CN103497106B - Method for extracting chlorogenic acid from green coffee beans - Google Patents
Method for extracting chlorogenic acid from green coffee beans Download PDFInfo
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- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/56—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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Abstract
The invention relates to a method for extracting chlorogenic acid from green coffee beans. With the method provided by the invention, problems of high energy consumption, difficulty in absorption resin cleaning, long extraction time, low extraction rate, low product purity, and high caffeine content of existing methods can be solved. The method comprises the steps that: a raw material is crushed and is sieved by using a 10-mesh sieve; the material is subjected to ultrasonic countercurrent continuous extraction by using a 0.1% sodium sulfite water solution; the extract liquid is filtered by using a 100-mesh vibrating sieve; the liquid is subjected to horizontal screw centrifugation and disc centrifugation, and is directly subjected to XAD-16 macroporous resin absorption; loss liquid is absorbed by using LX-28 macroporous resin, when absorption is saturated, the resin is cleaned by flushing by using purified water; the resin is eluted by using 50-80% ethanol; the elution liquid is concentrated; ethanol is recovered, and spray dying is carried out. The product of XAD-16 macroporous resin elution is caffeine. The product of LX-28 macroporous resin elution is 50% chlorogenic acid, and the yield is approximately 10%. The 50% chlorogenic acid is dissolved by using 80% ethanol with an amount of 10 times; the solution is subjected to active carbon decolorization and filtration, and is concentrated to a specific weight of 1.15; the solution is settled, frozen, and crystallized; microwave dying is carried out, such that a product with a content of 90% is obtained, and the yield is higher than 3.5%.
Description
technical field:
The present invention relates to a kind of Technology of chlorogenic acid extracting from green coffee berry, especially relate to the ultrasonic countercurrent extraction of a kind of employing and the green coffee berry Content of Chlorogenic Acid of macroporous resin separation and purification, and effectively remove the processing method of caffeine.
background technology:
Green coffee berry derives from the seed of madder wort Coffea arabica, middle fruit coffee and large fruit coffee.Containing more chlorogenic acid in green coffee bean extract, therefore used by the source as a kind of effective chlorogenic acid frequently.
The intoxicated acid of contracting that chlorogenic acid (chlorogenic acid) is made up of coffic acid (caffeic acid) and quinic acid (quinic acid), chemical name 3-caffetannic acid, be described as " plant gold ", be the object that production is chased by numerous producer.Chlorogenic acid is a kind of important biologically active substance, have antibacterial, antiviral, increase white cell, hepatic cholagogic, antitumor, hypotensive, reducing blood-fat, the effect such as scavenging free radicals and stimulating central nervous system system, modern science has been deep into multiple fields such as food, health care, medicine and daily-use chemical industry to the bioactive research of chlorogenic acid.The main source of chlorogenic acid extracts from natural phant, and domestic be with the plant material such as Japanese Honeysuckle, the bark of eucommia always, abroad mainly with coffee berry etc. for raw material.At present the extracting method of chlorogenic acid is mainly contained:
1) water extraction: water extraction is the characteristic utilizing chlorogenic acid soluble in water, carries out extracting method with hot water as digestion agent.Adopt 10 times of amount of water, decoct 2 times under 50 DEG C of conditions, decoct 1.5h at every turn, obtain chlorogenic acid crude product.Water extraction technique is simple, cost is low, less investment.But energy consumption is high, the production cycle is long, wastewater flow rate is large, product purity is low.
2) organic solvent extraction: chlorogenic acid is soluble in methyl alcohol, ethanol, acetone polar solvent.With 10 times amount 70% alcohol heat reflux 1h, obtain chlorogenic acid crude product.Organic solvent extraction technique is simple, invests little, is applicable to industrialization and produces, but due to an organic solvent, increases solvent recuperation cost.
3) physical field strengthening extraction method: add as the physical field such as ultrasonic wave or microwave in conventional solvent extraction, strengthening extraction, reduce extraction time, reduces active substance degraded.Microwave power 340W, radiated time 20min, banyan agent volume fraction of ethanol 60%, ethanol consumption be 9 times, under the processing condition of soak time 30min chlorogenic acid crude product.But Industrialized processing technique is also immature at present, awaits further research.
