CN108112855A - A kind of method that wholefood antioxidant is extracted from areca leaf - Google Patents
A kind of method that wholefood antioxidant is extracted from areca leaf Download PDFInfo
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Abstract
The invention belongs to the technical fields of food additives, provide a kind of method that wholefood antioxidant is extracted from areca leaf.This method cleans areca leaf, dry after crush, then mixed with acid, alcohols material and water, it adds in progress ultrasound-assisted extraction in extractor and obtains extracting solution, then extracting solution is concentrated, infrared drying, you can wholefood antioxidant is made.Compared with conventional method, the present invention the extracting method time is short, recovery rate is high, all from natural component, antioxygen property is good for the polyphenol compound of gained, medical performance is good, it has no toxic side effect, and entire extracting method raw material is easy to get, and process is simple, cost is relatively low, pollute it is small, the invention have certain development and application values, can be applicable.
Description
Technical field
The invention belongs to the technical fields of food additives, provide one kind and wholefood antioxidant is extracted from areca leaf
Method.
Background technology
Polyphenols refers to the general designation of chemical substance in one group of plant, gains the name when containing multiple phenolic group group, can be used as excellent
Antioxidant resource, in entire plant kingdom, containing polyphenol or phenolic compound and its derivative up to 6500 kinds or more, these are all
Secondary side-products in vegetable metabolic process are present in many light water fruits and vegetables, are that people absorb quantity from food daily
Most antioxidant.Polyphenol compound also has in addition in there is good anti-oxidation function and strengthens vascular wall, stomach is promoted to disappear
Change, reducing blood lipid, enhancing body immunity, preventing arteriosclerosis, thrombosis and diuresis, blood pressure lowering are inhibited bacteria and given birth to cancer cell
The effects that long.Therefore the extraction to polyphenol compound and application are concerned by people.
Polyphenol compound extracting method is varied, and widely used method has organic solvent extractionprocess, is the most frequently used
A kind of extracting method, because of different solubility of the different material in different solvents, according to the principle of " similar to mix ", certain
Under conditions of target substance is separated, this method is at low cost and easy to operate, is widely used, but there is extraction efficiencies
The problems such as low, of high cost, complicated for operation, therefore Novel supercritical CO2 extractions, ultrasound-assisted extraction method, microwave radiation technology extract
It follows the example of and is increasingly taken seriously with biological enzymolysis extraction etc..Wherein, the mechanism of ultrasonic wave assisted extraction comes from its cavitation
The reinforcing power brought, the effect cause mechanical effect, cavitation effect and fuel factor etc., strengthen the release of intracellular matter,
Diffusion and dissolving, so as to accelerate the leaching of active ingredient, have it is easy to operate, Extracting temperature is low, extraction efficiency is high, extract
The features such as structure is survivable.
At this stage, it is that polyphenol compound is ground to find and screen more healthier polyphenol compound plants that can extract
Study carefully the important directions of application development.It is that one kind has potential reproducibility very much to have now found that the catechin contained in areca leaf
Polyatomic phenol substance, easy oxidation by air, is commonly used for antioxidant in aqueous solution, has prevention and cure of cardiovascular disease, pre- anti-cancer
The multiple functions such as disease, therefore with preferable development prospect.
It has been achieved both at home and abroad in terms of the extraction of the extraction of natural plants antioxidant, especially polyphenol compound at present
Certain effect.Wherein a kind of extracting method of plant polyphenol in purple Chinese yam has been invented in Du Fang ridges et al.（Chinese invention patent application
Numbers 201710316882.6）, step is as follows：Purple Chinese yam crushes, and adds in ether, double（2- ethylhexyls）Disodium sulfosuccinate,
Carbon dioxide is passed through, is stirred, recycles ether, purple Chinese yam must be pre-processed, add in tetramethylammonium hydroxide ethanol solution, filtered, dried
It is dry, it sieves after grinding, obtains purple Chinese yam powder；Purple Chinese yam powder is added in into ionic liquid, Ultrasonic Heating filters after extracting 2 times, from
The heart, the concentrate that lower floor obtains are ionic liquid recovery, and water layer is purple Chinese yam polyphenol extracting solution；By purple Chinese yam polyphenol
Extracting solution freeze-drying process.In addition, Wang Weixiang et al. has invented a kind of double-aqueous phase system extraction oil olive leaf polyphenol
Method（Chinese invention patent application number 201510211626.1）, include the following steps：The olive growing leaves of drying and crushing are added to
In hydrophilic small molecules organic solvent and inorganic salt solution double-aqueous phase system, mixing carries out ultrasonic extraction, olive growing leaves polyphenol extraction
Get phase；Upper phase passes through macroporous adsorbing resin for purification, and organic solvent elution, eluent is concentrated, dry to get olive growing leaves
Polyphenol.
