CN112159383A - Method for extracting procyanidine from cortex Pini - Google Patents
Method for extracting procyanidine from cortex Pini Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
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- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a method for extracting procyanidine by using pine bark, which comprises the following steps of taking the cortex of the pine bark as a raw material, and adding water with the weight 10-20 times that of the raw material for extraction to obtain an extracting solution; keeping the extracting solution at the temperature of 50-70 ℃ for 1-2 hours, centrifuging the extracting solution, and removing fine particles and residues to obtain a centrifugal solution; standing the centrifugate for 2-4 hours to obtain a clear extracting solution; slowly introducing the clear extractive solution into macroporous resin column, performing selective adsorption, washing the resin with purified water or deionized water, discharging impurities, and eluting with 30-50% ethanol for 2-3 times to obtain alcoholic eluate of procyanidin; further concentrating the eluate to obtain a concentrated solution with a percentage concentration of 11-18%; drying the concentrated solution at 210-220 deg.C to obtain powdered procyanidin, inspecting, and packaging. The process is simple and easy to operate, the raw materials are pine bark with rich resources and low price, and the high added value of the pine bark is fully developed while the production cost is reduced.
Description
Technical Field
The invention relates to the field of preparation of procyanidine, in particular to a method for extracting procyanidine from pine bark.
Background
With the improvement of modern living standard and quality, people's health consciousness is increasingly enhanced, and procyanidine with excellent physiological characteristics and functions becomes a hot spot of people's attention. Because it has antioxidant, anti-inflammatory, antibacterial, antiaging, anticancer and cardiovascular, heart and vision protecting effects, procyanidin is used as an important health product and therapeutic drug for improving blood circulation, treating diabetic retinopathy, relieving edema and inhibiting varicosis. At the same time, procyanidins also play an important role as feed additives in animal husbandry. The previous research shows that the diarrhea of weaned piglets is mainly caused by the fact that the intestinal mucosa barrier function of the piglets is not complete, and the piglets are easily invaded by external pathogens during weaning to cause the oxidative stress injury of the intestinal mucosa and further cause the oxidative stress diarrhea. Theoretically, if a high-efficiency antioxidant can be found to relieve the damage of intestinal barriers caused by oxidative stress, diarrhea caused by weaning stress can be obviously reduced, and the production benefit of the pig industry is improved.
Procyanidin is a bioflavonoid with a special molecular structure, is formed by combining different amounts of catechin or epicatechin, is a high-efficiency cofactor, and is a substance which is internationally recognized as a natural antioxidant with the strongest activity, can remove free radicals and has an anti-aging effect. The antioxidant effect of the procyanidine is far stronger than that of the vitamin C and the vitamin E, and no side effect is found in the existing research; meanwhile, the antiallergic effect of the compound has attracted high attention of the scientific community and becomes an international popular research subject. The chemical components are divided into two main categories: oligomers with a low molecular weight and superior functionality, and polymers with a high molecular weight and slightly inferior functionality. Procyanidin has effects of scavenging free radicals in human body, preventing and treating cardiovascular disease and cerebrovascular disease, resisting tumor, resisting radiation, resisting inflammation, resisting allergy, etc., and has direct and indirect effects of preventing and treating various diseases of human body 70. Is also a beauty and health care product and has the reputation of skin vitamin and oral cosmetics. Therefore, procyanidins are widely applied to the cosmetic industry, the health food industry and the pharmaceutical industry, and are also used as preservatives and coloring agents of beverages, and are particularly pretty in the European and American markets.
In recent years, China pays more attention to the production of the pine bark procyanidin, and the production process is continuously improved and innovated. At present, some production processes are laggard, the working procedures are complex, the consumption is large, the heat energy consumption is high, and the time consumption is long; the cost is too high due to the above conditions, and the reasonability and the scientificity of the process are not enough, so that the quality of the product is influenced.
Disclosure of Invention
The invention overcomes the defects of the prior art and provides a method for extracting procyanidine by using pine bark.
In order to achieve the purpose, the invention adopts the technical scheme that: a method for extracting procyanidin from cortex Pini comprises the following steps: step S1: taking the cortex of pine bark as a raw material, adding water with the weight 10-20 times that of the raw material for extraction to obtain an extracting solution; step S2: keeping the extracting solution at the temperature of 50-70 ℃ for 1-2 hours, centrifuging the extracting solution, and removing fine particles and residues to obtain a centrifugal solution; standing the centrifugate for 2-4 hours to obtain a clear extracting solution; step S3: slowly introducing the clear extractive solution into macroporous resin column, performing selective adsorption, washing the resin with purified water or deionized water, discharging impurities, and eluting with 30-50% ethanol for 2-3 times to obtain alcoholic eluate of procyanidin; step S4: recovering alcohol at 60-80 deg.C under 0.6Mpa, and further concentrating the eluate to obtain 11-18% concentrated solution; step S5: drying the concentrated solution at 210-220 deg.C, introducing hot air at 110-150 deg.C for auxiliary evaporation to obtain powdered procyanidin, and packaging after inspection.
