CN105343186A - Mulberry active phenolic compound and pollution-free extraction and purification method thereof - Google Patents
Mulberry active phenolic compound and pollution-free extraction and purification method thereof Download PDFInfo
- Publication number
- CN105343186A CN105343186A CN201510862706.3A CN201510862706A CN105343186A CN 105343186 A CN105343186 A CN 105343186A CN 201510862706 A CN201510862706 A CN 201510862706A CN 105343186 A CN105343186 A CN 105343186A
- Authority
- CN
- China
- Prior art keywords
- fructus mori
- extracting solution
- phenolic compound
- extraction
- mulberry
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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)
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Mycology (AREA)
- Engineering & Computer Science (AREA)
- Epidemiology (AREA)
- Microbiology (AREA)
- Botany (AREA)
- Biotechnology (AREA)
- Chemical & Material Sciences (AREA)
- Birds (AREA)
- Alternative & Traditional Medicine (AREA)
- Medical Informatics (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Dermatology (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a mulberry active phenolic compound and a pollution-free extraction and purification method thereof. The method comprises the steps that microwave and vapor high temperature instantaneous enzyme deactivation is carried out on fresh mulberries in sequence, then mechanical crushing, centrifugal layering, food grade acidified alcohol extraction, vacuum concentration and ultrafiltration membrane purification are carried out, and therefore a mulberry phenolic compound extracting solution with the biological activity is obtained. An organic reagent with the low concentration is adopted, mulberry crushing and phenolic compound extraction and purification are achieved under the mild condition, and the natural character and biological activity of the mulberry phenolic compound can be maintained. Compared with a conventional extraction method, the mulberry extracting solution has the higher-concentration total phenol and total anthocyanins, the extraction solution has the good color and luster and high oxidation resistance, alpha-glucosidase enzymatic inhibitory activity and food safety, and the mulberry active phenolic compound can be used as a safety raw material of antioxidant and hypoglycemic drug and health care product development. The conditions are mild, operation is convenient, and industrial production of high-activity natural products is facilitated.
Description
Technical field
The present invention relates to a kind of Fructus Mori to extract, particularly relate to a kind of green method for extraction and purification of Fructus Mori reactive phenolic compounds; Be specifically related to one and make main extractant with water, the method for the extraction Fructus Mori phenolic compound of highly effective and safe, belong to the extractive technique field of natural product.
Background technology
Fructus Mori (FructusMori) are a kind of generally acknowledged integration of edible and medicinal herbs raw materials, and the Polyphenols contained by it, anthocyan isoreactivity natural product are guide's class chemical compositions that Fructus Mori play health care.Natural product with its safety, wide material sources, the active advantage such as strong, in current and following medicine, food, Cosmetic Manufacture field in occupation of critical positions.But the content of natural product in raw material is often lower, can not meet commercial Application demand.Therefore, the new method of natural products component high efficiency extraction from raw material and new technology are also arisen at the historic moment.Publication number is that the patent of CN1969890, CN101406487 and CN101642632 individually discloses and adopts cryotherapy and immersing in liquid nitrogen freeze grinding technology, supercritical and subcritical abstraction technology to extract active component in animal and plant and marine prods.Though this technology improves productive rate, the apparatus expensive used, operational factor complexity is wayward.Publication No. is the extractive technique that the Chinese invention patent of CN102690320 discloses active component in tea cake, need in extraction purification process to use the organic reagents such as a large amount of ethanol, ethyl acetate to carry out separation and purification to extract, the use of organic reagent not only increases processing cost, is also unfavorable for environmental protection and health.
Membrane separation technique, as a kind of non-thermal physical separation purification technique, is particularly useful for the separation and purification of thermal sensitivity natural product.Compared with other separating and purifying technology, membrane separation and purification technology has the following advantages: 1 can realize continued operation and purge process can not cause the phase transformation for the treatment of fluid; 2 processing procedures do not need to add other reagent in addition, more Environmental Safety; 3 separation and purification processes are carried out at normal temperatures, are more conducive to the protection of the heat-sensitive components such as phenolic compound.
The organic reagents such as extractant such as methanol, ethanol, acetone, chloroform rely on its higher extraction efficiency, and in extract, impurity content is relatively less, and remain the primary selection in most of natural product extraction process.But, incidentally when making extractant with organic reagent to impair one's health, high cost, environmental pollution, the negative effect such as reagent waste be also undisputable fact.Make extractant with pure water, though effectively can avoid the negative effect that above-mentioned organic reagent brings, the extraction efficiency of pure water is lower than extracting with high concentration organic reagent.In addition, because the polarity of water is comparatively large, the more impurity can introduced in Aqua pure extract liquid, these impurity can make extracting solution more easily occur the deterioration such as layering, muddiness in storage process.
