CN106075108A - A kind of extracting method of Caulis Sacchari sinensis polyphenol - Google Patents
A kind of extracting method of Caulis Sacchari sinensis polyphenol Download PDFInfo
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- CN106075108A CN106075108A CN201610412044.4A CN201610412044A CN106075108A CN 106075108 A CN106075108 A CN 106075108A CN 201610412044 A CN201610412044 A CN 201610412044A CN 106075108 A CN106075108 A CN 106075108A
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- sacchari sinensis
- caulis sacchari
- polyphenol
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/899—Poaceae or Gramineae (Grass family), e.g. bamboo, corn or sugar cane
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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Abstract
The present invention relates to the extracting method of a kind of Caulis Sacchari sinensis polyphenol, through pretreatment of raw material → extract → filter → concentrate, reclaim → purification → concentrate, reclaim → be dried and to obtain Caulis Sacchari sinensis polyphenol.Use microwave radiation exaraction, after absorbing microwave energy, cell interior pressure exceedes cell wall expansion ability to bear and causes cell rupture, accelerate intracellular organic matter diffusion, the polar water molecules obtaining energy transfers energy to other materials, accelerate warm-up movement, thus improve extraction ratio and greatly reduce extraction time.Whole extraction process simply, easily operate, can realize continuous large-scale production, without chemical agent residue, it is ensured that Product quality and safety.
Description
Technical field
The present invention relates to the extracting method of a kind of Caulis Sacchari sinensis polyphenol, particularly from cane stalk, sugarcane toppers, leaf of Caulis Sacchari sinensis, Caulis Sacchari sinensis
Extraction to polyphenols in slag.
Background technology
The polyphenol compound contained in Caulis Sacchari sinensis is cinnamic acid and the predecessor of flavonoid of self-assembling formation under the effect of enzyme
It is derived, cane stalk, sugarcane toppers, leaf of Caulis Sacchari sinensis, bagasse all contains abundant polyphenols, especially at growing point
Sugarcane toppers position around is more concentrated.Research shows, Caulis Sacchari sinensis polyphenol has important biological activity and multiple pharmacological function.Energy
Enough effectively remove free radical, anti-lipid peroxidation, antitumor, mutation, atherosclerosis etc..In food, medicine, change
The every field such as cosmetic all have wide practical use.China's Caulis Sacchari sinensis aboundresources, but it is used for supplying sugar industry, industry is raw
The a large amount of bagasse produced in product often become waste material and not only pollute environment, more waste useful resource, and therefore exploitation Caulis Sacchari sinensis is many
Phenol products, the comprehensive utilization improving Caulis Sacchari sinensis is necessary.
Polyphenols in plant tissue generally and protein, polysaccharide form stable chemical combination with hydrogen bond and hydrophobic bond
Thing, polyphenol is intermolecular is also such.Extract reagent and not only polyphenol is had good dissolubility, and there is fracture hydrogen bond
Ability.Selecting alcohol-water mix reagent to extract Caulis Sacchari sinensis polyphenol, ethanol can be beneficial to many with the hydrogen bond between saboteur and hydrophobic bond
The release of phenol.Extracting method about Caulis Sacchari sinensis polyphenol need to optimize further at present.
Summary of the invention
In order to overcome deficiency of the prior art, it is achieved the effective utilization to Caulis Sacchari sinensis polyphenol, the present invention uses microwave-assisted
Being fully dissolved out of extraction, beneficially polyphenols.
The extracting method of a kind of Caulis Sacchari sinensis polyphenol, comprises the steps:
Step one: pretreatment of raw material: original sugarcane material is soaked in 80 ± 2 DEG C of water-baths 2-5min enzyme denaturing, is cooled to 10
Below DEG C, dewatering, smashing, freezing standby；
Step 2: extract: with 50-65% (volume ratio) ethanol solution as extractant, according to feed liquid weight ratio 1:5-1:10
Ratio, use microwave radiation exaraction, Extracting temperature is 55-65 DEG C, and extraction time is 10-20min, and power is 540W；
Step 3: filter: carry out sucking filtration through suction filter pump after extraction, isolate residue, obtain filtrate；
Step 4: concentrate, reclaim: concentrated by rotated for filtrate in step 3 vaporizer, obtains Caulis Sacchari sinensis polyphenol concentrated solution
1, and reclaim ethanol；
Step 5: purification: Caulis Sacchari sinensis polyphenol concentrated solution 1 in step 4 is adsorbed through NKA-9 type macroporous resin, and uses
60%-80% (volume ratio) ethanol solution carries out eluting, obtains Caulis Sacchari sinensis polyphenol eluent；
Step 6: concentrate, reclaim: the rotated vaporizer of Caulis Sacchari sinensis polyphenol eluent in step 5 is concentrated, obtains Caulis Sacchari sinensis
Polyphenol concentrated solution 2, and reclaim ethanol；
Step 7: be dried: by Caulis Sacchari sinensis polyphenol concentrated solution 2 vacuum freeze-drying in step 6, obtain Caulis Sacchari sinensis polyphenol.
