CN108558668A - A method of the chlorogenic acid extracting from jerusalem artichoke leaves - Google Patents
A method of the chlorogenic acid extracting from jerusalem artichoke leaves Download PDFInfo
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- CN108558668A CN108558668A CN201810401835.6A CN201810401835A CN108558668A CN 108558668 A CN108558668 A CN 108558668A CN 201810401835 A CN201810401835 A CN 201810401835A CN 108558668 A CN108558668 A CN 108558668A
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- jerusalem artichoke
- chlorogenic acid
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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
- 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
- C07C67/60—Separation; Purification; Stabilisation; Use of additives by treatment giving rise to chemical modification
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C69/00—Esters of carboxylic acids; Esters of carbonic or haloformic acids
- C07C69/66—Esters of carboxylic acids having esterified carboxylic groups bound to acyclic carbon atoms and having any of the groups OH, O—metal, —CHO, keto, ether, acyloxy, groups, groups, or in the acid moiety
- C07C69/73—Esters of carboxylic acids having esterified carboxylic groups bound to acyclic carbon atoms and having any of the groups OH, O—metal, —CHO, keto, ether, acyloxy, groups, groups, or in the acid moiety of unsaturated acids
- C07C69/732—Esters of carboxylic acids having esterified carboxylic groups bound to acyclic carbon atoms and having any of the groups OH, O—metal, —CHO, keto, ether, acyloxy, groups, groups, or in the acid moiety of unsaturated acids of unsaturated hydroxy carboxylic acids
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- General Chemical & Material Sciences (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The present invention relates to belonging to technical field of plant extraction, more particularly to a kind of method of the chlorogenic acid extracting from jerusalem artichoke leaves, including steps are as follows：1) it ferments；2) ultrasonication；3) enzymatic treatment；4) microwave treatment；5) resin adsorption；6) kieselguhr adsorption；The method of the present invention has the extraction cost for reducing chlorogenic acid, improves plant tissue permeability, reduces chlorogenic acid resistance to mass tranfer, increases chlorogenic acid yield, ensure that chlorogenic acid stability, improve the purity of chlorogenic acid, the advantage of yield；And the raw material of the method for the present invention is cheap and easy to get, production cost is low, easy to operate, and method is environmentally protective.
Description
Technical field
The present invention relates to belonging to technical field of plant extraction, more particularly to a kind of side of the chlorogenic acid extracting from jerusalem artichoke leaves
Method.
Background technology
Jerusalem artichoke also known as ground ginger, Jerusalem artichoke and Jerusalem artichoke are composite family Helianthus herbaceos perennials, original North America, ten
Seventh century are incoming European, rear incoming China.Contain abundant nutriment in leaf of canada potato, and anti-oxidant containing natural biological
Agent-chlorogenic acid, according to measurement, dry leaf of canada potato Content of Chlorogenic Acid is up to 3% or so.Chlorogenic acid has extensive bioactivity,
Modern science has been deep into the multiple fields such as food, health care, medicine and daily-use chemical industry to the research of chlorogenic acid bioactivity.Green original
Acid is a kind of important bioactive substance, have antibacterial, it is antiviral, increase white blood cell, hepatic cholagogic, antitumor, blood pressure lowering,
The effects that free radical and stimulating central nervous system system, is removed in reducing blood lipid.
Currently, the country, mainly using the high prices such as honeysuckle, Cortex Eucommiae medicine resource as raw material chlorogenic acid extracting, resource is limited and valence
Lattice are expensive, and Chinese patent 201210531489.6 extracts separating chlorogenic acid from tobacco, but contains multiple harmful substances in tobacco,
Its safety cannot ensure.In addition, the Land use systems of jerusalem artichoke are relatively single, are also rarely reported to the research that its blade utilizes,
The nutriment that how to make full use of leaf of canada potato abundant and its health functions is developed, becomes research from now on and be badly in need of solving
The problem of.
Invention content
The present invention in order to solve the above technical problems, the present invention provides a kind of from jerusalem artichoke leaves chlorogenic acid extracting method.
It is realized particular by following technical scheme：
A method of the chlorogenic acid extracting from jerusalem artichoke leaves, including steps are as follows：1) it ferments；2) ultrasonication；3) enzyme
Processing；4) microwave treatment；5) resin adsorption；6) kieselguhr adsorption.
