CN106631797A - Extraction method of chlorogenic acid in tobacco leaves - Google Patents
Extraction method of chlorogenic acid in tobacco leaves Download PDFInfo
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- CN106631797A CN106631797A CN201611266573.4A CN201611266573A CN106631797A CN 106631797 A CN106631797 A CN 106631797A CN 201611266573 A CN201611266573 A CN 201611266573A CN 106631797 A CN106631797 A CN 106631797A
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- extracting method
- chlorogenic acid
- tobacco leaf
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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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Abstract
The invention belongs to the field of the processing of tobacco products, and particularly relates to an extraction method of chlorogenic acid in tobacco leaves. The invention provides the extraction method of the chlorogenic acid in the tobacco leaves. The extraction method comprises a step I of extraction, a step II of concentration and a step III of purification. Known through experimental determination, by using the technical scheme provided by the invention, the purity of the chlorogenic acid obtained through the extraction can reach 87.4 percent; the yield of the chlorogenic acid can reach 1.762 percent. In the technical scheme provided by the invention, raw materials are waste and inferior tobacco leaves; the costs of the raw materials are low; the aim of waste utilization in the current green society is met; meanwhile, the technical scheme provided by the invention is simple, convenient and quick, and is suitable for industrialized large-scale popularization. The technical defects that an extraction method of the chlorogenic acid in the tobacco leaves is high in cost and unsuitable for industrialized extraction in the prior art are solved. The extraction method provided by the invention is simple, convenient and quick, is low in cost, and is suitable for large-scale industrialized popularization.
Description
Technical field
The invention belongs to tobacco product manufacture field, more particularly to a kind of extracting method of tobacco leaf Content of Chlorogenic Acid.
Background technology
Chlorogenic acid (Chlorogenic acid) is a kind of highly important active medicinal matter, not only with antibacterial and is supported
Antiviral function, also with prevent white blood cell increase, protection liver and gall-bladder, it is antitumor, hypotensive, remove free radical and
Digestive system, hematological system and genital system diseases are had significant curative effect, to golden yellow by the functions such as stimulating central nervous system system
Staphylococcus, hemolytic streptococcus, shigella dysenteriae, typhoid bacillus have significant inhibitory action, and highly purified chlorogenic acid price is held high
It is expensive, it is current internationally recognized " plant gold ".
Tobacco (Nicotiana tabacum L.) belongs to annual herb plant for Solanaceae cigarette, is a kind of important economic work
Thing, it has extensive research in terms of botany, life science, physical chemistry and biotechnology.But have a large amount of useless every year
Abandon tobacco leaf and cannot be used for production of cigarettes, both waste of resource, and to environment.Content of the chlorogenic acid in tobacco leaf is up to
3%, at present the country is mainly from the huge of chlorogenic acid extracting in honeysuckle, the bark of eucommia, sunflower seeds, the few raw material of its valency a large amount and product
Demand contrast forces people to seek more extensive raw material, therefore, not only widen chlorogenic acid using waste/hypo-tobacco leaf production chlorogenic acid
Raw material sources, the added value at tobacco planting family can also be improved, scientific utilization tobacco is had important practical significance.Additionally,
China has every year the leftover bits and pieces such as 30% discarded tobacco leaf, offal to go out of use as tobacco leaf production big country, and this is not only to plant resources
It is a kind of waste, also severe contamination environment.Potential value and the effect of these discarded objects are how played, tobacco is better profited from
Resource, improves its economic worth, it has also become much-talked-about topic in recent years, is particularly subject to the very big of the industries such as medicine, chemical industry, food
Concern.
In prior art, the method for chlorogenic acid extracting mainly has：Microwave loss mechanisms, ultrasonic extraction, enzyme extraction method with
And heating reflux method etc..Wherein, although microwave loss mechanisms, ultrasonic extraction and enzyme extraction method extraction efficiency are high, its cost
It is too high, the small-scale extraction such as laboratory is only applicable to, there is limitation in commercial process.Therefore, prior art
In, the extracting method of tobacco leaf Content of Chlorogenic Acid has high cost, is not suitable for industrializing the technological deficiency extracted.
Therefore, develop a kind of extracting method of tobacco leaf Content of Chlorogenic Acid, for solving prior art in, tobacco leaf Content of Chlorogenic Acid
Extracting method there is high cost, be not suitable for industrialize extract technological deficiency, become those skilled in the art and urgently solve
Problem certainly.