In described step 3, the pressure of sucking filtration is 20-30MPa.
In described step 4 and step 6, thickening temperature is 55-65 DEG C, and the time is 1-2h, and vacuum is 0.01-
0.015KPa。
In described step 7 vacuum freeze-drying be temperature be 60-70 DEG C, vacuum be 0.02-0.03KPa under the conditions of enter
Row, dry to moisture less than 4%.
In described step one, original sugarcane material is cane stalk, sugarcane toppers, leaf of Caulis Sacchari sinensis or bagasse.
When original sugarcane material is cane stalk in described step one, also include the step removed the peel by cane stalk.
The beneficial effects of the present invention is: utilize high temperature to soak enzyme denaturing in short-term, can effectively prevent enzyme effect in Caulis Sacchari sinensis
Enzymatic browning is caused to cause aldehydes matter to convert to quinones substance in aldehydes matter.Use microwave radiation exaraction, absorb microwave
After energy, cell interior pressure exceedes cell wall expansion ability to bear and causes cell rupture, accelerates intracellular organic matter diffusion, it is thus achieved that energy
The polar water molecules of amount transfers energy to other materials, accelerates warm-up movement, when thus improving extraction ratio and greatly reduce extraction
Between.Remove bulky grain insoluble matter, the rotated evaporation and concentration of filtrate through sucking filtration after extraction, obtain Caulis Sacchari sinensis polyphenol concentrated solution, sweet
Sugarcane polyphenol yield is up to 70%, and reclaims ethanol.The absorption of macroporous resin is the most clear to the impurity in Caulis Sacchari sinensis polyphenol concentrated solution
Removing, and carry out eluting with ethanol solution, rotated evaporation and concentration obtains the Caulis Sacchari sinensis polyphenol concentrated solution that purity is about 35%.Select
Caulis Sacchari sinensis polyphenol concentrated solution is dried by vacuum freeze-drying mode, and protection polyphenols is not destroyed to the full extent.Whole carry
Take process simply, easily operate, continuous large-scale production can be realized, without chemical agent residue, it is ensured that Product quality and safety.
Detailed description of the invention
Below by the description to embodiment, and the present invention is made further details of using cane stalk as original sugarcane material
Illustrate, to help those skilled in the art that inventive concept, the technical scheme of the present invention are had more complete, accurate and deep reason
Solve.
Embodiment 1
Step one: pretreatment of raw material: soak 2min enzyme denaturing after being removed the peel by cane stalk in 80 ± 2 DEG C of water-baths, be cooled to 10
Below DEG C, dewatering, smashing, freezing standby；
Step 2: extract:, adopt according to the ratio of feed liquid weight ratio 1:7 as extractant with 50% (volume ratio) ethanol solution
With microwave radiation exaraction, Extracting temperature is 55 DEG C, and extraction time is 10min, and power is 540W；
Step 3: filter: carrying out sucking filtration through suction filter pump after extraction, sucking filtration pressure is 20MPa, isolates residue, obtains filtrate；
Step 4: concentrate, reclaim: rotated for filtrate in step 3 vaporizer is concentrated, thickening temperature is 55 DEG C, time
Between be 1h, vacuum is 0.01Kpa, obtains Caulis Sacchari sinensis polyphenol concentrated solution 1, and reclaims ethanol；
Step 5: purification: Caulis Sacchari sinensis polyphenol concentrated solution 1 in step 4 is adsorbed through NKA-9 type macroporous resin, and uses
60% (volume ratio) ethanol solution carries out eluting, obtains Caulis Sacchari sinensis polyphenol eluent；
Step 6: concentrate, reclaim: concentrated by the rotated vaporizer of Caulis Sacchari sinensis polyphenol eluent in step 5, concentrates temperature
Degree is 55 DEG C, and the time is 1h, and vacuum is 0.01Kpa, obtains Caulis Sacchari sinensis polyphenol concentrated solution 2, and reclaims ethanol；
Step 7: be dried: by Caulis Sacchari sinensis polyphenol concentrated solution 2 in step 6 temperature be 60 DEG C, vacuum be 0.02Kpa condition
Lower vacuum freeze-drying, obtains Caulis Sacchari sinensis polyphenol.
