CN103497106A - 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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- CN103497106A CN103497106A CN201310395334.9A CN201310395334A CN103497106A CN 103497106 A CN103497106 A CN 103497106A CN 201310395334 A CN201310395334 A CN 201310395334A CN 103497106 A CN103497106 A CN 103497106A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- 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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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/14—The ring being saturated
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 from green coffee berry the Technology of chlorogenic acid extracting, especially relate to the green coffee berry Content of Chlorogenic Acid of the ultrasonic countercurrent extraction of a kind of employing and 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 fruitlet coffee, middle fruit coffee and large fruit coffee.Contain more chlorogenic acid in green coffee bean extract, the source that therefore is used as frequently a kind of effective chlorogenic acid is used.
The intoxicated acid of contracting that chlorogenic acid (chlorogenic acid) is comprised 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 producers.Chlorogenic acid is a kind of important biologically active substance, have antibiotic, antiviral, increase the effects such as white cell, hepatic cholagogic, antitumor, hypotensive, reducing blood-fat, removing free radical and stimulating central nervous system system, to chlorogenic acid, bioactive research has been deep into a plurality of fields such as food, health care, medicine and daily-use chemical industry to modern science.The main source of chlorogenic acid is to extract from natural phant, and domestic is with plant materials such as Japanese Honeysuckle, the barks of eucommia always, is mainly abroad that to take coffee berry etc. be raw material.At present the extracting method of chlorogenic acid mainly contained:
1) water extraction: water extraction is the characteristic of utilizing chlorogenic acid soluble in water, with hot water, as digestion agent, carries out extracting method.Adopt 10 times of amount of water, decoct 2 times under 50 ℃ of conditions, decoct 1.5h at every turn, obtain the 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 method: chlorogenic acid is soluble in methyl alcohol, ethanol, acetone isopolarity solvent.With 10 times of amount 70% alcohol heat reflux 1h, obtain the chlorogenic acid crude product.Organic solvent extraction technique is simple, invests littlely, is applicable to industrialization production, but, due to an organic solvent, increases the solvent recuperation cost.
3) physical field strengthening extraction method: in the conventional solvent extraction, add as physical fields such as ultrasonic wave or microwaves, strengthening extraction, reduce extraction time, reduces the active substance degraded.Microwave power 340W, radiated time 20min, banyan agent volume fraction of ethanol 60%, ethanol consumption be under 9 times, the processing condition of soak time 30min the 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 polymeric sorbent that does not contain cation exchange groups, has macroporous structure, it is also a kind of lipophilic substance, have that selectivity is good, physical strength is high, manipulation of regeneration is convenient, rate of adsorption is fast, the advantage such as simple to operate, constant product quality, production cost are low, so be particularly suitable for the separating-purifying water-soluble cpds.CN 101704748A adopts the polar macroporous resin of NKA-II, loading concentration 0.26mg/mL, and pH2.0, sample introduction liquid is long-pending/and macroporous resin quality ratio is 12, and flow velocity is 2mL/ min, eluent 30% ethanol, the chlorogenic acid extract purity can reach 25.3%.But the method consumption time is long, clean polymeric adsorbent more difficult.
Generally speaking, the method for above chlorogenic acid extracting commonly used, self all 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 purpose of this invention is to provide that a kind of energy consumption is low, to clean polymeric adsorbent 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) at first green coffee berry was pulverized to 10 mesh sieves, obtained green coffee berry powder;
(2) adding 10 times of amount mass percentage concentration of green coffee berry powder is 0.1% sodium sulfite aqueous solution, the ultrasonic continuous countercurrent extraction equipment extracts continuously 40～60 ℃ of ultrasonic adverse currents, the 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 filtered through 100 order concussion sieve filtrations, horizontal screw centrifuge, disk plate centrifuge, obtain supernatant liquor;
(4) gained supernatant liquor in step (3) is directly poured into to the XAD-16 macroporous resin, the effect of XAD-16 macroporous resin is selective adsorption coffee thereby do not adsorb chlorogenic acid, the resin absorption amount with supernatant liquor than being 1:1; Adsorb saturated rinse well by purified water afterwards, the ethanol elution that is 50～80% by mass percentage concentration, elution amount is 2 times of resin volume, collects elutriant;
(5) XAD-16 macroporous resin loss liquid in step (4) is poured into to the LX-28 macroporous resin, resin absorption amount and loss liquor ratio are 1:1; Adsorb saturated rinse well by purified water afterwards, the ethanol elution that is 50～80% by mass percentage concentration, elution amount is 2 times of resin volume, collects elutriant;
(6) gained elutriant in step (4) is concentrated, reclaim ethanol, spraying drying obtains the caffeine byproduct; Gained elutriant in step (5) is concentrated, reclaim ethanol, spraying drying obtains chlorogenic acid;
(7) dissolve with ethanol that the mass percentage concentration of the chlorogenic acid in step (6) doubly being measured with its 8-10 is 80%, activated carbon decolorizing is concentrated to proportion 1.15 and places freezing and crystallizing after filtering, must the chlorogenic acid product after microwave drying.