In a preferred embodiment of the invention, the extraction temperature is 30 ℃, the pressure is 30Mpa, the flow rate of CO2 is 2.78L/min, and the extraction time is 30 min.
In a preferred embodiment of the present invention, the centrifugal force in step S2 is 4000g to 6000g, and the time for centrifugation is 10min to 30 min.
In a preferred embodiment of the invention, the temperature of the concentrated and recovered alcohol is 40-70 ℃ until a high-purity concentrated solution with the mass percentage concentration of 15% is obtained.
In a preferred embodiment of the present invention, in step S4, the crude procyanidin is prepared into an aqueous solution, and then is adsorbed by macroporous adsorbent resin; then eluting with water and ethanol solution in sequence.
In a preferred embodiment of the invention, the eluent is ethanol water solution with the mass percentage concentration of 70-90%; the pH value of the eluent is 3.0-4.0.
In a preferred embodiment of the present invention, the alcohol eluent is vacuum filtered, and the filtrate is concentrated under reduced pressure to a viscous state and then dried.
The invention solves the defects in the background technology, and has the following beneficial effects:
(1) the preparation method of the procyanidine provided by the invention is simple and easy to operate, is beneficial to industrial application, and the selected raw materials are pine barks with abundant resources and low price, so that the high added value of the pine barks is fully developed while the production cost is reduced; compared with the organic solvent extraction commonly used in the current commercialization, the method has the advantages that the extraction solvent is water, the cost is reduced, the emission of organic solvents such as ethanol and methanol is obviously reduced, and the problem of environmental pollution caused by the emission of a large amount of organic waste liquid is effectively solved.
(2) The preparation method successfully extracts the procyanidin with a high success rate, greatly improves the extraction efficiency, realizes high-valued and high-efficiency utilization of the larch bark, applies the modern extraction technology to the fine utilization of the larch bark, and can expand the production raw materials of procyanidin products. The brand new high-efficiency utilization technology greatly improves the added value of bark utilization, the production has good economy and competitiveness, and the product has larger market demand.
(3) The invention has simple process flow, complete working hours of only about 10 hours, low equipment requirement, little alcohol consumption and low production cost. The raw material yield is high and reaches more than 10 percent, the yield of active ingredients is more than 80 percent, the content of the procyanidin can be effectively improved, and compared with the original production process, the alcohol consumption of each kilogram of procyanidin products is reduced to a great extent.
(4) The invention destroys the cell membrane of the pine bark by alcohol elution, increases the permeability of the cell membrane, accelerates the mass transfer process of the intracellular procyanidine to the extracellular space, greatly improves the extraction rate of the procyanidine and shortens the extraction time. In addition, the whole extraction process has mild conditions, and the problem of degradation of procyanidine caused by high-temperature heating is reduced.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart of a fabrication process according to a preferred embodiment of the present invention.
Detailed Description
In order that the above objects, features and advantages of the present invention can be more clearly understood, a more particular description of the invention will be rendered by reference to the appended drawings. It should be noted that the embodiments and features of the embodiments of the present application may be combined with each other without conflict.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced in other ways than those specifically described herein, and therefore the scope of the present invention is not limited by the specific embodiments disclosed below.
As shown in fig. 1, a method for extracting procyanidin from pine bark comprises: the method comprises the following steps: step S1: taking the cortex of pine bark as a raw material, adding water with the weight 10-20 times that of the raw material for extraction to obtain an extracting solution; step S2: keeping the extracting solution at the temperature of 50-70 ℃ for 1-2 hours, centrifuging the extracting solution, and removing fine particles and residues to obtain a centrifugal solution; standing the centrifugate for 2-4 hours to obtain a clear extracting solution; step S3: slowly introducing the clear extractive solution into macroporous resin column, performing selective adsorption, washing the resin with purified water or deionized water, discharging impurities, and eluting with 30-50% ethanol for 2-3 times to obtain alcoholic eluate of procyanidin; step S4: recovering alcohol at 60-80 deg.C under 0.6Mpa, and further concentrating the eluate to obtain 11-18% concentrated solution; step S5: drying the concentrated solution at 210-220 deg.C, introducing hot air at 110-150 deg.C for auxiliary evaporation to obtain powdered procyanidin, and packaging after inspection.
In a preferred embodiment of the invention, the extraction temperature is 30 ℃, the pressure is 30Mpa, the flow rate of CO2 is 2.78L/min, the extraction time is 30min, the centrifugal force is 4000g-6000g in step S2, the centrifugal time is 10min-30min, the temperature of concentrated recovered alcohol is 40-70 ℃ until high-purity concentrated solution with the mass percentage concentration of 15% is obtained, and the crude procyanidine is prepared into aqueous solution in step S4 and then is absorbed by macroporous absorption resin; then eluting with water and ethanol solution in sequence, wherein the eluent is ethanol water solution with the mass percentage concentration of 70-90%; the pH value of the eluent is 3.0-4.0, the alcoholic eluent is vacuum filtered, the filtrate is decompressed and concentrated to be in a viscous state, and then drying treatment is carried out.
