CN105343186B - A kind of mulberries reactive phenolic compounds and its green method for extraction and purification - Google Patents
A kind of mulberries reactive phenolic compounds and its green method for extraction and purification Download PDFInfo
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- CN105343186B CN105343186B CN201510862706.3A CN201510862706A CN105343186B CN 105343186 B CN105343186 B CN 105343186B CN 201510862706 A CN201510862706 A CN 201510862706A CN 105343186 B CN105343186 B CN 105343186B
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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)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/60—Moraceae (Mulberry family), e.g. breadfruit or fig
- A61K36/605—Morus (mulberry)
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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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
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
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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
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
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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
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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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
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/10—General cosmetic use
Abstract
The invention discloses a kind of mulberries reactive phenolic compounds and its green method for extraction and purification.This method first successively carries out microwave and vapor high-temperature instantaneous enzyme deactivation to fresh mulberries, then carries out Mechanical Crushing, centrifugation layering, the extraction of food grade acidulant ethyl alcohol, is concentrated under reduced pressure, ultrafiltration membrane purification process, obtains biologically active mulberries phenolic compound extracting solution.The present invention uses the organic reagent of low concentration, and realizes broken to mulberries, phenolic compound extraction and purifying in a mild condition, is conducive to the natural character and bioactivity of safeguarding mulberries phenolic compound.Relative to traditional extraction method, the total phenol of method imparting mulberries extract higher concentration of the present invention and total anthocyanidin, and extracting solution has good color, stronger anti-oxidant and inhibition a- glucosidase activity, and foodsafety, it can be used as the safe materials that anti-oxidant and hypoglycemic drug and health care product are developed.Mild condition of the present invention, it is easy to operate, be conducive to the industrialized production of high-activity natural product.
Description
Technical field
The present invention relates to a kind of extractions of mulberries, more particularly to a kind of green extraction purification of mulberries reactive phenolic compounds
Method；Main extractant is made with water more particularly to one kind, the method for the extraction mulberries phenolic compound of highly effective and safe belongs to natural and produces
The extractive technique field of object.
Background technique
Mulberries (Fructus Mori) are a kind of generally acknowledged integration of drinking and medicinal herbs raw materials, contained by Polyphenols, anthocyan etc.
Bioactive natural product is guide's class chemical component that mulberries play healthcare function.Natural products is safe with its, from a wealth of sources, active
The advantages that strong, in current and future drug, food, Cosmetic Manufacture field in occupation of critical positions.But natural products is in former material
Content in material is often lower, is not able to satisfy industrial application demand.Therefore, by natural products component from raw material high efficiency extraction
New method and new process also come into being.The patent of Publication No. CN1969890, CN101406487 and CN101642632 point
It does not disclose and dynamic, plant is extracted using superfreeze and immersing in liquid nitrogen freeze grinding technology, overcritical and subcritical abstraction technology
Active constituent in object and marine prods.Though the technology improves yield, used equipment is expensive, and operating parameter complexity is not
It is easy to control.The Chinese invention patent that publication No. is CN102690320 discloses the extractive technique of active component in tea cake, extracts pure
It needs to isolate and purify extract using organic reagents such as a large amount of ethyl alcohol, ethyl acetate during changing, the use of organic reagent
Not only increase processing cost, is also unfavorable for environmental protection and health.
Membrane separation technique is particularly suitable for point of thermal sensitivity natural products as a kind of non-thermal physical separation purification technique
From purifying.Compared with other separating and purifying technologies, membrane separation and purification technology have the advantage that 1 can realize continuous operation and
Purification process not will lead to the phase transformation for the treatment of fluid；2 treatment processes are not required in addition add other reagents, more environmentally friendly safety；3 separation are pure
Change process carries out at normal temperature, is more advantageous to the protection of the heat-sensitive components such as phenolic compound.
The organic reagents such as extractant such as methanol, ethyl alcohol, acetone, chloroform rely on its higher extraction efficiency, and extract
Middle impurity content is relatively fewer, and is still the primary selection during most of natural product extraction.But with organic reagent
The negative effects such as incidental damage health, Gao Chengben, environmental pollution, reagent waste are also undisputable fact when making extractant.
Make extractant with pure water, though it can effectively avoid negative effect, the extraction efficiency of pure water brought by above-mentioned organic reagent from being lower than
It is extracted with high concentration organic reagent.Further, since the polarity of water is larger, the more impurity that can be introduced in Aqua pure extract liquid, this
A little impurity can make extracting solution be easier to the deterioration such as layering, muddiness occur during storage.
Therefore, the purity and safety of Polyphenols component and extracting solution can maximumlly be discharged by exploring one kind
Property, and the green purification technique for even enhancing its bioactivity is maintained, in the research field and food of natural products, drug
Etc. application fields be all of great significance.
Summary of the invention
Object of the present invention is to solve existing high organic reagent dosage during current natural product extraction, Gao Chengben, set
Standby complicated problem, provides that a kind of operating condition is mild, and equipment is simple, high efficiency extraction and purifying phenolic compound from fresh mulberries
Green method.Gained purification liquid is bright in colour, safe and non-toxic, content of phenolic compounds is high, and has stronger removing peroxide
Free radical ability and the active ability for inhibiting a- glucuroide, can be directly used as food, drug, health care product, cosmetics
It processes raw material.