Gac described in step (7) is medical needle type gac, and consumption is 5% of chlorogenic acid quality, and temperature is 70 ℃, and soaking time is 20 min; The proportion of crystallization is 1.10～1.15, and temperature is 0～4 ℃.
In step (1), require green coffee berry powder to cross 10 orders, scope is 10～20 orders, and too large extraction is insufficient, too thin extracting solution fluid difficulty;
The sodium sulfite aqueous solution that described in step (2), extracting solution is 0.1%, this extracting solution, the one, can guarantee the weakly alkaline of extracting solution, increase the water-soluble of chlorogenic acid.Experiment shows that the pH value of extracting solution of the present invention is 7～7.5, and do not add the extracting solution pH value that mass percentage concentration is 0.1% S-WAT, is 5～6, and chlorogenic acid solubleness descends 16% simultaneously.The 2nd, prevent that chlorogenic acid is oxidized, reduce the degraded of chlorogenic acid, experimental data proves: the chlorogenic acid aqueous solution that mass percentage concentration is 5% 1 hour degradation rate in boiling water is that 6.2%, 2 hour degradation rate is 10.7%.1 hour degradation rate of the sodium sulfite aqueous solution that the chlorogenic acid aqueous solution that mass percentage concentration is 5% is 0.1% in mass percentage concentration is that 0.3%, 2 hour degradation rate is 0.57%.
Extracting temperature described in step (2) is 40～60 ℃, and the too low extract of temperature is insufficient, and too the easy pasty state of high material, be unfavorable for fluid;
Described in step (2), extraction equipment is the ultrasonic continuous countercurrent extraction equipment, and this equipment advantage is not high for extracting temperature, and material and extracting solution flow to contrary, improve extraction yield, can effectively reduce the oxidation of chlorogenic acid simultaneously.With conventional multi-function extractor, compare, chlorogenic acid yield brings up to 96% from 87%, and extraction effect improves more than 10%.
Filtration condition described in step (3), for the filtration of concussion sieve, horizontal screw centrifuge, the centrifugal assurance extracting solution clarification of disk plate centrifuge, does not stop up macroporous resin on postprocessing working procedures;
Described in described step (4), polymeric adsorbent is the XAD-16 macroporous resin, and this resin is 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, most of client wishes that in content 50% chlorogenic acid product, caffeine is more low better, in order to reduce content of caffeine, at present mainly to use tetrachloromethane, tetrachloromethane be that the poisonous substances lethal quantity is 4 milliliters.The present invention selects the XAD-16 macroporous resin and can solve this problem, and the chlorogenic acid product content of caffeine of the content 50% of processing through XAD-16 is below 0.5%.
Described in described step (5), polymeric adsorbent is the LX-28 macroporous resin, and this resin is the low-pole resin, can select the absorption chlorogenic acid, with other macroporous resins, compares, and it is large that the LX-28 resin possesses adsorptive capacity, adsorbs very concentrated.Elutriant content is more than 50%.The product of LX-28 macroporous resin wash-out is the chlorogenic acid that content is 50%, and yield is 10% left and right (1 ton of raw material goes out 100 kilograms of products).