As it can be seen that existing in the prior art but there is the time is long, recovery rate is low, of high cost, heavy contamination, complicated for operation etc.
The shortcomings of problem, and at present using more general polyphenol compound antioxygen property is relatively low, security is poor, it is same with this
When, catechin is a kind of polyphenol compound antioxidant of great potential in areca leaf, but without corresponding extraction and application aspect
Research.
The content of the invention
For such case, the purpose of invention is to provide a kind of method that wholefood antioxidant is extracted from areca leaf,
It can solve that traditional polyphenol compound antioxidant extracting method time is long, recovery rate is low, of high cost, heavy contamination, operation are multiple
The shortcomings of the problems such as miscellaneous, and the antioxygen property of gained polyphenol compound is higher, security is good.Obtained polyphenol compound
With certain anti-oxidant, antibacterial isoreactivity, it can be used as food antioxidant, all from natural component, have no toxic side effect,
With certain development and application values.
Specific technical solution of the present invention is as follows：
It is a kind of from areca leaf extract wholefood antioxidant method, areca leaf is cleaned, dry after crush, Ran Houyu
Acid, alcohols material and water mixing, add in extractor and carry out ultrasound-assisted extraction, obtain extracting solution, then will extraction
Liquid is concentrated, infrared drying, you can wholefood antioxidant is made, preparation is as follows：
（1）Take grow fine, the blade of the betelnut tree of no disease and pests harm, it is miscellaneous that soil, greasy dirt, insect on blade etc. are cleaned with clear water
Matter is placed in drying equipment and removes the partial moisture of surface moisture and inside, then adds in leaf slicing shredder, after crushing
It sieves, the areca leaf particle for taking 20~50 mesh is for use；
（2）Acid, alcohols material and water are mixed, are made into acidity alcohol solution, adds in extractor, then adds in step
（1）The areca leaf particle of gained is impregnated, and uses ultrasonic wave assisted extraction, under the action of acid, Polyphenols object
Matter can generate salt and accelerate the dissolving in alcohols material, and ultrasonic wave can destroy the cell membrane of plant, make intracellular reactive object
Matter is exposed, promotes contacting directly for active material and acidity alcohol solution；Wherein, 1~2 parts by weight of acid, alcohols material 40
~60 parts by weight, 38~59 parts by weight of water；
（3）By step（2）Extracting solution concentrated using thin film evaporator, be then dried using infrared drier,
Until moisture content is less than 5%, you can wholefood antioxidant is made.
Preferably, step（1）The betelnut tree be cigarette fruit betel nut, Chinese olive betel nut, smokeless betel nut or black fruit betel nut in extremely
Few one kind.
Preferably, step（1）The drying equipment turns round vacuum desiccator, vacuum rake dryer or vacuum for bicone
One kind in baking oven.
Preferably, step（1）Drying temperature is 60~80 DEG C, and drying time is 10~15min.
Preferably, step（1）The dried moisture content of betel nut blade should be not higher than 10%.
Preferably, step（1）The slicer number of the leaf slicing shredder is 2~4, the number of crushing knife and flail knife
Mesh is 8~12, and cutterhead revolution is 2300~2500r/min during crushing.
Preferably, step（2）The acid is hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, boric acid, hydrobromic acid, hydroiodic acid, secondary
At least one of chloric acid or hypoiodous acid.
Preferably, step（2）The alcohols material is ethyl alcohol, ethylene glycol, normal propyl alcohol, isopropanol, glycerine, 1,2- dipropyls
At least one of alcohol, n-butanol, isobutanol, sec-butyl alcohol or tert-butyl alcohol.