4) macroreticular resin absorbing method: macroporous adsorbent resin is a kind of not containing cation exchange groups, the polymeric sorbent with macroporous structure, also be a kind of lipophilic substance, there is the advantages such as selectivity is good, physical strength is high, manipulation of regeneration is convenient, rate of adsorption is fast, simple to operate, constant product quality, production cost are low, so be particularly suitable for separating-purifying water-soluble cpds.CN 101704748A adopts NKA-II polar macroporous resin, sample concentration 0.26mg/mL, pH2.0, and sample introduction liquid is long-pending/and macroporous resin mass values is 12, and flow velocity is 2mL/ min, and eluent 30% ethanol, chlorogenic acid extract purity can reach 25.3%.But the method consumes time is long, cleaning polymeric adsorbent is more difficult.
Generally speaking, the method for above conventional chlorogenic acid extracting, self all also exists some defects, as: energy consumption is high, extraction time is long, extraction yield is low, and product purity is low, content of caffeine is excessively high.
Summary of the invention
The object of this invention is to provide that a kind of energy consumption is low, cleaning polymeric adsorbent is easy, extraction time is few, extraction yield is high, the method for product purity is high, content of caffeine is low from green coffee berry chlorogenic acid extracting.
The present invention is achieved in that
The method of chlorogenic acid extracting from green coffee berry, its leaching process comprises the following steps:
(1) first green coffee berry is pulverized 10 mesh sieves, obtain green coffee berry powder;
(2) adding green coffee berry powder 10 times amount mass percentage concentration is 0.1% sodium sulfite aqueous solution, ultrasonic continuous countercurrent extraction equipment extracts continuously 40 ~ 60 DEG C of ultrasonic adverse currents, sodium sulfite aqueous solution flow is 5 times of green coffee berry powder quality, obtains green coffee berry extracting solution;
(3) gained extracting solution in step (2) is shaken sieved filter, horizontal screw centrifuge, disk plate centrifuge filtration through 100 orders, obtain supernatant liquor;
(4) gained supernatant liquor in step (3) is directly poured into XAD-16 macroporous resin, the effect of XAD-16 macroporous resin is that thus selective adsorption coffee do not adsorb chlorogenic acid, and resin absorption amount and supernatant liquor are than being 1:1; Adsorbing saturated rear purified water to rinse well, is the ethanol elution of 50 ~ 80% by mass percentage concentration, and elution amount is 2 times of resin volume, collects elutriant;
(5) XAD-16 macroporous resin loss liquid in step (4) is poured into LX-28 macroporous resin, resin absorption amount and loss liquor ratio are 1:1; Adsorbing saturated rear purified water to rinse well, is the ethanol elution of 50 ~ 80% by mass percentage concentration, and elution amount is 2 times of resin volume, collects elutriant;
(6) concentrated by gained elutriant in step (4), reclaim ethanol, spraying dry obtains caffeine byproduct; Concentrated by gained elutriant in step (5), reclaim ethanol, spraying dry obtains chlorogenic acid;
(7) be the dissolve with ethanol of 80% by the chlorogenic acid in step (6) by the mass percentage concentration of its 8-10 times amount, activated carbon decolorizing is concentrated to proportion 1.15 after filtering and places freezing and crystallizing, must chlorogenic acid product after microwave drying.
Gac described in step (7) is medical needle-like gac, and consumption is 5% of chlorogenic acid quality, and temperature is 70 DEG C, and soaking time is 20 min; The proportion of crystallization is 1.10 ~ 1.15, and temperature is 0 ~ 4 DEG C.
Require in step (1) that 10 orders crossed by green coffee berry powder, scope is 10 ~ 20 orders, and too large extraction is insufficient, too thin extracting solution fluid difficulty;
Described in step (2), extracting solution is the sodium sulfite aqueous solution of 0.1%, this extracting solution, and one is the weakly alkaline that can ensure extracting solution, increases the water-soluble of chlorogenic acid.Experiment shows that the pH value of extracting solution of the present invention is 7 ~ 7.5, and not add mass percentage concentration be the extracting solution pH value of 0.1% S-WAT is 5 ~ 6, and chlorogenic acid solubleness declines 16% simultaneously.Two is prevent chlorogenic acid oxidized, and reduce the degraded of chlorogenic acid, experimental data proves: mass percentage concentration be 5% the chlorogenic acid aqueous solution 1 hour degradation rate in boiling water be 6.2%, 2 hours degradation rates be 10.7%.Mass percentage concentration be 5% the chlorogenic acid aqueous solution be 0.3%, 2 hours degradation rates at sodium sulfite aqueous solution 1 hour degradation rate that mass percentage concentration is 0.1% be 0.57%.
Described in step (2), Extracting temperature is 40 ~ 60 DEG C, and the too low extract of temperature is insufficient, and too the easy pasty state of high material, is unfavorable for fluid;
Described in step (2), extraction equipment is ultrasonic continuous countercurrent extraction equipment, and this equipment advantage is that Extracting temperature is not high, and material and extracting solution flow to contrary, improve extraction yield, effectively can reduce the oxidation of chlorogenic acid simultaneously.Compared with conventional multi-function extractor, chlorogenic acid yield brings up to 96% from 87%, and extraction effect improves more than 10%.