Method of the present invention is to use the Technology of ultrasonic countercurrent extraction and two kinds of macroreticular resin absorbing method couplings chlorogenic acid extracting and purifying from green coffee berry, the present invention crosses 10 orders by raw material pulverizing, use supersound extraction, adopt the filtration of concussion sieve, horizontal screw centrifuge, disk plate centrifuge centrifugal, solved in independent employing macroporous resin adsorption method, resin cleans difficult problem; The present invention adopts XAD-16 macroporous resin selective adsorption coffee thereby does not adsorb chlorogenic acid, effectively reduces content of caffeine in the chlorogenic acid product, has solved the high problem of content of caffeine in general resin absorption process Content of Chlorogenic Acid product; While caffeine recoverable; In the present invention, solvent is only used purified water and ethanol, safety and environmental protection, and the chlorogenic acid purity obtained after alcohol wash and washing are refining is up to 90%.The chlorogenic acid transformation efficiency is high, and the 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 is only used purified water and ethanol, safety and environmental protection, the characteristics such as content of caffeine is very low in 50% chlorogenic acid product.
the accompanying drawing explanation:
Fig. 1 is process flow sheet of the present invention.
embodiment:
Embodiment 1:
Technological method of the present invention mainly comprises the steps:
Material is prepared: green coffee bean powder is broken into to 15 purpose powder;
1. supersound extraction: by 50 ℃ of ultrasonic adverse currents of 8 times of amount sodium sulfite aqueous solutions (mass percentage concentration is 0.1%), extract continuously, discharge is quality of material 5 times, obtain green coffee berry extracting solution;
2. centrifuging: supersound extraction liquid is filtered through 100 order concussion sieve filtrations, horizontal screw centrifuge, disk plate centrifuge;
3.XAD-16 macroporous resin adsorption caffeine: by the XAD-16 macroporous resin adsorption of the clear liquid after centrifugal, resin absorption amount and raw material ratio are the 1:1(volume/mass, the extracting solution of 1 cube of corresponding 1 ton of green coffee berry raw material of resin);
4.XAD-16 macroporous resin is resolved: adsorb and saturatedly rinse limpidly by purified water afterwards, elution amount is 2 times of resin volume; Collect elutriant, concentrate drying, obtain the 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 the 1:1(volume/mass, the extracting solution of 1 cube of corresponding 1 ton of green coffee berry raw material of resin);
6.LX-28 macroporous resin is resolved (wash-out): adsorb and saturatedly rinse limpidly by purified water afterwards, with the ethanol elution of mass percentage concentration 70%, elution amount is 2 times of resin volume;
7. concentrated, dry: concentrate eluant, after recovery ethanol, spraying drying obtains the chlorogenic acid product that content is 50%;
8. decolouring, crystallization: the dissolve with ethanol that the chlorogenic acid that content is 50% is 80% by the mass percentage concentration of 10 times, activated carbon decolorizing is concentrated to proportion 1.15 after filtering, rear placement freezing and crystallizing, obtain the product that chlorogenic acid content is 90% after microwave drying, yield is more than 3.5%.
Embodiment 2:
The method of chlorogenic acid extracting, comprise the steps:
(1) at first green coffee berry was pulverized to 10 mesh sieves, obtained green coffee berry powder; Get 1 kilogram and extracted, the raw material chlorogenic acid content is 6.04%;
(2) adding 10 times of amount mass percentage concentration is 0.1% sodium sulfite aqueous solution, and under 40 ℃ of conditions, ultrasonic adverse current is extracted continuously, discharge is quality of material 5 times, obtain green coffee berry crude extract;
(3) extracting solution in (2) is filtered through 100 order concussion sieve filtrations, horizontal screw centrifuge, disk plate centrifuge, obtain supernatant liquor; Supernatant liquor pours in the resin column that 7 liters of XAD-16 resins are housed, and the purified water of 2 times of column volumes of rear use is rinsed, and collects respectively loss liquid and water lotion, by 1 liter of LX-28 macroporous resin adsorption on loss liquid, by mass percentage concentration, be 80% ethanol elution, concentrate eluant, spraying drying.It is 73.6% that the water lotion concentrate drying is obtained to caffeine purity.