Preferably, step（2）The extractor is laminated to for right cone formula multifunctional extracting pot or oblique conic multifunctional extracting pot, folder
0.3~0.5MPa, pressure inside the tank are 0.08~0.1MPa, and heating power is 6~10kW, stirring motor power for 0.2~
0.4kW, speed of agitator are 200~300r/min.
Preferably, step（2）The ultrasonic power of the assisted extraction is 500~1000W, and frequency is 40~80Hz.
Preferably, step（2）The time of the ultrasonic wave auxiliary soak extraction is 2~4h.
Preferably, step（3）The thin film evaporator can be film-rising evaporator, downward film evaporator, scraper-type evaporation
One kind in device or centrifugal evaporator, material heated time are 0.5~1s.
Preferably, step（3）The infrared drier can be that oscillatory type infrared drier or tunnel type infrared ray dry
One kind in room.
Preferably, step（3）During the infrared drying, a length of 200~400nm of infrared wave, power for 10~
20kW, drying time are 30~60min.
By the method and organic solvent extractionprocess, microwave-assisted and biological enzyme of present invention extraction polyphenol compound
Recovery rate, extraction time, antioxygen property, toxic side effect, the feature of environmental protection and the extraction cost of solution extraction are compared, such as 1 institute of table
Show, it is seen then that method of the invention can improve the extraction efficiency of antioxidant, while products obtained therefrom excellent performance, and application value is high, fit
It is added together in food.
Table 1：
The present invention provides a kind of methods that wholefood antioxidant is extracted from areca leaf, compared with prior art, protrude
The characteristics of and excellent effect be：
1. the polyphenol compound that the present invention extracts, antioxygen property is good, is suitable for food addition.
2. the extracting method of the present invention employs acidity alcohol solution as extraction organic solvent, polyphenols can generate
Salt and quickly dissolved in alcohols material, and ultrasonic wave can destroy the cell membrane of plant, make intracellular reactive packaged material, promote
Contacting directly for active material and acidity alcohol solution, improves the recovery rate and extraction efficiency of polyphenols.
3. antioxidant has no toxic side effect all from natural component obtained by the extracting method of the present invention, development and application valency
Value is high.
4. the preparation method of the present invention, raw material are easy to get, process is simple, and cost is relatively low, and pollution is small, can large-scale promotion.
Specific embodiment
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Scope be only limitted to following example.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
Take grow fine, the blade of the black fruit betelnut tree of no disease and pests harm, soil, greasy dirt, insect on blade etc. are cleaned with clear water
Impurity is placed in bicone revolution vacuum desiccator, the dry 15min at a temperature of 80 DEG C, removes the portion of surface moisture and inside
Divide moisture, then add in leaf slicing shredder, crushed with the cutterhead revolution of 2300r/min, sieved, take the Bin of 20~50 mesh
Bulky leaf particle is for use；2kg hydrochloric acid, 50kg ethyl alcohol and 48kg water are mixed, are made into acidity alcohol solution, adds in the extraction of oblique conic multipotency
In tank, then add in areca leaf particle and impregnated, adjusting speed of agitator is 200r/min, and uses power as 1000W, frequency
For the ultrasonic wave assisted extraction of 80Hz, under the action of hydrochloric acid, polyphenols can generate salt and accelerate dissolving in ethanol,
And ultrasonic wave can destroy the cell membrane of plant, make intracellular reactive packaged material, promote the straight of active material and acidity alcohol solution
Contact, extraction time 3h；Extracting solution is concentrated using film-rising evaporator, then heated time 1s utilizes ripple
A length of 200nm, the infrared drier that power is 10kW dries 30min, until moisture content is less than 5%, you can wholefood is made
Antioxidant；
The method that embodiment 1 extracts wholefood antioxidant, Test extraction rate, extraction time, antioxygen property, toxic side effect and carries
Cost is taken, obtains that the results are shown in Table 2.