Therefore, explore one and can discharge Polyphenols component substantially, purity and the safety of extracting solution can be ensured again, and maintain and even strengthen its bioactive green purification technique, the research field of natural product and the application such as food, medicine all significant.
Summary of the invention
The present invention seeks to solve in current natural product extraction process exist high organic reagent consumption, high cost, equipment complexity problem, provide a kind of operating condition gentle, equipment is simple, the green method of high efficiency extraction and purification of phenol compounds from fresh Fructus Mori.Gained purification liquid lovely luster, safety non-toxic, content of phenolic compounds are high, and there is stronger removing peroxy radical ability and suppress a ?the ability of activity of glucosidase, directly can be used as food, medicine, health product, the processing raw material of cosmetics.
The Fructus Mori reactive phenolic compounds that the present invention also provides said extracted purification process to obtain.
Fructus Mori fruit cell tissue character is special, there is large, the breakable characteristic of volume of vacuole in the fragility of cell wall and flexibility and Cytoplasm, the type cellularity makes Fructus Mori in course of defrosting, and the active component in its cell tissue and metabolic enzymes are easier to release.Existing Fructus Mori process technology is in order to avoid the loss of Fructus Mori juice, and direct for the Fructus Mori thawed Pasteur is heated enzyme denaturing by adopt more, and heat time heating time at least maintains 10min.But due to the heat sensitivity of reactive phenolic compounds, Short Time Heating is more conducive to the reservation of this active component.The present invention directly utilizes " intermolecular " heating of microwave and " surface " thermal source process of steam to the Fructus Mori do not thawed, and achieves the effect of instantaneous enzyme denaturing, maximized content and the activity safeguarding thermal sensitivity phenolic compound in Fructus Mori.
Inventor finds, be that experimental raw is extracted in the process of its phenolic component with Fructus Mori, ultrasound wave adds the decomposition, oxidation etc. of this active component, the present invention only carries out supersound process to the residue of the first water extraction of Fructus Mori, and ultrasonic environment has evaded the unfavorable factor to phenolic component, effective measures reduce the oxidation Decomposition of active component in ultrasonic procedure, improve stability and the extracted amount of phenolic compound in raw material.
The problem of the high organic reagent consumption existed in prior art natural product extraction process, the present invention adopts acidic ethanol solution, with 1:3 ?the low solvent use amount of 1:15 (feed liquid quality and volume ratio), overcome the ubiquitous problem of prior art.
The object of the invention is achieved through the following technical solutions:
A green method for extraction and purification for Fructus Mori reactive phenolic compounds, comprises the following steps:
(1) raw material enzyme denaturing: through microwave deactivating enzyme and the process of water vapour enzyme denaturing after fresh Fructus Mori are first;
(2) broken: by the Fructus Mori of step (1) enzyme denaturing and frozen water by feed liquid mass volume ratio 1:2 ?1:9 mix, through colloid mill fragmentation, the power of motor of control colloid mill be 1.5 ?2.2Kw, obtain Fructus Mori suspension;
(3) preparation of mulberry fruit polyphenol extracting solution: by the suspension of step (2) gained, centrifugal under room temperature, collects supernatant and residue respectively; Supernatant is the first aqueous extract of Fructus Mori polyphenol;
(4) supersound extraction of Fructus Mori slag polyphenol: using kilogram and rise as quality and volume units, by the residue of step (3) gained and volumetric concentration be 10 ?25% acidic ethanol solution by feed liquid mass volume ratio 1:3 ?1:15 mix, mixture in 25 ?under 40 DEG C of conditions, ultrasound assisted extraction 0.5 ?2.5h; Described ultrasonic power be 500w ?700w, frequency be 30 ?50KHz;
(5) preparation of Fructus Mori slag polyphenol extracting solution: supersound extraction liquid is centrifugal under room temperature, supernatant in 35 ?under 50 DEG C of conditions, reduction vaporization 20 ?50min, obtain the Fructus Mori slag polyphenol extracting solution without alcohol;
(6) Fructus Mori extracting solution purification: the Fructus Mori slag polyphenol extracting solution of the supernatant of step (3) step gained and step (5) step gained is merged, with 200 ?500rmin
?1the peristaltic pump of running is power, this amalgamation liquid is delivered to 3000 ?the hollow fiber ultrafiltration film of 10000 molecular retention amounts, carry out grading purification process, collect penetrating fluid, obtain Fructus Mori active polyphenol extracting solution.