In the above method, it is described fermentation be jerusalem artichoke leaves handles in steam ambient to blade surface water content be 35-
45%, it is then beaten, obtains jerusalem artichoke leaf juice, and by the inulin enzyme solution of addition jerusalem artichoke leaf juice 3-7% under the conditions of temperature is 37-45 DEG C
Microwave treatment 3-8h, then water-bath isothermal holding 8-12h；Then glucose, the jerusalem artichoke leaf juice of jerusalem artichoke leaf juice quality 10-15% is added
The carbonated water of quality 4-7%d Rui Shi lactobacillus, jerusalem artichoke leaf juice quality 80-90%, constant temperature is sent out under the conditions of being 10-15 DEG C in temperature
Ferment 2-3d.
In the above method, the ultrasonication is placed in tunning under the ultrasound condition that power is 160-190W
Handle 15min.
In the above method, the enzymatic treatment is the complex enzyme that its quality 0.3-0.8% is added into ultrasonication product,
7-12h is handled under the conditions of being 10-15 DEG C in bath temperature.
In the above method, the microwave treatment is placed in enzymatic treatment product under the microwave condition that power is 230-250W
Manage 20min.
In the above method, the resin adsorption is by treating products with microwaves by macroporous resin column, Dynamic Adsorption to being saturated,
It is colourless to efflux with the flow velocity elution macroporous resin column of 6-8BV/h with the hydrochloric acid solution of pH=5.5-6.5.
In the above method, the kieselguhr adsorption is that fat adsorbed product quality 45-50% is added into resin adsorption product
Modification infusorial earth stir evenly after heat and be completely absorbed to liquid, then take out modification infusorial earth and squeezed, received
Collect squeezed fluid to get chlorogenic acid.
In the above method, the steam ambient, vapor (steam) temperature is 120-128 DEG C.
In the above method, the complex enzyme includes in parts by weight：2-3 parts of papain, 5-9 parts of lignoenzyme, fruit
4-7 parts of glue enzyme, 1-2 parts of tyrosinase, 0.6-1.8 parts of peroxidase, 8-14 parts of cellulase.
In the above method, the macroreticular resin is the polarity or intermediate-polarity macroporous adsorption resin for meeting medicinal requirements.
In the above method, the modification infusorial earth is by diatomite：Bamboo leaf powder=(13-17)：1 mass ratio is mixed
It closes, is placed in grinding in grinder and then handles 15min in the case where power is the ultrasound condition of 160-200W to 180-260 mesh.
Specially：
1) it ferments：It is 35-45% that jerusalem artichoke leaves, which are handled in steam ambient to blade surface water content, is then beaten, obtains
Jerusalem artichoke leaf juice, and press and add microwave treatment 3-8h under the conditions of the inulin enzyme solution of jerusalem artichoke leaf juice 3-7% is 37-45 DEG C in temperature, then
Water-bath isothermal holding 8-12h；Then glucose, the jerusalem artichoke leaf juice quality 4-7%d Rui Shi of jerusalem artichoke leaf juice quality 10-15% is added
The carbonated water of lactobacillus, jerusalem artichoke leaf juice quality 80-90%, ferment at constant temperature 2-3d under the conditions of being 10-15 DEG C in temperature；
2) ultrasonication：Step 1) gains are placed under the ultrasound condition that power is 160-190W and handle 15min；
3) enzymatic treatment：The complex enzyme of its quality 0.3-0.8% is added into step 2) gains, in bath temperature be 10-
7-12h is handled under the conditions of 15 DEG C；
4) microwave treatment：Step 3) gains are placed under the microwave condition that power is 230-250W and handle 20min；
5) resin adsorption：By gains in step 4) by macroporous resin column, Dynamic Adsorption uses pH=5.5- to being saturated
6.5 hydrochloric acid solution is colourless to efflux with the flow velocity elution macroporous resin column of 6-8BV/h；
6) kieselguhr adsorption：The modification infusorial earth of step 5) gains quality 45-50% is added into step 5) gains
After stirring evenly heat treatment be completely absorbed to liquid, then take out modification infusorial earth and squeezed, collect squeezed fluid to get
Chlorogenic acid.
The beneficial effects of the present invention are：
The present invention selects inulinase, Lactobacillus helveticus to carry out fermentation process using jerusalem artichoke leaves as raw material so that and jerusalem artichoke produces wine,
And then the use of organic solvent during extraction chlorogenic acid is avoided, and contribute to the dissolution of chlorogenic acid；Reduce production peace
Full hidden danger avoids increasing the secondary pollution caused by environment using auxiliary agent, is conducive to environmental protection, while also reducing auxiliary agent and washing
De- process, greatly reduces the extraction cost of chlorogenic acid.