The content of the invention
In view of this, the invention provides a kind of extracting method of tobacco leaf Content of Chlorogenic Acid, for solving prior art in, cigarette
The extracting method of leaf Content of Chlorogenic Acid has high cost, is not suitable for industrializing the technological deficiency extracted.The extraction that the present invention is provided
Method, it is simple, convenient, it is with low cost, it is suitable for large-scale industrialization popularization.
The invention provides a kind of extracting method of tobacco leaf Content of Chlorogenic Acid, the extracting method is：
Step one, extraction：After tobacco leaf mixes with extractant, it is heated at reflux, obtains leaching liquor；
Step 2, concentration：After the leaching liquor concentration, concentrate is obtained；
Step 3：Purification：The concentrate purification, obtains chlorogenic acid.
Preferably, the extracting method also includes：Pretreatment, the pretreatment is carried out before the extraction；
The method of the pretreatment is：It is size-reduced and sieve successively after tobacco leaf drying, obtain prefinished products.
Preferably, the temperature of the drying is 50～60 DEG C, and the time of the drying is 48～72h, and the pretreatment is produced
The particle diameter of product is 40 mesh.
Preferably, the extractant is the ethanol water that mass fraction is 95%, and the pH of the extractant is 4～6.
Preferably, the extracting method also includes：Suction filtration：
The suction filtration is carried out between the step one and step 2.
Preferably, the temperature being heated at reflux is 60～80 DEG C, and the time being heated at reflux is 75～105min.
Preferably, the method for the concentration is reduced pressure concentration, and the temperature of the reduced pressure concentration is 40～45 DEG C.
Preferably, the method for the purification is：After the concentrate stands, be collected by centrifugation supernatant, the supernatant according to
Secondary freeze-dried and recrystallization, obtains chlorogenic acid.
Preferably, the temperature of the standing is 4 DEG C, and the time of the standing is 12～24h；
The rotating speed of the centrifugation is 12000r/min, and the time of the centrifugation is 20～30min；
The solvent of the recrystallization is methyl alcohol.
Preferably, the cryodesiccated method is：The supernatant is freezed after 0.5～1h in -40 DEG C～-60 DEG C, -
It is dried under the conditions of 0.05～-0.09MPa and 40～60 DEG C.
In sum, the invention provides a kind of extracting method of tobacco leaf Content of Chlorogenic Acid, the extracting method is：Step
First, extract：After tobacco leaf mixes with extractant, it is heated at reflux, obtains leaching liquor；Step 2, concentration：After the leaching liquor concentration, obtain
Concentrate；Step 3：Purification：The concentrate purification, obtains chlorogenic acid.Jing measurings can be obtained, the technical side that the present invention is provided
Case, extracts the chlorogenic acid purity for obtaining and can reach 87.4%, and the yield of chlorogenic acid can obtain 1.762%.The technology that the present invention is provided
In scheme, raw material is waste/hypo-tobacco leaf, and cost of material is low, meets the objective of current green society twice laid；Meanwhile, the present invention
The technical scheme of offer, it is simple and convenient, it is adapted to industrialization large-scale promotion.In solving prior art, tobacco leaf Content of Chlorogenic Acid
Extracting method has high cost, is not suitable for industrializing the technological deficiency extracted.The extracting method that the present invention is provided, simply, just
Victory, it is with low cost, it is suitable for large-scale industrialization popularization.
Specific embodiment
The invention provides a kind of extracting method of tobacco leaf Content of Chlorogenic Acid, for solving prior art in, green original in tobacco leaf
The extracting method of acid has high cost, is not suitable for industrializing the technological deficiency extracted.The extracting method that the present invention is provided, letter
It is single, convenient, it is with low cost, it is suitable for large-scale industrialization popularization.
The technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described enforcement
Example is only a part of embodiment of the invention, rather than the embodiment of whole.Based on the embodiment in the present invention, this area is common
The every other embodiment that technical staff is obtained under the premise of creative work is not made, belongs to the model of present invention protection
Enclose.
In order to the present invention is described in more detail, with reference to embodiment carrying to a kind of tobacco leaf Content of Chlorogenic Acid for providing of the invention
Method is taken, is specifically described.
Embodiment 1
Waste/hypo-tobacco leaf is placed in pulverizer and crushes after 50 DEG C of oven for drying 48h, crosses 40 mesh sieves, obtains tobacco leaf powder 1.
10g tobacco leaves powder 1 and 100mL extractants 1 mix, and under the conditions of 60 DEG C 75min is heated at reflux, and obtain leaching liquor 1.Its
In, extractant 1 is the ethanol water that mass concentration is 95%, and the pH of extractant 1 is 4.