For realizing the object of the invention further, preferably, the microwave power of described microwave deactivating enzyme is 400-700W, and the time is 1-5min; The time of described steam enzyme denaturing is 1-5min.
Preferably, described ethanol is food-grade ethanol, and acidic ethanol refers to the food stage citric acid containing 0.1-0.9%.
Preferably, described Mechanical Crushing is through colloid mill, broken under 1.5-2.2Kw condition; Time is 3-10min.
Preferably, the centrifugal rotating speed described in step (3) is 3000-8000g, and the time is 10-20min.
Preferably, the centrifugal rotating speed described in step (5) is 3000-8000g, and the time is 10-20min.
Preferably, the temperature of described frozen water is 0-4 DEG C.
A kind of Fructus Mori reactive phenolic compounds, obtained by said extracted method, phenolic compound in prepared Fructus Mori extracting solution (120 ?400mgGAE/gdw) and anthocyan (60 ?90mgcyd ?3 ?glu/gdw) concentration be all significantly higher than that method routinely extracts, and extracting solution lovely luster have concurrently antioxidation and suppression a ?glucosidase activity.
Relative to prior art, the present invention has following innovative point and beneficial effect:
(1) relative to single microwave heating or the process of steam enzyme denaturing, the microwave adopted in the present invention and steam synergism, not only obviously suppress the activity of polyphenol oxidase in mulberry juice, also can realize the reservation to total phenol content in mulberry juice preferably.In the industrial production, many employing one step enzyme denaturing methods, as microwave heating, irradiation, electric field and chemical-agent technique etc., but from food safety, the reservation of active component and the ease of production equipment, microwave and steam synergism will more be conducive to reaching this purpose, and this synergistic enzyme denaturing effect is verified first in Fructus Mori fruit.
(2) with generally use at present by direct for raw material ultrasonic extraction, the present invention only carries out supersound process to the residue of the first water extraction of Fructus Mori, and ultrasonic environment has evaded the unfavorable factor to phenolic component.Method of the present invention effectively reduces the Degradation of ultrasound wave to phenolic component in extracting solution, improves stability and the extracted amount of phenolic compound in raw material.This kind of ultrasound treatment patterns yet there are no all reports.
(3) unique organic reagent that extracting method of the present invention is used is acidified foods level ethanol, and working concentration lower (10 ?25%) extraction conditions is gentle, process environmental protection, involved equipment is comparatively common, production cost is low, in industrialized natural product extraction process, the method reducing organic reagent use amount is more with potential applications.
Accompanying drawing explanation
Fig. 1 is comparative example 5 Fructus Mori raw material through the electron-microscope scanning figure of the broken gained Fructus Mori granule of juice extractor under 180 × amplification.
Fig. 2 is comparative example 5 Fructus Mori raw material through juice extractor broken gained Fructus Mori granule, the electron-microscope scanning figure under 500 × amplification.
Fig. 3 is embodiment 4 Fructus Mori raw material through the electron-microscope scanning figure of the broken gained Fructus Mori granule of colloid mill under 180 × amplification.
Fig. 4 is embodiment 4 Fructus Mori raw material through the electron-microscope scanning figure of the broken gained Fructus Mori granule of colloid mill under 500 × amplification.
Detailed description of the invention
For understanding the present invention better, below in conjunction with drawings and Examples, the present invention will be further described, but embodiments of the present invention are not limit so.
In embodiment, related detection method is described as follows below:
(1) polyphenol oxidase (PPO) is active
In 0.3g Fructus Mori sample, add 7.5mL reaction reagent (the sodium dihydrogen phosphate one sodium hydrogen phosphate buffer of 10mmol/L catechol and pH6.0), water bath with thermostatic control vibration (130 ?140r/min) 5min under 37 DEG C of conditions, by cessation reaction under ice bath environment.Take reaction reagent as contrast, under 410nm, survey absorbance, represent that PPO is active with OD410nm.
(2) total phenol content
100 μ L extracting solution, mix with 400 μ L deionized waters and add 100 μ L forint phenol reagents, mixing, leave standstill 6min, then add the Na of 1mL7%
2cO
3solution and 800 μ L deionized waters, after mixing, lucifuge leaves standstill 90min, in 760nm wavelength, its light absorption value is detected at place, take gallic acid as standard control, result represents (mgGallicacidequivalent/dryweight, mgGAE/gdw) with milligram gallic acid equivalant contained by every gram of dry
(3) anthocyanidin content
With the buffer solution of pH1.0 and pH4.5 by diluted sample 20 times, detect light absorption value respectively at 510nm and 700nm wavelength place, result with milligram corn flower Se Su contained by every gram of dry ?glucoside represent (mgcyanidin ?3 ?glucoside/gdw).