The present invention is first with ultrasonic excitation so that the substances such as lignin, cellulose are activated, then rationally utilize complex enzyme
Processing effectively interrupts the institutional framework for hindering chlorogenic acid dissolution, improves plant tissue permeability, reduces chlorogenic acid resistance to mass tranfer,
Increase chlorogenic acid yield.
The present invention is in conjunction with microwave treatment, it is suppressed that the growth of microorganism ensure that chlorogenic acid stability, improve chlorogenic acid
Recovery rate and product quality, therefore, chlorogenic acid yield is up to 99.3% obtained by the method for the present invention.
The present invention is adsorbed using resin and diatomite, and the rate of adsorption is fast, macroreticular resin and the repeatable utilization of diatomite,
Also, the diatomite for having adsorbed Multiple components can be additionally used in the other fields such as building, improve the purity of chlorogenic acid, therefore, this
Chlorogenic acid purity is up to 97.9% obtained by inventive method.
The raw material of the method for the present invention is cheap and easy to get, and production cost is low, easy to operate, and method is environmentally protective.
Specific implementation mode
Specific embodiments of the present invention will be described in further detail below, but the invention is not limited in these realities
Mode is applied, it is claimed to still fall within the claims in the present invention for any improvement or replacement on the present embodiment essence spirit
Range.
Embodiment 1
The method of the present embodiment provides a kind of from jerusalem artichoke leaves chlorogenic acid extracting, step include：
1) it ferments：By jerusalem artichoke leaves, processing is aqueous to blade surface in steam ambient under conditions of vapor (steam) temperature is 128 DEG C
Amount is 45%, is then beaten, and obtains jerusalem artichoke leaf juice, and by the inulin enzyme solution of addition jerusalem artichoke leaf juice 7% under the conditions of temperature is 45 DEG C
Microwave treatment 8h, then water-bath isothermal holding 12h；Then glucose, the jerusalem artichoke leaf juice quality 7% of jerusalem artichoke leaf juice quality 15% is added
Rui Shi lactobacillus, jerusalem artichoke leaf juice quality 90% carbonated water, in temperature be 15 DEG C under the conditions of ferment at constant temperature 3d；
2) ultrasonication：Step 1) gains are placed under the ultrasound condition that power is 190W and handle 15min；
3) enzymatic treatment：The complex enzyme of its quality 0.8% is added into step 2) gains, in bath temperature be 15 DEG C of conditions
Lower processing 12h；
4) microwave treatment：Step 3) gains are placed under the microwave condition that power is 250W and handle 20min；
5) resin adsorption：Gained in step 4) is gone through macroporous resin column, Dynamic Adsorption is to being saturated, with pH=6.5's
Hydrochloric acid solution is colourless to efflux with the flow velocity elution macroporous resin column of 8BV/h；
6) kieselguhr adsorption：The modification infusorial earth of step 5) gains quality 45-50% is added into step 5) gains
After stirring evenly heat treatment be completely absorbed to liquid, then take out modification infusorial earth and squeezed, collect squeezed fluid to get
Chlorogenic acid；
The complex enzyme includes：Papain 3g, lignoenzyme 9g, pectase 7g, tyrosinase 2g, peroxidase
1.8g, cellulase 14g；
The macroreticular resin is the polarity or intermediate-polarity macroporous adsorption resin for meeting medicinal requirements；
The modification infusorial earth is by diatomite：Bamboo leaf powder=17：1 mass ratio is mixed, and is placed in grinder
Then grinding handles 15min to 260 mesh in the case where power is the ultrasound condition of 200W.