Filtration condition described in step (3) is the sieved filter of concussion, the centrifugal guarantee extracting solution clarification of horizontal screw centrifuge, disk plate centrifuge, and postprocessing working procedures does not block macroporous resin;
Described in described step (4), polymeric adsorbent is XAD-16 macroporous resin, and this resin to the selective absorption of caffeine in green coffee berry, and does not adsorb chlorogenic acid.On market, content 50% chlorogenic acid product content of caffeine is generally more than 5%, because caffeine can improve nerve excitability, major part client wishes that in content 50% chlorogenic acid product, caffeine is more low better, mainly use tetrachloromethane at present to reduce content of caffeine, tetrachloromethane is poisonous substances lethal quantity is 4 milliliters.The present invention selects XAD-16 macroporous resin and can solve this problem, through the chlorogenic acid product content of caffeine of the content 50% of XAD-16 process below 0.5%.
Described in described step (5), polymeric adsorbent is LX-28 macroporous resin, and this resin is low-pole resin, and energy adsorption selection chlorogenic acid, compared with other macroporous resins, it is large that LX-28 resin possesses adsorptive capacity, adsorbs very concentrated.Elutriant content is more than 50%.The product of LX-28 macroporous resin wash-out to be content be 50% chlorogenic acid, yield is about 10% (namely 1 ton of raw material goes out 100 kilograms of products).
Method of the present invention is the Technology using ultrasonic countercurrent extraction and two kinds of macroreticular resin absorbing method couplings chlorogenic acid extracting and purifying from green coffee berry, raw material pulverizing is crossed 10 orders by the present invention, by supersound extraction, adopt the sieved filter of concussion, horizontal screw centrifuge, disk plate centrifuge centrifugal, solve and adopt separately in macroporous resin adsorption method, the problem of resin cleaning difficulty; The present invention adopts XAD-16 macroporous resin selective adsorption coffee thus not adsorb chlorogenic acid, effectively reduces content of caffeine in chlorogenic acid product, solves the problem that in general resin absorption process Content of Chlorogenic Acid product, content of caffeine is high; Caffeine recoverable simultaneously; In the present invention, solvent only uses purified water and ethanol, safety and environmental protection, and the chlorogenic acid high purity 90% obtained after alcohol wash and washing are refined.Chlorogenic acid transformation efficiency is high, and product Content of Chlorogenic Acid is high.Have that extraction efficiency is high, simple to operate, production cost is low, be easy to large production application, solvent only uses purified water and ethanol, safety and environmental protection, the feature such as in the chlorogenic acid product of 50% content of caffeine is very low.
accompanying drawing illustrates:
Fig. 1 is present invention process schema.
embodiment:
Embodiment 1:
Technological method of the present invention mainly comprises the steps:
Material prepares: green coffee bean powder is broken into 15 object powder;
1. supersound extraction: extract continuously by 8 times amount sodium sulfite aqueous solutions (mass percentage concentration is 0.1%), 50 DEG C of ultrasonic adverse currents, discharge is 5 times of quality of material, obtains green coffee berry extracting solution;
2. centrifuging: supersound extraction liquid is shaken sieved filter, horizontal screw centrifuge, disk plate centrifuge filtration through 100 orders;
3.XAD-16 macroporous resin adsorption caffeine: by the clear liquid XAD-16 macroporous resin adsorption after centrifugal, resin absorption amount and raw material ratio are 1:1(volume/mass, the extracting solution of 1 cube of corresponding 1 ton of green coffee bean of resin);
4.XAD-16 macroporous resin is resolved: adsorb saturated rear purified water and rinse limpid, elution amount is 2 times of resin volume; Collect elutriant, concentrate drying, obtains caffeine crude product
5.LX-28 macroporous resin enrichment chlorogenic acid: by loss liquid macroporous resin adsorption, resin absorption amount and raw material ratio are 1:1(volume/mass, the extracting solution of 1 cube of corresponding 1 ton of green coffee bean of resin);
6.LX-28 macroporous resin resolves (wash-out): adsorb saturated rear purified water and rinse limpid, with the ethanol elution of mass percentage concentration 70%, elution amount is 2 times of resin volume;
7. concentrated, dry: concentrate eluant, after reclaiming ethanol, spraying dry obtains the chlorogenic acid product that content is 50%;
8. decolour, crystallization: content be 50% the chlorogenic acid mass percentage concentration of 10 times be the dissolve with ethanol of 80%, activated carbon decolorizing is concentrated to proportion 1.15 after filtering, rear placement freezing and crystallizing, obtaining chlorogenic acid content after microwave drying is the product of 90%, and yield is more than 3.5%.