(4) peroxy radical absorbability (ORAC) experiment
Pipette the phosphate buffer (blank) of 20 μ L or sample liquid, Trolox marks liquid in 96 orifice plate correspondence positions, model will be added under 37 DEG C of environment, hatching 10min, then 0.96 μM of fluorescence working solution is added by 200 μ L/ holes, 37 DEG C of hatching 20min again, then 119mMABAP working solution is added by 20 μ L/ holes, in excitation wavelength 485nm, reading under incident wavelength 520nm condition.The amount that ORAC value is equivalent to micromole Trolox with every milliliter of extracting solution represents (μm olTrolox/gdw).
(5) a ?glucosidase activity suppress
20 μ L Fructus Mori extracting solution and 20 μ La ?Glucosidase solution (0.5u/mL) mix, be placed in 37 DEG C of water-bath 10min, add 20 μ L p-nitrophenyl a ?d ?glucoside, hatch 20min, add 1mL1mol/LNa for 37 DEG C
2cO
3cessation reaction, detect light absorption value in 400nm wavelength place, the percentage ratio that result accounts for matched group enzymatic activity with the enzymatic activity of sample sets represents.
(6) color value detects
Draw each sample 1mL, in color difference meter, read the L* of each sample, a*, b* value.Wherein L* represents black and white ,+represent inclined Bai ， ?represent partially dark; A* represents red green ,+represent inclined Hong ， ?represent partially green; B* represents champac ,+represent inclined Huang ， ?represent partially blue.
(7) granularity Detection
Laser particle size detector is used to detect granularity, detect light wave be 0.02 ?2000 μm, a small amount of repeatedly interpolation Fructus Mori residue in detection liquid, until measure signal value be in 10 ?20% time start detect, each sample reads three times, result represents with table volume D [4,3] (μm) value of granule.
Embodiment 1
Get a freezing Fructus Mori, without thawing, first microwave deactivating enzyme (in packaging bag reserved steam vent) (600W, 1min), then through secondary steam enzyme denaturing (3min).With 4 times of volume frozen water mixing Fructus Mori, precrushing 3min in colloid mill (1.5Kw).Gained mixed liquor centrifugal (8000g, 10min), collects supernatant (first Aqueous extracts), for subsequent use.The extractant (by 1:3 solid-liquid ratio) of residue polyphenol is made, lucifuge supersound process (500W, 40KHz) 40min, temperature 25 DEG C with 10% food grade acidulant ethanol water (citric acid containing 0.1%).By centrifugal for supersound extraction liquid (3000g, 10min), supernatant is under 35 DEG C of conditions, and concentrating under reduced pressure 20min, obtains decompressed concentrate, collects for subsequent use.First Aqueous extracts is mixed with decompressed concentrate, for subsequent use.With 250rmin
?1the peristaltic pump of running is power, the mixed liquor of first Aqueous extracts and decompressed concentrate is delivered to hollow fiber ultrafiltration film (JM ?S0522W, 10000MWCO), collection filter liquor.
Comparative example 1,2
Get two parts of freezing Fructus Mori (similarly to Example 1 quality) of equivalent, after thawed at room temperature, respectively through microwave deactivating enzyme (500W, 10min) with steam enzyme denaturing 10min, then respectively with 10% ethanol (by 1:3 solid-liquid ratio, w/v, by mass unit be kilogram that volume unit calculates for rising) mixing, mixture in colloid mill (JM ?65, Shanghai multi-source Mechanology Inc.) in broken 5min, gained mixture respectively ultrasonic (500W, 40KHz) extracts 40min, then centrifugal (8000g under room temperature, 10min), supernatant is collected.The extractant (by 1:3 solid-liquid ratio) of residue polyphenol is made respectively, lucifuge supersound process (500W, 40KHz) 40min, temperature 25 DEG C with 10% food grade acidulant ethanol water (citric acid containing 0.1%).Respectively by centrifugal for supersound extraction liquid (3000g, 10min), supernatant is under 35 DEG C of conditions, and concentrating under reduced pressure 20min, obtains decompressed concentrate, collects for subsequent use.Respectively first Aqueous extracts is mixed with decompressed concentrate, for subsequent use.With 250rmin
?1the peristaltic pump of running is power, respectively the mixed liquor of first Aqueous extracts and decompressed concentrate is delivered to hollow fiber ultrafiltration film (JM ?S0522W, 10000MWCO), collects each filter liquor.