After the suction filtration of extractant 1, reduced pressure concentration under the conditions of 40 DEG C of gained smoke filtrate obtains concentrate 1.
After concentrate 1 stands 12h under the conditions of 4 DEG C, 20min is centrifuged with the rotating speed of 12000r/min, collects supernatant, will
20min is centrifuged with the rotating speed of 12000r/min after precipitation distillation water washing after centrifugation, supernatant is collected；Merge on gained twice
Clear liquid, obtains supernatant 1.
After supernatant 1 freezes 0.5h under the conditions of -60 DEG C, do in vacuum drier under the conditions of -0.09MPa, 40 DEG C
It is dry；Gained dry products recrystallizing methanol, obtains the 0.244g of chlorogenic acid product 1.
In the present embodiment, the yield of chlorogenic acid product 1 is 86.17%, and the purity of chlorogenic acid product 1 is 1.726%.
Embodiment 2
Waste/hypo-tobacco leaf is placed in pulverizer and crushes after 55 DEG C of oven for drying 60h, crosses 40 mesh sieves, obtains tobacco leaf powder 2.
10g tobacco leaves powder 2 and 120mL extractants 2 mix, and under the conditions of 70 DEG C 90min is heated at reflux, and obtain leaching liquor 2.Its
In, extractant 2 is the ethanol water that mass concentration is 95%, and the pH of extractant 2 is 5.
After the suction filtration of extractant 2, reduced pressure concentration under the conditions of 40 DEG C of gained smoke filtrate obtains concentrate 2.
After concentrate 2 stands 18h under the conditions of 4 DEG C, 25min is centrifuged with the rotating speed of 12000r/min, collects supernatant, will
25min is centrifuged with the rotating speed of 12000r/min after precipitation distillation water washing after centrifugation, supernatant is collected；Merge on gained twice
Clear liquid, obtains supernatant 2.
After supernatant 2 freezes 0.5h under the conditions of -50 DEG C, do in vacuum drier under the conditions of -0.07MPa, 50 DEG C
It is dry；Gained dry products recrystallizing methanol, obtains the 0.267g of chlorogenic acid product 2.
In the present embodiment, the yield of chlorogenic acid product 2 is 91.21%, and the purity of chlorogenic acid product 2 is 1.856%.
Embodiment 3
Waste/hypo-tobacco leaf is placed in pulverizer and crushes after 60 DEG C of oven for drying 72h, crosses 40 mesh sieves, obtains tobacco leaf powder 3.
10g tobacco leaves powder 3 and 140mL extractants 3 mix, and under the conditions of 80 DEG C 105min is heated at reflux, and obtain leaching liquor 3.Its
In, extractant 3 is the ethanol water that mass concentration is 95%, and the pH of extractant 3 is 6.
After the suction filtration of extractant 3, reduced pressure concentration under the conditions of 45 DEG C of gained smoke filtrate obtains concentrate 3.
After concentrate 3 stands 24h under the conditions of 4 DEG C, 30min is centrifuged with the rotating speed of 12000r/min, collects supernatant, will
30min is centrifuged with the rotating speed of 12000r/min after precipitation distillation water washing after centrifugation, supernatant is collected；Merge on gained twice
Clear liquid, obtains supernatant 3.
After supernatant 3 freezes 1h under the conditions of -40 DEG C, it is dried in vacuum drier under the conditions of -0.05MPa, 60 DEG C；
Gained dry products recrystallizing methanol, obtains the 0.238g of chlorogenic acid product 3.
In the present embodiment, the yield of chlorogenic acid product 3 is 84.82%, and the purity of chlorogenic acid product 3 is 1.703%.
In sum, the invention provides a kind of extracting method of tobacco leaf Content of Chlorogenic Acid, the extracting method is：Step
First, extract：After tobacco leaf mixes with extractant, it is heated at reflux, obtains leaching liquor；Step 2, concentration：After the leaching liquor concentration, obtain
Concentrate；Step 3：Purification：The concentrate purification, obtains chlorogenic acid.Jing measurings can be obtained, the technical side that the present invention is provided
Case, extracts the chlorogenic acid purity for obtaining and can reach 87.4%, and the yield of chlorogenic acid can obtain 1.762%.The technology that the present invention is provided
In scheme, raw material is waste/hypo-tobacco leaf, and cost of material is low, meets the objective of current green society twice laid；Meanwhile, the present invention
The technical scheme of offer, it is simple and convenient, it is adapted to industrialization large-scale promotion.In solving prior art, tobacco leaf Content of Chlorogenic Acid
Extracting method has high cost, is not suitable for industrializing the technological deficiency extracted.The extracting method that the present invention is provided, simply, just
Victory, it is with low cost, it is suitable for large-scale industrialization popularization.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of extracting method of tobacco leaf Content of Chlorogenic Acid, it is characterised in that the extracting method is：
Step one, extraction：After tobacco leaf mixes with extractant, it is heated at reflux, obtains leaching liquor；
Step 2, concentration：After the leaching liquor concentration, concentrate is obtained；
Step 3：Purification：The concentrate purification, obtains chlorogenic acid.