Embodiment 2
Take grow fine, the blade of the Chinese olive betelnut tree of no disease and pests harm, soil, greasy dirt, insect on blade etc. are cleaned with clear water
Impurity is placed in vacuum drying oven, the dry 12min at a temperature of 70 DEG C, removes the partial moisture of surface moisture and inside, Ran Houjia
Enter in leaf slicing shredder, crushed with the cutterhead revolution of 2500r/min, sieved, the areca leaf particle for taking 20~50 mesh is for use；
1kg phosphoric acid, 40kg glycerine and 59kg water are mixed, are made into acidity alcohol solution, is added in right cone formula multifunctional extracting pot, Ran Houjia
Enter areca leaf particle to be impregnated, adjusting speed of agitator is 300r/min, and uses power as 1000W, and frequency is the super of 40Hz
Sound wave assisted extraction, under the action of phosphoric acid, polyphenols can generate salt and accelerate the dissolving in glycerine, and ultrasonic wave
The cell membrane of plant can be destroyed, makes intracellular reactive packaged material, promotes contacting directly for active material and acidity alcohol solution, carries
It is 2h to take the time；Extracting solution using centrifugal evaporator is concentrated, heated time 1s, is then 400nm using wavelength,
The infrared drier that power is 10kW dries 60min, until moisture content is less than 5%, you can wholefood antioxidant is made；
The method that embodiment 2 extracts wholefood antioxidant, Test extraction rate, extraction time, antioxygen property, toxic side effect and carries
Cost is taken, obtains that the results are shown in Table 2.
Embodiment 3
Take grow fine, the blade of the smokeless betelnut tree of no disease and pests harm, soil, greasy dirt, insect on blade etc. are cleaned with clear water
Impurity is placed in vacuum rake dryer case, and the dry 15min at a temperature of 65 DEG C removes surface moisture and the part water of inside
Point, it then adds in leaf slicing shredder, is crushed with the cutterhead revolution of 2350r/min, sieved, take the areca leaf of 20~50 mesh
Particle is for use；2kg hypoiodous acid, 46kg sec-butyl alcohols and 52kg water are mixed, are made into acidity alcohol solution, adds in the extraction of oblique conic multipotency
In tank, then add in areca leaf particle and impregnated, adjusting speed of agitator is 250r/min, and uses power as 700W, frequency
For the ultrasonic wave assisted extraction of 60Hz, under the action of hypoiodous acid, polyphenols can generate salt and accelerate in sec-butyl alcohol
Dissolving, and ultrasonic wave can destroy the cell membrane of plant, make intracellular reactive packaged material, promote active material and acidity alcohol solution
Contact directly, extraction time 3h；Extracting solution is concentrated using downward film evaporator, heated time 0.5s, then
It is 300nm using wavelength, the infrared drier that power is 15kW dries 40min, until moisture content is less than 5%, you can day is made
Right food antioxidant；
The method that embodiment 3 extracts wholefood antioxidant, Test extraction rate, extraction time, antioxygen property, toxic side effect and carries
Cost is taken, obtains that the results are shown in Table 2.
Embodiment 4
Take grow fine, the blade of the black fruit betelnut tree of no disease and pests harm, soil, greasy dirt, insect on blade etc. are cleaned with clear water
Impurity is placed in bicone revolution vacuum desiccator, the dry 12min at a temperature of 75 DEG C, removes the portion of surface moisture and inside
Divide moisture, then add in leaf slicing shredder, crushed with the cutterhead revolution of 2400r/min, sieved, take the Bin of 20~50 mesh
Bulky leaf particle is for use；1kg hypoiodous acid, the 50kg tert-butyl alcohols and 49kg water are mixed, are made into acidity alcohol solution, adds in right cone formula multipotency
In extractor, then adding in areca leaf particle and impregnated, adjusting speed of agitator is 280r/min, and uses power as 800W,
Frequency is the ultrasonic wave assisted extraction of 75Hz, and under the action of hypoiodous acid, polyphenols can generate salt and accelerate in the tert-butyl alcohol
In dissolving, and ultrasonic wave can destroy the cell membrane of plant, make intracellular reactive packaged material, promote active material and acid alcohol
Solution contacts directly, extraction time 2h；Extracting solution is concentrated using scraper-type evaporator, heated time 1s, so
It is afterwards 200nm using wavelength, the infrared drier that power is 12kW dries 50min, until moisture content is less than 5%, you can be made
Wholefood antioxidant；
The method that embodiment 4 extracts wholefood antioxidant, Test extraction rate, extraction time, antioxygen property, toxic side effect and carries
Cost is taken, obtains that the results are shown in Table 2.