Embodiment 2
Step one: pretreatment of raw material: soak 3min enzyme denaturing after being removed the peel by cane stalk in 80 ± 2 DEG C of water-baths, be cooled to 10
Below DEG C, dewatering, smashing, freezing standby；
Step 2: extract:, adopt according to the ratio of feed liquid weight ratio 1:5 as extractant with 60% (volume ratio) ethanol solution
With microwave radiation exaraction, Extracting temperature is 65 DEG C, and extraction time is 20min, and power is 540W；
Step 3: filter: carrying out sucking filtration through suction filter pump after extraction, sucking filtration pressure is 30MPa, isolates residue, obtains filtrate；
Step 4: concentrate, reclaim: rotated for filtrate in step 3 vaporizer is concentrated, thickening temperature is 65 DEG C, time
Between be 1.5h, vacuum is 0.01Kpa, obtains Caulis Sacchari sinensis polyphenol concentrated solution 1, and reclaims ethanol；
Step 5: purification: Caulis Sacchari sinensis polyphenol concentrated solution 1 in step 4 is adsorbed through NKA-9 type macroporous resin, and uses
70% (volume ratio) ethanol solution carries out eluting, obtains Caulis Sacchari sinensis polyphenol eluent；
Step 6: concentrate, reclaim: concentrated by the rotated vaporizer of Caulis Sacchari sinensis polyphenol eluent in step 5, concentrates temperature
Degree is 65 DEG C, and the time is 1.5h, and vacuum is 0.01Kpa, obtains Caulis Sacchari sinensis polyphenol concentrated solution 2, and reclaims ethanol；
Step 7: be dried: by Caulis Sacchari sinensis polyphenol concentrated solution 2 in step 6 temperature be 60 DEG C, vacuum be 0.02Kpa condition
Lower vacuum freeze-drying, obtains Caulis Sacchari sinensis polyphenol.
Embodiment 3
Step one: pretreatment of raw material: soak 5min enzyme denaturing after being removed the peel by cane stalk in 80 ± 2 DEG C of water-baths, be cooled to 10
Below DEG C, dewatering, smashing, freezing standby；
Step 2: extract: with 65% (volume ratio) ethanol solution as extractant, according to the ratio of feed liquid weight ratio 1:10,
Using microwave radiation exaraction, Extracting temperature is 65 DEG C, and extraction time is 20min, and power is 540W；
Step 3: filter: carrying out sucking filtration through suction filter pump after extraction, sucking filtration pressure is 30MPa, isolates residue, obtains filtrate；
Step 4: concentrate, reclaim: rotated for filtrate in step 3 vaporizer is concentrated, thickening temperature is 65 DEG C, time
Between be 2h, vacuum is 0.015Kpa, obtains Caulis Sacchari sinensis polyphenol concentrated solution 1, and reclaims ethanol；
Step 5: purification: Caulis Sacchari sinensis polyphenol concentrated solution 1 in step 4 is adsorbed through NKA-9 type macroporous resin, and uses
80% (volume ratio) ethanol solution carries out eluting, obtains Caulis Sacchari sinensis polyphenol eluent；
Step 6: concentrate, reclaim: concentrated by the rotated vaporizer of Caulis Sacchari sinensis polyphenol eluent in step 5, concentrates temperature
Degree is 65 DEG C, and the time is 2h, and vacuum is 0.015Kpa, obtains Caulis Sacchari sinensis polyphenol concentrated solution 2, and reclaims ethanol；
Step 7: be dried: by Caulis Sacchari sinensis polyphenol concentrated solution 2 in step 6 temperature be 70 DEG C, vacuum be 0.03Kpa condition
Lower vacuum freeze-drying, obtains Caulis Sacchari sinensis polyphenol.
Above the present invention is exemplarily described, it is clear that the present invention implements and is not subject to the restrictions described above,
As long as the improvement of the various unsubstantialities that the method design that have employed the present invention is carried out with technical scheme, or the most improved by this
Bright design and technical scheme directly apply to other occasion, all within protection scope of the present invention.