Embodiment 2:
The method of chlorogenic acid extracting, comprises the steps:
(1) first green coffee berry is pulverized 10 mesh sieves, obtain green coffee berry powder; Get 1 kilogram to extract, raw material chlorogenic acid content is 6.04%;
(2) adding 10 times amount mass percentage concentration is 0.1% sodium sulfite aqueous solution, and under 40 DEG C of conditions, ultrasonic adverse current is extracted continuously, and discharge is 5 times of quality of material, obtains green coffee berry crude extract;
(3) extracting solution in (2) is shaken sieved filter, horizontal screw centrifuge, disk plate centrifuge filtration through 100 orders, obtain supernatant liquor; Supernatant liquor pours in the resin column that 7 liters of XAD-16 resins are housed, and the purified water of rear use 2 times of column volumes is rinsed, and collects loss liquid and water lotion respectively, by 1 liter of LX-28 macroporous resin adsorption on loss liquid, be 80% ethanol elution by mass percentage concentration, concentrate eluant, spraying dry.Water lotion concentrate drying being obtained caffeine purity is 73.6%.
In the present embodiment, the content of chlorogenic acid is 53.3%, and yield is 3.6%, and purity is 90.5%.Caffeine purity (content) is 73.6%.
Embodiment 3:
(1) first green coffee berry is pulverized 10 mesh sieves, obtain green coffee berry powder; Get 1 kilogram to extract, raw material chlorogenic acid content is 6.04%;
(2) add 10 times amount purified water, under 40 DEG C of conditions, ultrasonic adverse current is extracted continuously, and discharge is 5 times of quality of material, obtains green coffee berry crude extract;
(3) extracting solution in (2) is shaken sieved filter, horizontal screw centrifuge, disk plate centrifuge filtration through 100 orders, obtain supernatant liquor; Supernatant liquor pours in the resin column that 7 liters of XAD-16 resins are housed, and the purified water of rear use 2 times of column volumes is rinsed, and collects loss liquid and water lotion respectively, by 1 liter of LX-28 macroporous resin on loss liquid, uses 80% ethanol elution, concentrate eluant, spraying dry.Water lotion concentrate drying being obtained caffeine purity is 73.6%.
In the present embodiment, obtain the chlorogenic acid that content is 33.2%, yield is 2.8%, and purity is 83%.Caffeine purity (content) is 73.6%.
Embodiment 4:
The method of chlorogenic acid extracting, comprises the steps:
(1) first green coffee berry is pulverized 10 mesh sieves, obtain green coffee berry powder; Get 7 kilograms to extract, raw material chlorogenic acid content is 6.04%;
(2) adding 10 times amount mass percentage concentration is 0.1% sodium sulfite aqueous solution, and under 40 DEG C of conditions, ultrasonic adverse current is extracted continuously, and discharge is 5 times of quality of material, obtains green coffee berry crude extract;
(3) extracting solution in (2) is shaken sieved filter, horizontal screw centrifuge, disk plate centrifuge filtration through 100 orders, obtain supernatant liquor; Supernatant liquor pours in the resin column that 7 liters of XAD-16 resins are housed, and the purified water of rear use 2 times of column volumes is rinsed, and collects loss liquid and water lotion.Merging and divide 7 parts equally, going up 1 liter of LX-28, DM130, D101, HZ816, AB-8, SPD600, HP-20 resin respectively, is 80% ethanol elution by mass percentage concentration, concentrate eluant, spraying dry.