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) at first green coffee berry was pulverized to 10 mesh sieves, obtained green coffee berry powder; Get 1 kilogram and extracted, the raw material chlorogenic acid content is 6.04%;
(2) add 10 times of amount purified water, under 40 ℃ of conditions, ultrasonic adverse current is extracted continuously, discharge is quality of material 5 times, obtain green coffee berry crude extract;
(3) extracting solution in (2) is filtered through 100 order concussion sieve filtrations, horizontal screw centrifuge, disk plate centrifuge, obtain supernatant liquor; Supernatant liquor pours in the resin column that 7 liters of XAD-16 resins are housed, and the purified water of 2 times of column volumes of rear use is rinsed, and collects respectively loss liquid and water lotion, by 1 liter of LX-28 macroporous resin on loss liquid, uses 80% ethanol elution, concentrate eluant, spraying drying.It is 73.6% that the water lotion concentrate drying is obtained to caffeine purity.
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, comprise the steps:
(1) at first green coffee berry was pulverized to 10 mesh sieves, obtained green coffee berry powder; Get 7 kilograms and extracted, the raw material chlorogenic acid content is 6.04%;
(2) adding 10 times of amount mass percentage concentration is 0.1% sodium sulfite aqueous solution, and under 40 ℃ of conditions, ultrasonic adverse current is extracted continuously, discharge is quality of material 5 times, obtain green coffee berry crude extract;
(3) extracting solution in (2) is filtered through 100 order concussion sieve filtrations, horizontal screw centrifuge, disk plate centrifuge, obtain supernatant liquor; Supernatant liquor pours in the resin column that 7 liters of XAD-16 resins are housed, and the purified water of 2 times of column volumes of rear use is rinsed, and collects loss liquid and water lotion.Merging and divide equally 7 parts, go up respectively 1 liter of LX-28, DM130, D101, HZ816, AB-8, SPD600, HP-20 resin, is 80% ethanol elution by mass percentage concentration, concentrate eluant, spraying drying.
Experimental example 1:LX-28 macroporous resin and other resin the finished product chlorogenic acid content and transformation efficiency
The experiment comparing result is as following table 1:
The contrast of table 1. different resins model experimental result
| The 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) at first green coffee berry was pulverized to 10 mesh sieves, obtained green coffee berry powder; Get 2 kilograms and extracted, material content 6.04%. content of caffeine 1.2%
(2) add 10 times of amount 0.1% sodium sulfite aqueous solutions, under 40 ℃ of conditions, ultrasonic adverse current is extracted continuously, discharge is quality of material 5 times, obtain 18 liters of green coffee berry crude extracts, be divided into 2 parts (every part of corresponding dry weight 314.7 gram 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, after upper prop finishes, by 2 times of volume purified water, rinses, and merges loss liquid and water lotion, the concentrated spray drying.Another part used tetrachloromethane, and consumption is 27 liters, extracts 3 times, each 9 liters, merges the water concentrate drying.Result is as table 2:
Table 2. resin method and carbon tetrachloride method are to the caffeine removal effect and to the contrast of chlorogenic acid transformation efficiency
As can be seen from the above table, with resin method, except caffeine, obviously be better than tetrachloromethane extraction process commonly used at present, the transformation efficiency of chlorogenic acid also obviously 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) at first green coffee berry was pulverized to 10 mesh sieves, obtained green coffee berry powder;
(2) adding 10 times of amount mass percentage concentration of green coffee berry powder is 0.1% sodium sulfite aqueous solution, the ultrasonic continuous countercurrent extraction equipment extracts continuously 40～60 ℃ of ultrasonic adverse currents, the 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 filtered through 100 order concussion sieve filtrations, horizontal screw centrifuge, disk plate centrifuge, obtain supernatant liquor;
(4) gained supernatant liquor in step (3) is directly poured into to the XAD-16 macroporous resin, the effect of XAD-16 macroporous resin is selective adsorption coffee thereby do not adsorb chlorogenic acid, the resin absorption amount with supernatant liquor than being 1:1; Adsorb saturated rinse well by purified water afterwards, the ethanol elution that is 50～80% by mass percentage concentration, elution amount is 2 times of resin volume, collects elutriant;
(5) XAD-16 macroporous resin loss liquid in step (4) is poured into to the LX-28 macroporous resin, resin absorption amount and loss liquor ratio are 1:1; Adsorb saturated rinse well by purified water afterwards, the ethanol elution that is 50～80% by mass percentage concentration, elution amount is 2 times of resin volume, collects elutriant;
(6) gained elutriant in step (4) is concentrated, reclaim ethanol, spraying drying is the caffeine byproduct that content is greater than 70%; Gained elutriant in step (5) is concentrated, reclaim ethanol, spraying drying is the chlorogenic acid that content is greater than 50%;
(7) dissolve with ethanol that the mass percentage concentration of the chlorogenic acid of gained in step (6) doubly being measured with its 8-10 is 80%, activated carbon decolorizing is concentrated to proportion 1.15 and places freezing and crystallizing after filtering, must the chlorogenic acid product after microwave drying.