Embodiment 5
Take grow fine, the blade of the black fruit betelnut tree of no disease and pests harm, soil, greasy dirt, insect on blade etc. are cleaned with clear water
Impurity is placed in vacuum drying oven, the dry 12min at a temperature of 65 DEG C, removes the partial moisture of surface moisture and inside, Ran Houjia
Enter in leaf slicing shredder, crushed with the cutterhead revolution of 2500r/min, sieved, the areca leaf particle for taking 20~50 mesh is for use；
2kg hydrochloric acid, 60kg normal propyl alcohols and 38kg water are mixed, are made into acidity alcohol solution, is added in right cone formula multifunctional extracting pot, Ran Houjia
Enter areca leaf particle to be impregnated, adjusting speed of agitator is 280r/min, and uses power as 600W, and frequency is the ultrasound of 70Hz
Ripple assisted extraction, under the action of hydrochloric acid, polyphenols can generate salt and accelerate the dissolving in normal propyl alcohol, and ultrasonic wave can
The cell membrane of plant is destroyed, makes intracellular reactive packaged material, promotes contacting directly for active material and acidity alcohol solution, extracts
Time is 3h；Extracting solution using downward film evaporator is concentrated, heated time 0.5s, is then 350nm using wavelength,
The infrared drier that power is 12kW dries 40min, until moisture content is less than 5%, you can wholefood antioxidant is made；
The method that embodiment 5 extracts wholefood antioxidant, Test extraction rate, extraction time, antioxygen property, toxic side effect and carries
Cost is taken, obtains that the results are shown in Table 2.
Embodiment 6
Take grow fine, the blade of the Chinese olive betelnut tree of no disease and pests harm, soil, greasy dirt, insect on blade etc. are cleaned with clear water
Impurity is placed in vacuum rake dryer, the dry 10min at a temperature of 80 DEG C, removes the partial moisture of surface moisture and inside,
Then add in leaf slicing shredder, crushed with the cutterhead revolution of 2300r/min, sieved, take the areca leaf of 20~50 mesh
Grain is for use；1kg hydrobromic acids, 40kg ethylene glycol and 59kg water are mixed, are made into acidity alcohol solution, adds in oblique conic multifunctional extracting pot
In, it then adds in areca leaf particle and is impregnated, adjustings speed of agitator is 300r/min, and uses power frequency is for 500W
The ultrasonic wave assisted extraction of 40Hz, under the action of hydrobromic acid, polyphenols can generate salt and accelerate molten in ethylene glycol
Solution, and ultrasonic wave can destroy the cell membrane of plant, make intracellular reactive packaged material, promote active material and acidity alcohol solution
It contacts directly, extraction time 4h；Extracting solution is concentrated using scraper-type evaporator, heated time 0.5s, Ran Houli
It is 400nm with wavelength, the infrared drier that power is 10kW dries 60min, until moisture content is less than 5%, you can is made natural
Food antioxidant；
The method that embodiment 6 extracts wholefood antioxidant, Test extraction rate, extraction time, antioxygen property, toxic side effect and carries
Cost is taken, obtains that the results are shown in Table 2.
Comparative example 1
In extraction process, not using acid, other preparation conditions and embodiment 6 are consistent；
To comparative example 1 extract wholefood antioxidant method, Test extraction rate, extraction time, antioxygen property, toxic side effect,
The feature of environmental protection and extraction cost, obtain that the results are shown in Table 2.
Comparative example 2
In extraction process, not using ultrasonic wave assisted extraction, other preparation conditions and embodiment 6 are consistent；
To comparative example 2 extract wholefood antioxidant method, Test extraction rate, extraction time, antioxygen property, toxic side effect and
Extraction cost, obtains that the results are shown in Table 2.