The present invention also provides the mulberries reactive phenolic compounds that said extracted purification process obtains.
Mulberries fruit cell tissue character is special, the body of vacuole in brittleness and flexibility and cytoplasm with cell wall
Big, the breakable characteristic of product, the type eucaryotic cell structure make mulberries in course of defrosting, active constituent in cell tissue and
Metabolic enzymes are easier to discharge.Existing mulberries processing technology mostly uses in order to avoid the loss of mulberries juice by the mulberry of defrosting
The direct Pasteur of Shen heats enzyme deactivation, and heating time at least maintains 10min.But due to the heat sensitivity of reactive phenolic compounds, in short-term
Heating is more advantageous to the reservation of the active constituent.The present invention to the mulberries not thawed directly utilize microwave it is " intermolecular " heating and
" surface " heat source of vapor is handled, and realizes the effect of instantaneous enzyme deactivation, maximized to safeguard thermal sensitivity phenols chemical combination in mulberries
The content and activity of object.
Inventors have found that during extracting its phenolic component as experimental raw using mulberries, ultrasonic wave add the activity at
Decomposition, the oxidation etc. divided, the present invention only carries out ultrasonic treatment to the residue that the first water of mulberries mentions, and the environment of ultrasound is evaded
To the unfavorable factor of phenolic component, effective measures reduce oxygenolysis of the active constituent in ultrasonic procedure, improve raw material
The stability and extracted amount of middle phenolic compound.
During the prior art natural product extraction the problem of existing high organic reagent dosage, the present invention is using acidification second
Alcoholic solution overcomes that the prior art is generally existing to ask with the low solvent usage amount of 1:3-1:15 (feed liquid quality and volume ratio)
Topic.
The object of the invention is achieved through the following technical solutions:
A kind of green method for extraction and purification of mulberries reactive phenolic compounds, comprising the following steps:
(1) raw material enzyme deactivation: by fresh mulberries successively through microwave deactivating enzyme and water vapour destroy the enzyme treatment；
(2) it is crushed: the mulberries of step (1) enzyme deactivation being mixed with ice water by feed liquid mass volume ratio 1:2-1:9, through colloid mill
Broken, the power of motor for controlling colloid mill is 1.5-2.2Kw, obtains mulberries suspension；
(3) preparation of mulberry fruit polyphenol extracting solution: step (2) resulting suspension is centrifuged under room temperature, is collected respectively
Clear liquid and residue；Supernatant is the first aqueous extract of mulberries polyphenol；
(4) ultrasonic extraction of mulberries slag polyphenol: using kilogram and rise as quality and volume units, by step (3)
Resulting residue is mixed with the acidic ethanol solution that volumetric concentration is 10-25% by feed liquid mass volume ratio 1:3-1:15, is mixed
Object is under the conditions of 25-40 DEG C, ultrasound assisted extraction 0.5-2.5h；The power of the ultrasound is 500w-700w, frequency 30-
50KHz；
(5) preparation of mulberries slag polyphenol extracting solution: ultrasonic extraction liquid is centrifuged under room temperature, supernatant is in 35-50 DEG C of item
Under part, 20-50min is evaporated under reduced pressure, obtains non-alcoholic mulberries slag polyphenol extracting solution；
(6) mulberries extract purifies: by the resulting supernatant of step (3) step and the resulting mulberries slag polyphenol of step (5) step
Extracting solution merges, with 200-500rmin‐1The peristaltic pump of operating is power, which is delivered to 3000-10000 molecule
The hollow fiber ultrafiltration film of interception carries out grading purification processing, collects penetrating fluid, obtains mulberries active polyphenol extracting solution.
To further realize the object of the invention, it is preferable that the microwave power of the microwave deactivating enzyme is 400-700W, and the time is
1-5min；The time of the vapor enzyme deactivation is 1-5min.
Preferably, the ethyl alcohol is food-grade ethanol, and acidic ethanol refers to the food-grade lemon containing 0.1-0.9%
Acid.
Preferably, the Mechanical Crushing is crushed under the conditions of 1.5-2.2Kw through colloid mill；Time is 3-10min.
Preferably, the revolving speed of centrifugation described in step (3) is 3000-8000g, time 10-20min.
Preferably, the revolving speed of centrifugation described in step (5) is 3000-8000g, time 10-20min.
Preferably, the temperature of the ice water is 0-4 DEG C.
A kind of mulberries reactive phenolic compounds, are made by said extracted method, phenol generalization in prepared mulberries extract
Close object (120-400mg GAE/g dw) and anthocyan (60-90mg cyd-3-glu/g dw) concentration be all remarkably higher than by
Conventional method is extracted, and extracting solution lovely luster has both anti-oxidant and inhibition a- glucosidase activity.