2. method according to claim 1, is characterized in that gac described in step (7) is medical needle type gac, and consumption is 5% of chlorogenic acid quality, and temperature is 70 ℃, and soaking time is 20 min; The proportion of crystallization is 1.10～1.15, and temperature is 0～4 ℃.
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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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| CN201310395334.9A CN103497106B (en) | 2013-09-04 | 2013-09-04 | Method for extracting chlorogenic acid from green coffee beans |
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Cited By (11)
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| WO2015032212A1 (en) * | 2013-09-04 | 2015-03-12 | 四川圣湖生物科技有限公司 | Method for extracting chlorogenic acid from green coffee beans |
| CN104876824A (en) * | 2015-01-23 | 2015-09-02 | 南通海天生物科技有限公司 | Technology for separation and purification of chlorogenic acid from coffee beans |
| CN105558213A (en) * | 2015-12-30 | 2016-05-11 | 重庆骄王天然产物股份有限公司 | Green coffee bean powder and making method thereof |
| CN106278891A (en) * | 2016-08-03 | 2017-01-04 | 桂林茗兴生物科技有限公司 | A kind of method of chlorogenic acid extracting from green coffee bean |
| CN106389597A (en) * | 2016-11-24 | 2017-02-15 | 广州和匠科技有限公司 | Method for efficiently extracting edible and medicinal monomers preventing and treating hyperuricemia and gout from coffee |
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| WO2015032212A1 (en) * | 2013-09-04 | 2015-03-12 | 四川圣湖生物科技有限公司 | Method for extracting chlorogenic acid from green coffee beans |
| CN104876824A (en) * | 2015-01-23 | 2015-09-02 | 南通海天生物科技有限公司 | Technology for separation and purification of chlorogenic acid from coffee beans |
| CN105558213A (en) * | 2015-12-30 | 2016-05-11 | 重庆骄王天然产物股份有限公司 | Green coffee bean powder and making method thereof |
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| CN108586242A (en) * | 2018-04-02 | 2018-09-28 | 太阳树（厦门）生物工程有限公司 | A method of extracting low-caffeine chlorogenic acid from green coffee bean |
| CN111387327A (en) * | 2020-03-30 | 2020-07-10 | 黑龙江八一农垦大学 | Preparation method of green coffee oil |
| CN111718263A (en) * | 2020-06-08 | 2020-09-29 | 颜如玉医药科技有限公司 | Process for extracting chlorogenic acid from green coffee beans |
| CN111718263B (en) * | 2020-06-08 | 2021-01-29 | 颜如玉医药科技有限公司 | Process for extracting chlorogenic acid from green coffee beans |
| CN111991847A (en) * | 2020-09-03 | 2020-11-27 | 河北瑞龙生物科技有限公司 | Preparation method of coffee bean hull extract |
| CN111991847B (en) * | 2020-09-03 | 2022-03-04 | 河北瑞龙生物科技有限公司 | Coffee bean hull extract and preparation method and application thereof |
| CN117682954A (en) * | 2024-02-04 | 2024-03-12 | 云南西草资源开发有限公司 | Chlorogenic acid-enriched coffee extract, preparation method and chlorogenic acid-enriched coffee powder |
| CN117682954B (en) * | 2024-02-04 | 2024-04-05 | 云南西草资源开发有限公司 | Chlorogenic acid-enriched coffee extract, preparation method and chlorogenic acid-enriched coffee powder |
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| WO2015032212A1 (en) | 2015-03-12 |
| CN103497106B (en) | 2015-01-07 |
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