Claims (7)
1. the extracting method of a Caulis Sacchari sinensis polyphenol, it is characterised in that comprise the steps:
Step one: pretreatment of raw material: original sugarcane material is soaked in 80 ± 2 DEG C of water-baths 2-5min enzyme denaturing, be cooled to 10 DEG C with
Under, dewatering, smashing, freezing standby；
Step 2: extract: with 50-65% ethanol solution as extractant, according to the ratio of feed liquid weight ratio 1:5-1:10, use micro-
Ripple assisted extraction, Extracting temperature is 55-65 DEG C, and extraction time is 10-20min, and power is 540W；
Step 3: filter: carry out sucking filtration through suction filter pump after extraction, isolate residue, obtain filtrate；
Step 4: concentrate, reclaim: concentrated by rotated for filtrate in step 3 vaporizer, obtains Caulis Sacchari sinensis polyphenol concentrated solution 1, and
Reclaim ethanol；
Step 5: purification: Caulis Sacchari sinensis polyphenol concentrated solution 1 in step 4 is adsorbed through NKA-9 type macroporous resin, and uses 60%-
80% ethanol solution carries out eluting, obtains Caulis Sacchari sinensis polyphenol eluent；
Step 6: concentrate, reclaim: the rotated vaporizer of Caulis Sacchari sinensis polyphenol eluent in step 5 is concentrated, obtains Caulis Sacchari sinensis polyphenol
Concentrated solution 2, and reclaim ethanol；
Step 7: be dried: by Caulis Sacchari sinensis polyphenol concentrated solution 2 vacuum freeze-drying in step 6, obtain Caulis Sacchari sinensis polyphenol.
The extracting method of a kind of Caulis Sacchari sinensis polyphenol the most according to claim 1, it is characterised in that: the pressure of sucking filtration in step 3
For 20-30MPa.
The extracting method of a kind of Caulis Sacchari sinensis polyphenol the most according to claim 1, it is characterised in that: dense in step 4 and step 6
Contracting temperature is 55-65 DEG C, and the time is 1-2h, and vacuum is 0.01-0.015KPa.
The extracting method of a kind of Caulis Sacchari sinensis polyphenol the most according to claim 1, it is characterised in that: in step 7, vacuum freeze-drying is
Temperature be 60-70 DEG C, vacuum be 0.02-0.03KPa under the conditions of carry out, dry to moisture less than 4%.
5. according to the extracting method of a kind of Caulis Sacchari sinensis polyphenol described in any one of claim 1-4, it is characterised in that: described step one
Middle original sugarcane material is cane stalk, sugarcane toppers, leaf of Caulis Sacchari sinensis or bagasse.
The extracting method of a kind of Caulis Sacchari sinensis polyphenol the most according to claim 5, it is characterised in that: original sugarcane in described step one
Material is cane stalk.
The extracting method of a kind of Caulis Sacchari sinensis polyphenol the most according to claim 6, it is characterised in that: step one also includes Caulis Sacchari sinensis
The step of stem peeling.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610412044.4A CN106075108A (en) | 2016-06-14 | 2016-06-14 | A kind of extracting method of Caulis Sacchari sinensis polyphenol |
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| CN201610412044.4A CN106075108A (en) | 2016-06-14 | 2016-06-14 | A kind of extracting method of Caulis Sacchari sinensis polyphenol |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113197975A (en) * | 2021-03-25 | 2021-08-03 | 中国科学院微生物研究所 | Preparation method and application of sugarcane leaf polyphenol |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102516319A (en) * | 2011-12-08 | 2012-06-27 | 广西大学 | Method for extracting phenolic compounds from sugarcane tips |
| CN104306758A (en) * | 2014-09-28 | 2015-01-28 | 广西大学 | Method for extracting polyphenol from sugar cane bark |
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2016
- 2016-06-14 CN CN201610412044.4A patent/CN106075108A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102516319A (en) * | 2011-12-08 | 2012-06-27 | 广西大学 | Method for extracting phenolic compounds from sugarcane tips |
| CN104306758A (en) * | 2014-09-28 | 2015-01-28 | 广西大学 | Method for extracting polyphenol from sugar cane bark |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113197975A (en) * | 2021-03-25 | 2021-08-03 | 中国科学院微生物研究所 | Preparation method and application of sugarcane leaf polyphenol |
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Application publication date: 20161109 |