Compared with the existing technology, the present invention have following innovative point and the utility model has the advantages that
(1) relative to single microwave heating or vapor destroy the enzyme treatment, microwave and vapor employed in the present invention
Synergistic effect not only obviously inhibits the activity of polyphenol oxidase in mulberry juice, also can preferably realize and contain to total phenol in mulberry juice
The reservation of amount.In the industrial production, a step enzyme deactivation method, such as microwave heating, irradiation, electric field and chemical-agent technique are mostly used,
But from food safety, for the reservation of active component and the ease of production equipment, microwave and vapor synergistic effect will
It is more advantageous to and reaches this purpose, and the enzyme deactivation effect of this synergistic effect is verified in mulberries fruit for the first time.
(2) be commonly used for the direct ultrasonic extraction of raw material, what the present invention only mentioned the first water of mulberries
Residue carries out ultrasonic treatment, and the environment of ultrasound has evaded the unfavorable factor to phenolic component.Method of the present invention effectively reduces
Ultrasonic wave improves the stability and extracted amount of phenolic compound in raw material to the degradation of phenolic component in extracting solution.It should
Kind ultrasound treatment patterns yet there are no all reports.
(3) unique organic reagent used in extracting method of the present invention is acidified foods grade ethyl alcohol, and lower using concentration
(10-25%) extraction conditions are mild, process is environmentally protective, and involved equipment is relatively conventional, and production cost is low, in industrialized day
In right product extraction process, the method for reducing organic reagent usage amount is more with potential applications.
Detailed description of the invention
Fig. 1 is 5 mulberries raw material of comparative example through Electronic Speculum of the mulberries particle under 180 × amplification factor obtained by juicing crusher machine
Scanning figure.
Fig. 2 is 5 mulberries raw material of comparative example in the electricity through mulberries particle obtained by juicing crusher machine, under 500 × amplification factor
Scarnning mirror figure.
Fig. 3 is 4 mulberries raw material of embodiment in the Electronic Speculum through the broken gained mulberries particle of colloid mill under 180 × amplification factor
Scanning figure.
Fig. 4 is 4 mulberries raw material of embodiment in the Electronic Speculum through the broken gained mulberries particle of colloid mill under 500 × amplification factor
Scanning figure.
Specific embodiment
For a better understanding of the invention, the present invention will be further described with reference to the accompanying drawings and examples, but the present invention
Embodiment it is unlimited so.
Related detection method is described as follows in following example:
(1) polyphenol oxidase (PPO) activity
In 0.3g mulberries sample, the 7.5mL reaction reagent (sodium dihydrogen phosphate of 10mmol/L catechol and pH6.0 is added
One disodium hydrogen phosphate buffer), (130-140r/min) 5min is vibrated in water bath with thermostatic control under the conditions of 37 DEG C, will terminate under ice bath environment
Reaction.It is control with reaction reagent, surveys absorbance at 410nm, PPO activity is indicated with OD 410nm.
(2) total phenol content
100 μ L extracting solutions are mixed and added into 100 μ L forint phenol reagents with 400 μ L deionized waters, mix, and stand 6min, then
The Na of 1mL 7% is added2CO3Solution and 800 μ L deionized waters after mixing, are protected from light and stand 90min, detect at 760nm wavelength
As a result its light absorption value indicates (mg using gallic acid as standard control with milligram gallic acid equivalant contained by every gram of dry matter
Gallic acid equivalent/dry weight,mg GAE/gdw)
(3) anthocyanidin content
Sample is diluted 20 times with the buffer solution of pH1.0 and pH4.5, detects and inhales at 510nm and 700nm wavelength
As a result light value indicates (mg cyanidin-3-glucoside/ with the cyanidin of milligram contained by every gram of dry matter-glucoside
g dw)。
(4) peroxy radical absorbability (ORAC) is tested
The phosphate buffer (blank) or sample liquid, Trolox standard liquid for pipetting 20 μ L will be loaded in 96 orifice plate corresponding positions
Plate hatches 10min, then adds 0.96 μM of fluorescence working solution, then 37 DEG C of hatching 20min by 200 holes μ L/, so under 37 DEG C of environment
119mMABAP working solution is added by 20 holes μ L/ afterwards, is read under the conditions of excitation wavelength 485nm, incident wavelength 520nm.ORAC value
(μm olTrolox/gdw) is indicated with the amount that every milliliter of extracting solution is equivalent to micromole Trolox.
(5) a- glucosidase activity inhibits
20 μ L mulberries extracts are mixed with 20 μ La- Glucosidase solutions (0.5u/mL), are placed in 37 DEG C of water-bath 10min,
20 μ L p-nitrophenyl a-d- glucosides are added, 37 DEG C of incubation 20min add 1mL 1mol/L Na2CO3Reaction is terminated, in
Light absorption value is detected at 400nm wavelength, is as a result indicated with the percentage that the enzymatic activity of sample sets accounts for control group enzymatic activity.
(6) color value detects
Each sample 1mL is drawn, the L* of each sample, a*, b* value are read in color difference meter.Wherein L* indicates black and white ,+indicate inclined
It is white ,-indicate partially dark；A* indicates red green ,+indicate partially red ,-indicate partially green；B* indicates champac ,+indicate partially yellow ,-indicate partially blue.
(7) granularity Detection
Using laser particle size detector test granularity, detecting light wave is 0.02-2000 μm, is repeatedly added on a small quantity into detection liquid
Add mulberries residue, start to detect when the signal value of measurement is in 10-20%, each sample is read three times, as a result with particle
Table volume D [4,3] (μm) value indicate.