2. extracting method according to claim 1, it is characterised in that the extracting method also includes：Pretreatment, it is described pre-
Process is carried out before the extraction；
The method of the pretreatment is：It is size-reduced and sieve successively after tobacco leaf drying, obtain prefinished products.
3. extracting method according to claim 2, it is characterised in that the temperature of the drying is 50～60 DEG C, the baking
The dry time is 48～72h, and the particle diameter of the prefinished products is 40 mesh.
4. extracting method according to claim 1, it is characterised in that the extractant is ethanol that mass fraction is 95%
The aqueous solution, the pH of the extractant is 4～6.
5. extracting method according to claim 1, it is characterised in that the extracting method also includes：Suction filtration：
The suction filtration is carried out between the step one and step 2.
6. extracting method according to claim 1, it is characterised in that the temperature being heated at reflux is 60～80 DEG C, institute
It is 75～105min to state time for being heated at reflux.
7. extracting method according to claim 1, it is characterised in that the method for the concentration is reduced pressure concentration, described to subtract
The temperature of pressure concentration is 40～45 DEG C.
8. extracting method according to claim 1, it is characterised in that the method for the purification is：The concentrate stands
Afterwards, supernatant is collected by centrifugation, the supernatant is freeze-dried successively and recrystallizes, and obtains chlorogenic acid.
9. extracting method according to claim 8, it is characterised in that the temperature of the standing is 4 DEG C, the standing when
Between be 12～24h；
The rotating speed of the centrifugation is 12000r/min, and the time of the centrifugation is 20～30min；
The solvent of the recrystallization is methyl alcohol.
10. extracting method according to claim 8, it is characterised in that the cryodesiccated method is：The supernatant
Freeze in -40 DEG C～-60 DEG C after 0.5～1h, be dried under the conditions of -0.05～-0.09MPa and 40～60 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611266573.4A CN106631797A (en) | 2016-12-31 | 2016-12-31 | Extraction method of chlorogenic acid in tobacco leaves |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611266573.4A CN106631797A (en) | 2016-12-31 | 2016-12-31 | Extraction method of chlorogenic acid in tobacco leaves |
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| CN106631797A true CN106631797A (en) | 2017-05-10 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201611266573.4A Pending CN106631797A (en) | 2016-12-31 | 2016-12-31 | Extraction method of chlorogenic acid in tobacco leaves |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107879937A (en) * | 2017-10-24 | 2018-04-06 | 四川九章生物科技有限公司 | A kind of new crystal of chlorogenic acid and preparation method thereof |
| CN108918711A (en) * | 2018-07-16 | 2018-11-30 | 中国烟草总公司郑州烟草研究院 | The detection method of polyphenol compound in a kind of tobacco leaf |
| CN112961136A (en) * | 2021-02-06 | 2021-06-15 | 云南省烟草公司玉溪市公司 | Method for extracting polyphenol from tobacco leaves |
-
2016
- 2016-12-31 CN CN201611266573.4A patent/CN106631797A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 艾心灵等: "大孔树脂吸附分离烟草绿原酸的研究", 《天然产物研究与开发》 * |
| 詹益兴: "《绿色精细化工——天然产品制造法》", 31 December 2005, 科学技术文献出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107879937A (en) * | 2017-10-24 | 2018-04-06 | 四川九章生物科技有限公司 | A kind of new crystal of chlorogenic acid and preparation method thereof |
| CN108918711A (en) * | 2018-07-16 | 2018-11-30 | 中国烟草总公司郑州烟草研究院 | The detection method of polyphenol compound in a kind of tobacco leaf |
| CN108918711B (en) * | 2018-07-16 | 2021-05-18 | 中国烟草总公司郑州烟草研究院 | Detection method of polyphenol compounds in tobacco leaves |
| CN112961136A (en) * | 2021-02-06 | 2021-06-15 | 云南省烟草公司玉溪市公司 | Method for extracting polyphenol from tobacco leaves |
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