In a preferred embodiment of the invention, the preparation method of the procyanidine is simple and easy to operate, and is beneficial to industrial application, and the selected raw materials are pine barks with abundant resources and low price, so that the high added value of the pine barks is fully developed while the production cost is reduced; compared with the organic solvent extraction commonly used in the current commercialization, the method has the advantages that the extraction solvent is water, the cost is reduced, the emission of organic solvents such as ethanol and methanol is obviously reduced, and the problem of environmental pollution caused by the emission of a large amount of organic waste liquid is effectively solved.
In a preferred embodiment of the invention, the preparation method has a high success rate to successfully extract the procyanidin, the extraction efficiency is greatly improved, the larch bark is highly valued and efficiently utilized, the modern extraction technology is applied to the fine utilization of the larch bark, and the production raw materials of the procyanidin product can be expanded. The brand new high-efficiency utilization technology greatly improves the added value of bark utilization, the production has good economy and competitiveness, and the product has larger market demand.
The invention has simple process flow, complete working hours of only about 10 hours, low equipment requirement, little alcohol consumption and low production cost. The raw material yield is high and reaches more than 10 percent, the yield of active ingredients is more than 80 percent, the content of the procyanidin can be effectively improved, and compared with the original production process, the alcohol consumption of each kilogram of procyanidin products is reduced to a great extent.
The invention destroys the cell membrane of the pine bark by alcohol elution, increases the permeability of the cell membrane, accelerates the mass transfer process of the intracellular procyanidine to the extracellular space, greatly improves the extraction rate of the procyanidine and shortens the extraction time. In addition, the whole extraction process has mild conditions, and the problem of degradation of procyanidine caused by high-temperature heating is reduced.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (7)
1. A method for extracting procyanidine from pine barks is characterized by comprising the following steps:
step S1: taking the cortex of pine bark as a raw material, adding water with the weight 10-20 times that of the raw material for extraction to obtain an extracting solution;
step S2: keeping the extracting solution at the temperature of 50-70 ℃ for 1-2 hours, centrifuging the extracting solution, and removing fine particles and residues to obtain a centrifugal solution; standing the centrifugate for 2-4 hours to obtain a clear extracting solution;
step S3: slowly introducing the clear extractive solution into macroporous resin column, performing selective adsorption, washing the resin with purified water or deionized water, discharging impurities, and eluting with 30-50% ethanol for 2-3 times to obtain alcoholic eluate of procyanidin;
step S4: recovering alcohol at 60-80 deg.C under 0.6Mpa, and further concentrating the eluate to obtain 11-18% concentrated solution;
step S5: drying the concentrated solution at 210-220 deg.C, introducing hot air at 110-150 deg.C for auxiliary evaporation to obtain powdered procyanidin, and packaging after inspection.
2. The method for extracting procyanidins from pine barks as claimed in claim 1, wherein the method comprises the steps of: the extraction temperature is 30 ℃, the pressure is 30Mpa, the flow rate of CO2 is 2.78L/min, and the extraction time is 30 min.
3. The method for extracting procyanidins from pine barks as claimed in claim 1, wherein the method comprises the steps of: in the step S2, the centrifugal force is 4000g-6000g, and the centrifugal time is 10min-30 min.
4. The method for extracting procyanidins from pine barks as claimed in claim 1, wherein the method comprises the steps of: the temperature of the concentrated recovered alcohol is 40-70 ℃ until a high-purity concentrated solution with the mass percentage concentration of 15% is obtained.
5. The method for extracting procyanidins from pine barks as claimed in claim 1, wherein the method comprises the steps of: in the step S4, the crude procyanidine product is prepared into an aqueous solution and then is absorbed by macroporous absorption resin; then eluting with water and ethanol solution in sequence.
6. The method for extracting procyanidins from pine barks as claimed in claim 1, wherein the method comprises the steps of: the eluent is ethanol water solution with the mass percentage concentration of 70-90 percent; the pH value of the eluent is 3.0-4.0.
7. The method for extracting procyanidins from pine barks as claimed in claim 1, wherein the method comprises the steps of: and (3) carrying out vacuum filtration on the alcoholic eluent, concentrating the filtrate under reduced pressure to be in a viscous state, and then drying.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1923830A (en) * | 2005-09-01 | 2007-03-07 | 浙江瑞康生物技术有限公司 | Preparation process of pine bark proanthocyanidin |
| CN102093328A (en) * | 2010-12-20 | 2011-06-15 | 大兴安岭林格贝有机食品有限责任公司 | Method for enriching and purifying procyanidin in pine bark |
| CN102532086A (en) * | 2012-01-12 | 2012-07-04 | 北京林业大学 | Method for extracting proanthocyanidins from dahurian larch bark |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1923830A (en) * | 2005-09-01 | 2007-03-07 | 浙江瑞康生物技术有限公司 | Preparation process of pine bark proanthocyanidin |
| CN102093328A (en) * | 2010-12-20 | 2011-06-15 | 大兴安岭林格贝有机食品有限责任公司 | Method for enriching and purifying procyanidin in pine bark |
| CN102532086A (en) * | 2012-01-12 | 2012-07-04 | 北京林业大学 | Method for extracting proanthocyanidins from dahurian larch bark |
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