Embodiment 1
A freezing mulberries are taken, without defrosting, first microwave deactivating enzyme (gas vent is reserved in packaging bag) (600W, 1min), then
Through secondary steam enzyme deactivation (3min).With 4 times of volume ice water mixing mulberries, the precrushing 3min in colloid mill (1.5Kw).Gained is mixed
Liquid centrifugation (8000g, 10min) is closed, is collected supernatant (first Aqueous extracts), it is spare.With 10% food grade acidulant ethanol water
(citric acid containing 0.1%) makees the extractant (by 1:3 solid-liquid ratio) of residue polyphenol, is protected from light ultrasonic treatment (500W, 40KHz)
40min, 25 DEG C of temperature.Ultrasonic extraction liquid is centrifuged (3000g, 10min), supernatant is concentrated under reduced pressure under the conditions of 35 DEG C
20min obtains decompressed concentrate, collects spare.First Aqueous extracts are mixed with decompressed concentrate, it is spare.With 250rmin‐1Fortune
Turn peristaltic pump be power, by the mixed liquor of first Aqueous extracts and decompressed concentrate be delivered to hollow fiber ultrafiltration film (JM-S0522W,
10000MWCO), filter liquor is collected.
Comparative example 1,2
Two parts of freezing mulberries (quality similarly to Example 1) of equivalent are taken, after thawing at room temperature, respectively through microwave deactivating enzyme
Then (500W, 10min) and vapor enzyme deactivation 10min (presses 1:3 solid-liquid ratio, w/v is by mass unit with 10% ethyl alcohol respectively
Kilogram, volume unit is to rise to calculate) mixing, mixture broken 5min in colloid mill (JM-65, Shanghai multi-source Mechanology Inc.),
Gained mixture extracts 40min respectively ultrasonic (500W, 40KHz), then (8000g, 10min) is centrifuged at room temperature, in collection
Clear liquid.The extractant of residue polyphenol is made (by 1:3 with 10% food grade acidulant ethanol water (citric acid containing 0.1%) respectively
Solid-liquid ratio), it is protected from light ultrasonic treatment (500W, 40KHz) 40min, 25 DEG C of temperature.Respectively by ultrasonic extraction liquid centrifugation (3000g,
10min), 20min is concentrated under reduced pressure under the conditions of 35 DEG C in supernatant, obtains decompressed concentrate, collects spare.First water is mentioned respectively
Liquid is mixed with decompressed concentrate, spare.With 250rmin‐1The peristaltic pump of operating is power, respectively by first Aqueous extracts and decompression
The mixed liquor of concentrate is delivered to hollow fiber ultrafiltration film (JM-S0522W, 10000MWCO), collects each filter liquor.
Through detecting, enzyme activity OD value is 0.15 in extracting solution obtained by 1 microwave deactivating enzyme of comparative example, the extracting solution total phenol and total cyanine
Cellulose content is respectively 12.71mg GAE/g dw and 7.47mgcyd-3-glu/g dw；It is extracted obtained by 2 vapor enzyme deactivation of comparative example
Enzyme activity OD value is 0.46 in liquid, the extracting solution total phenol and total anthocyanidin content be respectively 19.69mg GAE/g dw and
5.23mgcyd‐3‐glu/g dw；Enzyme activity OD value is 0.42 in 1 gained extracting solution of embodiment, and extracting solution total phenol and total anthocyanidin contain
Amount is respectively 120.95mg GAE/g dw and 80.62mgcyd-3-glu/g dw.In addition, the brightness of 1 gained extracting solution of embodiment
Value L* and red chrominance value a* is respectively 56.37 and 39.36, which is significantly higher than (the L*=of the single microwave deactivating enzyme of comparative example 1 extraction
16.89, a*=21.46) and the single vapor enzyme deactivation of comparative example 2 extract (L*=14.24, a*=15.39).And embodiment
The 1 extract obtained ability for showing stronger inhibition a- glucosidase activity, inhibiting rate are 62.40% and remove oxygen freedom
The ability (ORAC=5276.20 μm of ol Trolox/gdw) of base, the single microwave deactivating enzyme of corresponding comparative example 1 and comparative example 2 are single
The inhibiting rate of extracting solution obtained by vapor enzyme deactivation is respectively 26.3% and 19.79%, and ORAC value is respectively 362.61 μm of ol
Trolox/gdw and 487.13 μm of ol Trolox/gdw.
Although microwave and vapor can significantly reduce the activity of oxidizing ferment in mulberries, but prolonged high-temperature process, also plus
The speed decomposition of thermal sensitivity phenolic compound causes the concentration of phenolic compound and activity in extracting solution to reduce.The present invention is based on
Morular cell wall is relatively thin, the biggish characteristic of vacuole tissue, which is easy to hot mass transfer effect, also, the present invention is first to freezing shape
Mulberries under state carry out high temperature, short time microwave treatment, keep morular cell tissue instantaneous using microwave energy and uniform avalanche, this is collapsed
The state collapsed increases the contact area of cell tissue and vapor, is conducive to realize high temperature, short time enzyme deactivation.Microwave and vapor are assisted
Enzyme activity on the one hand is reduced with processing, while shortening the time of high-temperature process, and then be effectively retained natural phenolic in mulberries
The bioactivity of compound simultaneously improves enzyme deactivation efficiency.
