 30 minutes, elute with 10% ethanol solution of 2BV upper column solution, discard the eluent, and then elute with 20% ethanol aqueous sol...

Embodiment 2

[0035] Grind the dried coffee bean raw material to 10-20 mesh, weigh 200KG and add 1200L ether for cold extraction for 3-4 hours; filter the coffee bean residue and ether-containing solution once with a ceramic membrane, and carry out the ether-containing solution at 40 Concentrate under reduced pressure at ~50°C, recover ether, and obtain 35kg of coffee bean fat; mix 100kg of coffee bean residue with 600L of acetone solution (made by mixing 480L of acetone with 120L of 0.001mol / L hydrochloric acid aqueous solution, etc.) and mix at room temperature Leaching, the time is 3-5 hours; the filtrate is obtained by filtering the ceramic membrane once, and the obtained filtrate is concentrated under reduced pressure to recover acetone and obtain 100L extract I; the extract I is directly applied to NKA-9 macroporous adsorption resin for adsorption After 30min, elute with 10% ethanol solution of 2BV upper column solution, discard the eluent, and then elute with 20% ethanol aqueous solut...

Embodiment 3

[0037] Grind the dried coffee bean raw material to 10-20 mesh, weigh 400KG and add 2000L ether for cold extraction for 3-4 hours; filter the coffee bean residue and ether-containing solution once with a ceramic membrane, and carry out the ether-containing solution at 40 Concentrate under reduced pressure at ~50°C, recover ether, and obtain 70kg of coffee bean fat; mix 200kg of coffee bean residue with 1200L of acetone solution (made by mixing 960L of acetone with 240L of 0.001mol / L hydrochloric acid aqueous solution, etc.) and mix at room temperature Leaching, the time is 3-5 hours; the filtrate is obtained by filtering the ceramic membrane once, and the obtained filtrate is concentrated under reduced pressure, acetone is recovered, and 200L extract Ⅰ is obtained; the extract Ⅰ is directly applied to NKA-9 macroporous adsorption resin for adsorption After 30 min, elute with 10% ethanol solution of 2BV upper column solution, discard the eluent, and then elute with 20% ethanol aq...

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Abstract

The invention provides a method for extracting chlorogenic acid and caffeic acid from coffee beans. The whole set of method is put forward for extracting high-purity chlorogenic acid and caffeic acid from coffee beans by conducting degreasing, conducting pyruvic acid water extraction, making the mixture pass through large-hole adsorption resin, conducting concentration, conducting extraction through ethyl acetate, conducting decoloration through activated carbon, and conducting crystallization and recrystallization. The requirement of the whole separation process for environment conditions is not high, the separation time is short, and purity is the highest. Separation materials can be easily obtained and are cheap, the separation operation process is simple and easy to control, crystallization and recrystallization are adopted, the purification efficiency is high, and yield is high.

Description

Technical field [0001] The invention relates to a method for extracting high-purity chlorogenic acid and caffeic acid from coffee beans, belonging to the technical field of natural product chemistry. Background technique [0002] Chlorogenic acid, alias: chlorogenic acid, coffee tannin, (1S, 3R, 4R, 5R)-3-[[3-(3,4-dihydroxyphenyl)-1-oxo-2-propenyl ]oxy]-1,4,5-trihydroxycyclohexanecarboxylic acid; systematic name: 1,3,4,5-tetrahydroxycyclohexanecarboxylic acid-(3,4-dihydroxycinnamate); chemical name : 3-O-caffeoylquinic acid (3-O-caffeoylquinic acid), plant source: Lonicera japonica Thumb., Lonicera hypoglauca Miq., Lonicera confusa DC. or Lonicera japonica Rehd.'s dry flower buds or With first flowers and Eucommia leaves. Chlorogenic acid hemihydrate is white or yellowish needle-like crystals, which become anhydrous at 110°C, co-heated with dilute hydrochloric acid to produce caffeic acid, melting point 208°C, specific rotation *α+D=352°(C =28). The solubility of chlorog...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/732C07C67/48C07C51/42C07C59/52
CPCC07C51/42C07C67/48C07C69/732C07C59/52
Inventor 向华唐克华唐忠海
Owner 湖南楚宏生物科技有限公司
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