Embodiment 2
The method of the present embodiment provides a kind of from jerusalem artichoke leaves chlorogenic acid extracting, step include：
1) it ferments：By jerusalem artichoke leaves, processing is aqueous to blade surface in steam ambient under conditions of vapor (steam) temperature is 120 DEG C
Amount is 35%, is then beaten, and obtains jerusalem artichoke leaf juice, and by the inulin enzyme solution of addition jerusalem artichoke leaf juice 3% under the conditions of temperature is 37 DEG C
Microwave treatment 3h, then water-bath isothermal holding 8h；Then glucose, the jerusalem artichoke leaf juice quality 4% of jerusalem artichoke leaf juice quality 10% is added
Rui Shi lactobacillus, jerusalem artichoke leaf juice quality 80% carbonated water, in temperature be 10 DEG C under the conditions of ferment at constant temperature 2d；
2) ultrasonication：Step 1) gains are placed under the ultrasound condition that power is 160W and handle 15min；
3) enzymatic treatment：The complex enzyme of its quality 0.3% is added into step 2) gains, in bath temperature be 10 DEG C of conditions
Lower processing 7h；
4) microwave treatment：Step 3) gains are placed under the microwave condition that power is 230W and handle 20min；
5) resin adsorption：Gained in step 4) is gone through macroporous resin column, Dynamic Adsorption is to being saturated, with pH=5.5's
Hydrochloric acid solution is colourless to efflux with the flow velocity elution macroporous resin column of 6BV/h；
6) kieselguhr adsorption：The modification infusorial earth stirring of step 5) gains quality 45% is added into step 5) gains
Heat treatment is completely absorbed to liquid after uniformly, is then taken out modification infusorial earth and is squeezed, and collects squeezed fluid to get green original
Acid；
The complex enzyme includes：Papain 2g, lignoenzyme 5g, pectase 4g, tyrosinase 1g, peroxidase
0.6g, cellulase 8g；
The macroreticular resin is the polarity or intermediate-polarity macroporous adsorption resin for meeting medicinal requirements；
The modification infusorial earth is by diatomite：Bamboo leaf powder=13：1 mass ratio is mixed, and is placed in grinder
Then grinding handles 15min to 180 mesh in the case where power is the ultrasound condition of 160W.
Embodiment 3
The method of the present embodiment provides a kind of from jerusalem artichoke leaves chlorogenic acid extracting, step include：
1) it ferments：By jerusalem artichoke leaves, processing is aqueous to blade surface in steam ambient under conditions of vapor (steam) temperature is 125 DEG C
Amount is 40%, is then beaten, and obtains jerusalem artichoke leaf juice, and by the inulin enzyme solution of addition jerusalem artichoke leaf juice 5% under the conditions of temperature is 40 DEG C
Microwave treatment 5h, then water-bath isothermal holding 10h；Then glucose, the jerusalem artichoke leaf juice quality 5% of jerusalem artichoke leaf juice quality 12% is added
The carbonated water of d Rui Shi lactobacillus, jerusalem artichoke leaf juice quality 85%, ferment at constant temperature 3d under the conditions of being 15 DEG C in temperature；
2) ultrasonication：Step 1) gains are placed under the ultrasound condition that power is 175W and handle 15min；
3) enzymatic treatment：The complex enzyme of its quality 0.5% is added into step 2) gains, in bath temperature be 15 DEG C of conditions
Lower processing 10h；
4) microwave treatment：Step 3) gains are placed under the microwave condition that power is 240W and handle 20min；
5) resin adsorption：Gained in step 4) is gone through macroporous resin column, Dynamic Adsorption is to being saturated, with pH=6.0's
Hydrochloric acid solution is colourless to efflux with the flow velocity elution macroporous resin column of 7BV/h；
6) kieselguhr adsorption：The modification infusorial earth stirring of step 5) gains quality 48% is added into step 5) gains
Heat treatment is completely absorbed to liquid after uniformly, is then taken out modification infusorial earth and is squeezed, and collects squeezed fluid to get green original
Acid；
The complex enzyme includes：Papain 2.5g, lignoenzyme 7g, pectase 5.5g, tyrosinase 1.5g, peroxide
Compound enzyme 1.2g, cellulase 11 g；
The macroreticular resin is the polarity or intermediate-polarity macroporous adsorption resin for meeting medicinal requirements；
The modification infusorial earth is by diatomite：Bamboo leaf powder=15：1 mass ratio is mixed, and is placed in grinder
Then grinding handles 15min to 200 mesh in the case where power is the ultrasound condition of 180W.
Claims (10)
1. a kind of method of the chlorogenic acid extracting from jerusalem artichoke leaves, which is characterized in that including steps are as follows：1) it ferments；2) ultrasonic wave
Processing；3) enzymatic treatment；4) microwave treatment；5) resin adsorption；6) kieselguhr adsorption；The fermentation is by jerusalem artichoke leaves in steam ambient
Middle processing to blade surface water content is 35-45%, is then beaten, and obtains jerusalem artichoke leaf juice, and by the chrysanthemum of addition jerusalem artichoke leaf juice 3-7%
Microwave treatment 3-8h under the conditions of powder enzyme solution is 37-45 DEG C in temperature, then water-bath isothermal holding 8-12h；Then jerusalem artichoke leaf juice is added
The glucose of quality 10-15%, the carbonated water of jerusalem artichoke leaf juice quality 4-7%d Rui Shi lactobacillus, jerusalem artichoke leaf juice quality 80-90%,
Ferment at constant temperature 2-3d under the conditions of being 10-15 DEG C in temperature.