Embodiment 2 (compared with conventional high concentration organic reagent extraction method)
Take a freezing mulberries without the direct microwave deactivating enzyme that thaws (reserving gas vent in packaging bag) (500W, 2min), then
It through secondary steam enzyme deactivation (3min), is then mixed with the pure water of 2 times of volumes, the mixture is in colloid mill (JM-65, Shanghai multi-source
Mechanology Inc.) in be crushed 3min, gained mulberries suspension be centrifuged (8000g, 10min) at room temperature, collect supernatant (for the first time
Extracting solution).(1:12 solid-liquid ratio, w/v, by matter are pressed with 20% food-grade ethanol aqueous solution (citric acid containing 0.9%) mixing residue
Measuring unit is kilogram that volume unit is to rise to calculate), gained mixture is protected from light ultrasound (500W, 30KHz) 2.5h, and 40 DEG C of temperature.It will
Ultrasonic extraction liquid is centrifuged (3000g, 20min), and supernatant is concentrated under reduced pressure 30min, it is more to obtain non-alcoholic mulberries slag under the conditions of 35 DEG C
Phenol extraction liquid.The first extracting solution of mulberries and mulberries slag ultrasonic extraction liquid are mixed, then by the mixed liquor and conventional method institute
Extracting solution is obtained respectively with 200rmin‐1The peristaltic pump of operating be power, conveying by hollow fiber ultrafiltration film (JM-S0522W,
3000MWCO), filter liquor is collected, the mulberries polyphenol extracting solution of purifying is obtained.
Comparative example 3
A freezing mulberries (quality is same as Example 2) is taken, after thawing at room temperature, (presses 1:3 feed liquid with 85% ethyl alcohol
It is kilogram that volume unit is to rise to calculate by mass unit than, w/v) mixing, mixture is in colloid mill (JM-65, Shanghai multi-source machine
Tool company) in be crushed (1.9Kw) 5min.By the broken gained mixed serum of colloid mill, it is placed in Clothoid type oscillator (Changzhou Australia Hua Yi
Device Co., Ltd) on, under 90rpm/min revolving speed, 2.5h is shaken in 60 DEG C of water-baths, is then centrifuged the concussion liquid at room temperature
(8000g, 10min) filters supernatant through No. 2 qualitative filter papers, and gained filtrate is the mulberries polyphenol extraction that conventional method extracts
Liquid.
Through detecting, routinely total phenol and the content of total anthocyanidin are respectively comparative example 3 in mulberries extract obtained by method
39.73mg GAE/g dw and 10.82mgcyd-3-glu/g dw.Total phenol and total anthocyanidin contains in 2 gained extracting solution of embodiment
Amount is respectively 175.96mg GAE/g dw and 87.67mgcyd-3-glu/g dw.In addition, the brightness of 2 gained extracting solution of embodiment
Value L* and red chrominance value a* is respectively 42.76 and 32.96, the value be significantly higher than the extraction of 3 conventional method of comparative example (L*=19.37,
A*=25.03).And embodiment 2 is extract obtained to show the stronger ability for inhibiting a- glucosidase activity, inhibiting rate
It is 57.46%, the inhibiting rate of corresponding 3 gained extracting solution of comparative example is 26.3%.In addition, 2 gained extracting solution of embodiment
ORAC value is 8496.27 μm of ol Trolox/gdw, and the ORAC value of extracting solution obtained by 3 conventional method of comparative example is 975.27 μm of ol
Trolox/gdw
The present invention combines microwave with vapor, on the one hand realizes and inactivates polyphenol oxidase and other decomposition in a short time
Enzyme, the on the other hand heat treatment have also softened morular cell tissue, have promoted the release of phenolic component intracellular.In conventional method,
The enzyme not being inactivated can decompose phenolic component in extracting solution in normal temperature unfreezing and subsequent impregnation stage, cause its concentration and
Activity reduces.In addition, the supersaturation of solution causes the extracted amount of phenolic compound will not in organic reagent soaking process
Increase with the extension of extraction time.When ultrasonic wave acts on extraction material, cavitation corrosion effect based on ultrasound
(cavitation effect) makes the fracture of the broken even chemical bond of material particles, which promotes those and mulberries base
Matter combines the release of more close phenolic component (insoluble phenols).In addition, the organic reagent of high concentration can lead to non-natural
Existing phenolic compound generation (Manuel Pinelo, AnisArnous and Anne S.Meyer.2007,
Upgrading of grape skins:Significance of plant cell‐wall structural
components and extraction techniques for phenol release.Trends in Food
Science&Technology,17,579‐590).To sum up, method of the present invention is in low concentration organic reagent (10-25%) usage amount
Under the premise of, realize the more excellent extraction to reactive phenolic component in mulberries raw material.