Experimental example 1:LX-28 macroporous resin and other resin end product chlorogenic acid content and transformation efficiency
Experimental comparison results is as following table 1:
Table 1. different resins model experimental result contrasts
| Resin model | LX-28 | DM130 | D101 | HZ816 | AB-8 | SPD600 | HP-20 |
| Weight (g) | 102.5 | 132.6 | 167.8 | 81.3 | 157.6 | 90.4 | 127.2 |
| Content (%) | 53.25 | 30.28 | 21.27 | 52.10 | 22.69 | 48.72 | 39.24 |
| Transformation efficiency (%) | 90.51 | 66.59 | 59.20 | 70.24 | 59.30 | 73.04 | 82.78 |
Experimental example 2:
(1) first green coffee berry is pulverized 10 mesh sieves, obtain green coffee berry powder; Get 2 kilograms to extract, material content 6.04%. content of caffeine 1.2%
(2) 10 times amount 0.1% sodium sulfite aqueous solutions are added, under 40 DEG C of conditions, ultrasonic adverse current is extracted continuously, and discharge is 5 times of quality of material, obtains green coffee berry crude extract 18 liters, be divided into 2 parts (every part of corresponding dry weight 314.7 grams of chlorogenic acid contents 18.39%, content of caffeine 1.89%).A upper 1 liter of XAD-16 resin, method is as follows: upper column flow rate is 3 times of column volumes, and upper prop terminates rear use 2 times of volume purified water and rinses, and merge loss liquid and water lotion, concentrated spray is dry.Another part tetrachloromethane, consumption is 27 liters, extracts 3 times, each 9 liters, merges aqueous phase concentrate drying.Result is as table 2:
Table 2. resin method and carbon tetrachloride method are to caffeine removal effect and the contrast to chlorogenic acid transformation efficiency
As can be seen from the above table, with resin method except caffeine is obviously better than tetrachloromethane extraction process conventional at present, the transformation efficiency of chlorogenic acid also significantly improves simultaneously.
Claims (2)
1. the method for chlorogenic acid extracting from green coffee berry, is characterized in that its leaching process comprises the following steps:
(1) first green coffee berry is pulverized 10 mesh sieves, obtain green coffee berry powder;
(2) adding green coffee berry powder 10 times amount mass percentage concentration is 0.1% sodium sulfite aqueous solution, ultrasonic continuous countercurrent extraction equipment extracts continuously 40 ~ 60 DEG C of ultrasonic adverse currents, sodium sulfite aqueous solution flow is 5 times of green coffee berry powder quality, obtains green coffee berry extracting solution;
(3) gained extracting solution in step (2) is shaken sieved filter, horizontal screw centrifuge, disk plate centrifuge filtration through 100 orders, obtain supernatant liquor;
(4) gained supernatant liquor in step (3) is directly poured into XAD-16 macroporous resin, the effect of XAD-16 macroporous resin is that thus selective adsorption coffee do not adsorb chlorogenic acid, and resin absorption amount and supernatant liquor are than being 1:1; Adsorbing saturated rear purified water to rinse well, is the ethanol elution of 50 ~ 80% by mass percentage concentration, and elution amount is 2 times of resin volume, collects elutriant;
(5) XAD-16 macroporous resin loss liquid in step (4) is poured into LX-28 macroporous resin, resin absorption amount and loss liquor ratio are 1:1; Adsorbing saturated rear purified water to rinse well, is the ethanol elution of 50 ~ 80% by mass percentage concentration, and elution amount is 2 times of resin volume, collects elutriant;
(6) concentrated by gained elutriant in step (4), reclaim ethanol, spraying dry is the caffeine byproduct that content is greater than 70%; Concentrated by gained elutriant in step (5), reclaim ethanol, spraying dry is the chlorogenic acid that content is greater than 50%;
(7) be the dissolve with ethanol of 80% by the chlorogenic acid of gained in step (6) by the mass percentage concentration of its 8-10 times amount, activated carbon decolorizing is concentrated to proportion 1.15 after filtering and places freezing and crystallizing, must chlorogenic acid product after microwave drying.
2. method according to claim 1, it is characterized in that gac described in step (7) is medical needle-like gac, consumption is 5% of chlorogenic acid quality, and temperature is 70 DEG C, and soaking time is 20 min; The proportion of crystallization is 1.10 ~ 1.15, and temperature is 0 ~ 4 DEG C.
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| CN201310395334.9A CN103497106B (en) | 2013-09-04 | 2013-09-04 | Method for extracting chlorogenic acid from green coffee beans |
| PCT/CN2014/077364 WO2015032212A1 (en) | 2013-09-04 | 2014-05-13 | Method for extracting chlorogenic acid from green coffee beans |
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| CN101973882B (en) * | 2010-10-08 | 2013-07-31 | 九环菊芋生物产业股份有限公司 | Method for extracting chlorogenic acid from jerusalem artichoke leaves |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106278891B (en) * | 2016-08-03 | 2019-03-05 | 桂林茗兴生物科技有限公司 | A method of the chlorogenic acid extracting from green coffee bean |
| CN108689852A (en) * | 2018-06-26 | 2018-10-23 | 江西省科学院应用化学研究所 | A method of chlorogenic acid extracting and isochlorogenic acid from Gynura procumbens (Lour.) Merr |
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| WO2015032212A1 (en) | 2015-03-12 |
| CN103497106A (en) | 2014-01-08 |
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