2. as described in claim 1 from jerusalem artichoke leaves chlorogenic acid extracting method, which is characterized in that the ultrasonication is
Tunning is placed under the ultrasound condition that power is 160-190W and handles 15min.
3. as described in claim 1 from jerusalem artichoke leaves chlorogenic acid extracting method, which is characterized in that the enzymatic treatment is to ultrasound
The complex enzyme of its quality 0.3-0.8% is added in wave processing product, 7-12h is handled under the conditions of being 10-15 DEG C in bath temperature.
4. as described in claim 1 from jerusalem artichoke leaves chlorogenic acid extracting method, which is characterized in that the microwave treatment is by enzyme
Processing product is placed under the microwave condition that power is 230-250W and handles 20min.
5. as described in claim 1 from jerusalem artichoke leaves chlorogenic acid extracting method, which is characterized in that the resin adsorption is will be micro-
Wave handles product by macroporous resin column, and Dynamic Adsorption is to being saturated, with the hydrochloric acid solution of pH=5.5-6.5 with the stream of 6-8BV/h
Speed elution macroporous resin column is colourless to efflux.
6. as described in claim 1 from jerusalem artichoke leaves chlorogenic acid extracting method, which is characterized in that the kieselguhr adsorption be to
The modification infusorial earth of addition fat adsorbed product quality 45-50% heats after stirring evenly to liquid quilt in resin adsorption product
It fully absorbs, then takes out modification infusorial earth and squeezed, collect squeezed fluid to get chlorogenic acid.
7. as described in claim 1 from jerusalem artichoke leaves chlorogenic acid extracting method, which is characterized in that the steam ambient, steam
Stripping temperature is 120-128 DEG C.
8. as claimed in claim 3 from jerusalem artichoke leaves chlorogenic acid extracting method, which is characterized in that the complex enzyme is with parts by weight
Meter includes：2-3 parts of papain, 5-9 parts of lignoenzyme, 4-7 parts of pectase, 1-2 parts of tyrosinase, peroxidase 0.6-
1.8 parts, 8-14 parts of cellulase.
9. as claimed in claim 5 from jerusalem artichoke leaves chlorogenic acid extracting method, which is characterized in that the macroreticular resin is to meet
The polarity or intermediate-polarity macroporous adsorption resin of medicinal requirements.
10. as claimed in claim 6 from jerusalem artichoke leaves chlorogenic acid extracting method, which is characterized in that the modification infusorial earth is
By diatomite：Bamboo leaf powder=(13-17)：1 mass ratio is mixed, and is placed in grinder that grinding is to 180-260 mesh, then
15min is handled in the case where power is the ultrasound condition of 160-200W.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103524348A (en) * | 2013-09-29 | 2014-01-22 | 湖南金地生物科技有限公司 | Process for extracting chlorogenic acid from honeysuckle and dry leaves of honeysucklestem through biological enzyme |
| CN106397202A (en) * | 2016-09-27 | 2017-02-15 | 重庆工商大学 | Method for carrying out metal-enzyme co-catalysis on lonicera japonica leaves to produce ethyl alcohol and simultaneously extracting chlorogenic acid |
-
2018
- 2018-04-28 CN CN201810401835.6A patent/CN108558668A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103524348A (en) * | 2013-09-29 | 2014-01-22 | 湖南金地生物科技有限公司 | Process for extracting chlorogenic acid from honeysuckle and dry leaves of honeysucklestem through biological enzyme |
| CN106397202A (en) * | 2016-09-27 | 2017-02-15 | 重庆工商大学 | Method for carrying out metal-enzyme co-catalysis on lonicera japonica leaves to produce ethyl alcohol and simultaneously extracting chlorogenic acid |
Non-Patent Citations (3)
| Title |
|---|
| 刘传安等: "RP-HPLC法测定杜仲叶发酵液中绿原酸的含量", 《安徽农业科学》 * |
| 孙鹏程: "菊芋叶片中高纯度绿原酸的规模化制备工艺研究", 《中国优秀硕士学位论文全文数据库 医药卫生科技辑》 * |
| 贾春凤等: "杜仲叶醋发酵工艺参数优化", 《食品与机械》 * |
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Application publication date: 20180921 |