Embodiment 3 (compares) with conventional Ultrasound method
Taking a freezing mulberries is raw material, direct microwave deactivating enzyme (gas vent is reserved in packaging bag) (500W, 4min), then is passed through
Secondary steam enzyme deactivation (1min) is broken in colloid mill (JM-65, Shanghai multi-source Mechanology Inc.) then with 2 times of ice water dilution mixing
Gained slurry mixed liquor is centrifuged (8000g, 20min) by broken 5min, and supernatant collection is spare.By remaining residue and 25% food
Grade acidic ethanol (citric acid containing 0.7%) mix (press 1:15 solid-liquid ratio, w/v, by mass unit for kilogram, volume unit is
Rise and calculate), which is protected from light ultrasound (500W, 30KHz) 2.5h, material temperature in ultrasonic procedure is maintained with the tap water of circulation
Degree is at 28 ± 2 DEG C.Ultrasonic extraction liquid is centrifuged (3000g, 10min), supernatant is concentrated under reduced pressure 30min, obtains under the conditions of 35 DEG C
Non-alcoholic mulberries slag polyphenol extracting solution.Under room temperature, merge supernatant and mulberries slag ultrasonic extraction liquid, by the amalgamation liquid with 290r
min‐1The peristaltic pump of operating is power transmission to hollow fiber ultrafiltration film (JM-S0522W, 3000MWCO), collects the mulberry that filtrate must purify
Shen polyphenol extracting solution.
Comparative example 4
A freezing mulberries (quality is same as Example 3) is taken, after thawing at room temperature, (presses 1:3 feed liquid with 25% ethyl alcohol
It is kilogram that volume unit is to rise to calculate by mass unit than, w/v) mixing, mixture is in colloid mill (JM-65, Shanghai multi-source machine
Tool company) in be crushed (2.0Kw) 5min.The broken gained mulberries mixed serum of colloid mill is placed directly in ultrasonic reactor ultrasonic
(500W, 30KHz) extracts 2.5h.Then the mixture is centrifuged (8000g, 10min) at room temperature, collects supernatant, it will be upper
Clear liquid is filtered through No. 2 qualitative filter papers, and gained filtrate is the mulberries polyphenol leaching liquor that conventional method extracts.
Through detecting, total phenol and the content of total anthocyanidin are respectively 42.69mg in mulberries extract obtained by conventional Ultrasound method
GAE/g dw and 17.57mgcyd-3-glu/g dw.By total phenol in extracting solution obtained by method of the present invention and the content of total anthocyanidin point
It Wei not 261.13mg GAE/g dw and 125.10mgcyd-3-glu/g dw.In addition, by the brightness of extracting solution obtained by method of the present invention
Value L* and red scale value a* is respectively 65.41 and 49.72, which is significantly higher than (L*=25.79, the a*=of conventional method extraction
30.14).And method of the present invention is extract obtained to show the stronger ability for inhibiting a- glucosidase activity, i.e., to the Portugal a-
Polyglycoside inhibition of enzyme activity rate is 70.34%, and the inhibiting rate of extracting solution obtained by corresponding conventional method is 32.2%.Method of the present invention
It is respectively 8724.16 μm of ol Trolox/gdw and 1092.35 μm of ol Trolox/ with extracting solution ORAC value obtained by conventional Ultrasound method
gdw。
Compared with conventional Ultrasound extraction method, the residue that embodiment 3 only mentions the first water of mulberries is ultrasonically treated, and very
The direct ultrasonic extraction of whole materials in rule method.The cavitation corrosion effect (cavitation effect) of ultrasound is although accelerate material
The release of internal active component, so that active component concentration is promoted in Extraction medium, but in liquid environment, ultrasonic wave
Huge energy caused by cavitation corrosion effect can cause water-molecule dissociation, generate a large amount of free radical (such as H, OH, O2And oxygen
Atom), these free radicals cause the oxidative degradation of the phenolic compound in Extraction medium, lead to phenolic compound in extracting solution
Concentration reduces.In addition, the molecule strenuous exercise that ultrasonic wave causes, also accelerates the heating of Extraction medium, high temperature also promotes temperature-sensitive
The degradation of property reactive phenolic compounds, and the ultrasound under light protected environment, effectively reduce the photodissociation of phenolic component in extracting solution.
It is of the present invention to extract twice, ultrasonic treatment only is taken to mulberries pomace, and ultrasonic procedure maintains room temperature state, effectively advises
The factor for making mulberries phenolic compound degrade is kept away.In addition, extracting solution middle-molecular-weihydroxyethyl is greater than 3000 after ultrafiltration membrane purification process
Impurity be excluded, refined solution small molecular phenolic compound is enriched with, and the extracting solution is made to show stronger a- glucose
Glycosides enzyme inhibition activity.
Embodiment 4 (compared with the conventional Ultrasound extraction method of common juicing crusher machine)
Taking a freezing mulberries is raw material, direct microwave deactivating enzyme (gas vent is reserved in packaging bag) (700W, 1min), then is passed through
Secondary steam enzyme deactivation (5min).With the mulberries of 9 times of ice water mixing enzyme deactivations, in colloid mill (JM-65, Shanghai multi-source Mechanology Inc.)