Table 2：
Claims (9)
1. it is a kind of from areca leaf extract wholefood antioxidant method, which is characterized in that areca leaf is cleaned, dry it is laggard
Row crushes, and is then mixed with acid, alcohols material and water, adds in progress ultrasound-assisted extraction in extractor and is extracted
Liquid, then extracting solution concentrated, infrared drying, you can wholefood antioxidant is made, preparation is as follows：
（1）Take grow fine, the blade of the betelnut tree of no disease and pests harm, it is miscellaneous that soil, greasy dirt, insect on blade etc. are cleaned with clear water
Matter is placed in drying equipment and removes the partial moisture of surface moisture and inside, then adds in leaf slicing shredder, after crushing
It sieves, the areca leaf particle for taking 20~50 mesh is for use；
（2）Acid, alcohols material and water are mixed, are made into acidity alcohol solution, adds in extractor, then adds in step
（1）The areca leaf particle of gained is impregnated, and uses ultrasonic wave assisted extraction, under the action of acid, Polyphenols object
Matter can generate salt and accelerate the dissolving in alcohols material, and ultrasonic wave can destroy the cell membrane of plant, make intracellular reactive object
Matter is exposed, promotes contacting directly for active material and acidity alcohol solution；Wherein, 1~2 parts by weight of acid, alcohols material 40
~60 parts by weight, 38~59 parts by weight of water；
（3）By step（2）Extracting solution concentrated using thin film evaporator, be then dried using infrared drier,
Until moisture content is less than 5%, you can wholefood antioxidant is made.
2. a kind of method that wholefood antioxidant is extracted from areca leaf according to claim 1, it is characterised in that：Step
（1）The drying equipment turns round one kind in vacuum desiccator, vacuum rake dryer or vacuum drying oven, dry temperature for bicone
It spends for 60~80 DEG C, drying time is 10~15min.
3. a kind of method that wholefood antioxidant is extracted from areca leaf according to claim 1, it is characterised in that：Step
（1）The dried moisture content of betel nut blade is not higher than 10%.
4. a kind of method that wholefood antioxidant is extracted from areca leaf according to claim 1, it is characterised in that：Step
（1）The slicer number of the leaf slicing shredder is 2~4, and the number of crushing knife and flail knife is 8~12, during crushing
Cutterhead revolution is 2300~2500r/min.
5. a kind of method that wholefood antioxidant is extracted from areca leaf according to claim 1, it is characterised in that：Step
（2）The acid be hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, boric acid, hydrobromic acid, hydroiodic acid, hypochlorous acid or hypoiodous acid in extremely
Few one kind；The alcohols material is ethyl alcohol, ethylene glycol, normal propyl alcohol, isopropanol, glycerine, 1,2-, bis- propyl alcohol, n-butanol, isobutyl
At least one of alcohol, sec-butyl alcohol or tert-butyl alcohol.
6. a kind of method that wholefood antioxidant is extracted from areca leaf according to claim 1, it is characterised in that：Step
（2）The extractor is right cone formula multifunctional extracting pot or oblique conic multifunctional extracting pot, and folder is laminated to 0.3~0.5MPa, tank internal pressure
Power is 0.08~0.1MPa, and heating power is 6~10kW, and stirring motor power is 0.2~0.4kW, speed of agitator for 200~
300r/min。
7. a kind of method that wholefood antioxidant is extracted from areca leaf according to claim 1, it is characterised in that：Step
（2）The ultrasonic power of the ultrasonic wave assisted extraction be 500~1000W, frequency be 40~80Hz, aid in soak extraction when
Between be 2~4h.
8. a kind of method that wholefood antioxidant is extracted from areca leaf according to claim 1, it is characterised in that：Step
（3）The thin film evaporator is one in film-rising evaporator, downward film evaporator, scraper-type evaporator or centrifugal evaporator
Kind, material heated time is 0.5~1s.
9. a kind of method that wholefood antioxidant is extracted from areca leaf according to claim 1, it is characterised in that：Step
（3）The infrared drier is one kind in oscillatory type infrared drier or tunnel type infrared ray drying chamber；The infrared ray
In drying process, a length of 200~400nm of infrared wave, power is 10~20kW, and drying time is 30~60min.
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