Precrushing 10min.By the broken gained slurry mixed liquor centrifugation (3000g, 10min) of colloid mill, supernatant collection.With 15% food
Grade acidic ethanol aqueous solution (citric acid containing 0.15%) makees the extractant of respective residue polyphenol, and (by 1:4 solid-liquid ratio, m/v is by matter
Measuring unit is kilogram that volume unit is to rise to calculate), which is protected from light ultrasound (500W, 50KHz) 0.5h, and 25 DEG C of temperature.It will surpass
Mulberries residue water mixed liquid after sonication is centrifuged (3000g, 10min), and 20min is concentrated under reduced pressure under the conditions of 50 DEG C in supernatant,
Obtain non-alcoholic mulberries slag polyphenol extracting solution.Under room temperature, respectively by juice extractor and the resulting supernatant of milling treatment of colloid and mulberries slag
Polyphenol extracting solution merges, and with 500rmin‐1The peristaltic pump of operating is power, is respectively passed through the conveying of each amalgamation liquid hollow super
Filter membrane (JM-S0522W, 10000MWCO) collects filter liquor, obtains the mulberries phenols extracting solution that method of the present invention is extracted.
Comparative example 5
A freezing mulberries (quality is identical as embodiment) is taken, after thawing at room temperature, with 15% food grade acidulant ethyl alcohol
Aqueous solution (citric acid containing 0.15%) (press 1:3 solid-liquid ratio, w/v, by mass unit be kilogram, volume unit be rise calculate) mix
It closing, mixture is crushed 10min in juice extractor (JYL-C63V, nine sun), and resulting broken slurry mixed liquor is placed in ultrasonic pond,
It is protected from light ultrasound (500W, 50KHz) 0.5h.Mulberries residue water mixed liquid after ultrasonic treatment is centrifuged (3000g, 10min), supernatant
Liquid is concentrated under reduced pressure 20min, obtains non-alcoholic mulberries slag polyphenol crude extract under the conditions of 50 DEG C.Under room temperature, and with 500rmin‐1
The peristaltic pump of operating is power, by crude extract conveying by hollow fiber ultrafiltration film (JM-S0522W, 10000MWCO), collects filter
Liquid out.
Through detecting, total phenol and the content of total anthocyanidin are respectively 55.53mg in 5 juice extractor of comparative example processing gained extracting solution
GAE/g dw and 14.28mgcyd-3-glu/g dw.Total phenol and the content of total anthocyanidin are respectively in 4 gained extracting solution of embodiment
392.17mg GAE/g dw and 63.28mgcyd-3-glu/g dw.In addition, the brightness value L * of 4 gained extracting solution of embodiment and red
Angle value a* is respectively 70.82 and 55.49, which is significantly higher than (L*=31.18, the a*=of 5 conventional method of comparative example extraction
24.21).And method of the present invention is extract obtained to show the stronger ability for inhibiting a- glucosidase activity, i.e., to the Portugal a-
Polyglycoside inhibition of enzyme activity rate is 76.89%, and the inhibiting rate of extracting solution obtained by corresponding conventional method is 29.43%.In addition, real
The ORAC value for applying 4 gained extracting solution of example is 6742.93 μm of ol Trolox/gdw, the ORAC of extracting solution obtained by 5 conventional method of comparative example
Value is 782.69 μm of ol Trolox/gdw
In food-processing industry, colloid mill is widely used in the emulsification procedure of high grease liquid, and juice extractor is then mainly answered
For the broken of fruits and vegetables class.But inventors have found that colloid mill is equally applicable for the break process of defrosting mulberry fruit and makes mulberries
Granularity reaches micron order (particle table volume D [4,3] value is 319 μm), and the particle of miniaturization increases the mass transfer speed of extraction process
Rate promotes phenolic component release.In addition, finding through detection, mulberries particle table volume D [4, the 3] value for crusher machine of squeezing the juice is 672 μ
M, the granularity are much larger than through milling treatment of colloid, and are found by electron-microscope scanning, and it is residue obtained that juice extractor handles (attached drawing 1,2)
In still retain the complete interface in part, but the mulberries of milling treatment of colloid, particle is more dispersed, and particle surface shows seriously
" incoherent " phenomenon namely milling treatment of colloid (attached drawing 3,4) to the broken more thorough of mulberries raw material.When ultrasonic wave acts on
When broken tiny material, ultrasonic cavitation corrosion effect (cavitation effect) can be given full play to, and particle is cracked
The even fracture of material chemical bond promotes the further release (document) of phenolic component in matrix.The present invention is reducing mulberries
It under the premise of grain granularity and integrality, makes full use of ultrasound to the positive effect of extract, realizes active phenol in gained extracting solution
Content and its activity extract better than conventional juicing crusher machine.Also illustrate simultaneously, colloid mill is in addition to being applied to liquid high in fat
Emulsification procedure other than, can also be applied to the Refinement operation of the berries material such as mulberries.
Claims (8)
1. a kind of green method for extraction and purification of mulberries reactive phenolic compounds, it is characterised in that the following steps are included:
(1) raw material enzyme deactivation: by fresh mulberries successively through microwave deactivating enzyme and water vapour destroy the enzyme treatment；
(2) it is crushed: the mulberries of step (1) enzyme deactivation being mixed with ice water by feed liquid mass volume ratio 1:2-1:9, are galled through colloid
Broken, the power of motor for controlling colloid mill is 1.5-2.2Kw, obtains mulberries suspension；
(3) it the preparation of mulberry fruit polyphenol extracting solution: by step (2) resulting suspension, is centrifuged under room temperature, collects supernatant respectively
Liquid and residue；Supernatant is the first aqueous extract of mulberries polyphenol；
(4) ultrasonic extraction of mulberries slag polyphenol: using kilogram and rise as quality and volume units, will be obtained by step (3)
Residue and volumetric concentration be 10-25% acidic ethanol solution mixed by feed liquid mass volume ratio 1:3-1:15, mixture in
Under the conditions of 25-40 DEG C, ultrasound assisted extraction 0.5-2.5h；The power of the ultrasound is 500w-700w, frequency 30-50KHz；
(5) preparation of mulberries slag polyphenol extracting solution: ultrasonic extraction liquid is centrifuged under room temperature, supernatant under the conditions of 35-50 DEG C,
20-50min is evaporated under reduced pressure, obtains non-alcoholic mulberries slag polyphenol extracting solution；
(6) mulberries extract purifies: the resulting supernatant of step (3) step and the resulting mulberries slag polyphenol of step (5) step are extracted
Liquid merges, with 200-500 rmin-1The peristaltic pump of operating is power, which is delivered to the retention of 3000-10000 molecule
The hollow fiber ultrafiltration film of amount carries out grading purification processing, collects penetrating fluid, obtains mulberries active polyphenol extracting solution.
2. the preparation method of mulberries phenolic compound extracting solution according to claim 1, which is characterized in that the microwave goes out
The microwave power of enzyme is 400-700W, time 1-5min；The time of the vapor enzyme deactivation is 1-5min.
3. the preparation method of mulberries phenolic compound extracting solution according to claim 1, which is characterized in that the ethyl alcohol
For food-grade ethanol, acidic ethanol refers to the food-grade citric acid containing 0.1-0.9%.
4. the preparation method of mulberries phenolic compound extracting solution according to claim 1, which is characterized in that described through glue
Body galls the broken time as 3-10min.
5. the preparation method of mulberries phenolic compound extracting solution according to claim 1, which is characterized in that step (3) institute
The revolving speed for the centrifugation stated is 3000-8000g, time 10-20min.
6. the preparation method of mulberries phenolic compound extracting solution according to claim 1, which is characterized in that step (5) institute
The revolving speed for the centrifugation stated is 3000-8000g, time 10-20min.
7. the preparation method of mulberries phenolic compound extracting solution according to claim 1, which is characterized in that the ice water
Temperature is 0-4 DEG C.
8. a kind of mulberries reactive phenolic compounds, it is characterised in that it is made by any one of the claim 1-7 extracting method,
Reactive phenolic compounds content is 120-400 mg GAE/g dw in the mulberries extract, and anthocyan content is 60-90
Mg cyd-3-glu/g dw, prepared mulberries extract is bright in colour, has anti-oxidant and inhibitsaGlucosidase activity.
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| CN106046848A (en) * | 2016-06-06 | 2016-10-26 | 西昌学院 | Method for extracting and purifying anthocyanin from mulberry pomace |
| CN107410462A (en) * | 2017-04-09 | 2017-12-01 | 湖南易科生物工程有限公司 | A kind of compound method of leaf vegetables antistaling agent |
| CN107080141A (en) * | 2017-04-09 | 2017-08-22 | 湖南易科生物工程有限公司 | A kind of compound method of chopped hot pepper antistaling agent |
| DE202018006387U1 (en) | 2017-06-13 | 2020-03-20 | Mary Kay, Inc. | Cosmetic compositions and their use to tighten the skin |
| CN107536870A (en) * | 2017-09-06 | 2018-01-05 | 哈尔滨商业大学 | A kind of method that mulberries secondary metabolite polyphenol is obtained with biotechnology |
| CN107927784B (en) * | 2017-12-15 | 2021-02-05 | 齐鲁工业大学 | Optimization research of paste preparation process of mulberry extraction pulp |
| CN112218616A (en) | 2018-03-23 | 2021-01-12 | 玫琳凯有限公司 | Topical compositions and methods |
| CN109181354A (en) * | 2018-10-17 | 2019-01-11 | 罗莱生活科技股份有限公司 | A kind of preparation method and its tint applications of mulberries pigment extract |
| CN109452439A (en) * | 2018-12-19 | 2019-03-12 | 广东正品生物科技股份有限公司 | Preserved fruit pickling liquid extraction process of effective component |
| CN111789204A (en) * | 2020-08-27 | 2020-10-20 | 蔡晓明 | Mulberry beverage and preparation method thereof |
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Effective date of registration: 20230825 Address after: Room 205-6, No. 25 Huanshi Avenue South, Nansha District, Guangzhou City, Guangdong Province, 511458 (self-designed Building 1, Research and Development Building A4) Patentee after: Guangdong Pulai Health Food Co.,Ltd. Address before: 510640 No. five, 381 mountain road, Guangzhou, Guangdong, Tianhe District Patentee before: SOUTH CHINA University OF TECHNOLOGY Patentee before: Guangzhou Zhongmei Pulai Health Technology Co.,Ltd. |