After testing, in comparative example 1 microwave deactivating enzyme gained extracting solution, live OD value of enzyme is 0.15, this extracting solution total phenols and total anthocyanidin content be respectively 12.71mgGAE/gdw and 7.47mgcyd ?3 ?glu/gdw; In comparative example 2 steam enzyme denaturing gained extracting solution, live OD value of enzyme is 0.46, this extracting solution total phenols and total anthocyanidin content be respectively 19.69mgGAE/gdw and 5.23mgcyd ?3 ?glu/gdw; In embodiment 1 gained extracting solution, live OD value of enzyme is 0.42, extracting solution total phenols and total anthocyanidin content be respectively 120.95mgGAE/gdw and 80.62mgcyd ?3 ?glu/gdw.In addition, brightness value L * and the red chrominance value a* of embodiment 1 gained extracting solution are respectively 56.37 and 39.36, this value is significantly higher than the (L*=16.89 that the single microwave deactivating enzyme of comparative example 1 extracts, and the single steam enzyme denaturing of comparative example 2 (L*=14.24, the a*=15.39) that extract a*=21.46).And embodiment 1 is extract obtained show stronger suppression a ?the ability of glucosidase activity, suppression ratio is the ability (ORAC=5276.20 μm of olTrolox/gdw) of 62.40% and scavenging activated oxygen, the corresponding single microwave deactivating enzyme of comparative example 1 and the suppression ratio of comparative example 2 single steam enzyme denaturing gained extracting solution be respectively 26.3% and 19.79%, ORAC value be respectively 362.61 μm of olTrolox/gdw and 487.13 μm olTrolox/gdw.
Although microwave and steam significantly can reduce oxidasic activity in Fructus Mori, high-temperature process, also accelerates the decomposition of thermal sensitivity phenolic compound for a long time, causes the concentration of phenolic compound in extracting solution and active reduction.The present invention is based on that morular cell wall is thinner, vacuole organizes larger characteristic, this characteristic is easy to hot mass transfer effect, and, the present invention first carries out high temperature, short time microwave treatment to the Fructus Mori under freezing state, microwave energy is utilized to make morular cell organize instantaneous and uniform avalanche, the state of this avalanche increases the contact area of cell tissue and steam, is beneficial to and realizes high temperature, short time enzyme denaturing.Microwave and steam associated treatment reduce enzyme on the one hand and live, and shorten the time of high-temperature process simultaneously, and then effectively remain the biological activity of natural phenolic compound in Fructus Mori and improve enzyme denaturing efficiency.
Embodiment 2 (compared with conventional high concentration organic reagent extraction method)
Get a freezing Fructus Mori without the direct microwave deactivating enzyme that thaws (in packaging bag reserved steam vent) (500W, 2min), again through secondary steam enzyme denaturing (3min), then mix with the pure water of 2 times of volumes, this mixture is broken 3min in colloid mill (JM ?65, Shanghai multi-source Mechanology Inc.), by gained Fructus Mori suspension centrifugal (8000g under room temperature, 10min), supernatant (first extracting solution) is collected.With 20% food-grade ethanol aqueous solution (citric acid containing 0.9%) mixing residue, (by 1:12 solid-liquid ratio, w/v, by mass unit is kilogram, volume unit calculates for rising), gained mixture lucifuge ultrasonic (500W, 30KHz) 2.5h, temperature 40 DEG C.By centrifugal for supersound extraction liquid (3000g, 20min), supernatant is under 35 DEG C of conditions, and concentrating under reduced pressure 30min, obtains the Fructus Mori slag polyphenol extracting solution without alcohol.By the first extracting solution of Fructus Mori and the mixing of Fructus Mori slag supersound extraction liquid, then by this mixed liquor and conventional method gained extracting solution respectively with 200rmin
?1the peristaltic pump of running is power, is conducted through hollow fiber ultrafiltration film (JM ?S0522W, 3000MWCO), collects filter liquor, obtains the Fructus Mori polyphenol extracting solution of purification.
Comparative example 3
Get a freezing Fructus Mori (quality is identical with embodiment 2), after thawed at room temperature, with 85% ethanol (by 1:3 solid-liquid ratio, w/v, by mass unit be kilogram, volume unit calculates for rising) mixing, mixture is broken (1.9Kw) 5min in colloid mill (JM ?65, Shanghai multi-source Mechanology Inc.).By broken for colloid mill gained mixed serum, be placed on Clothoid type agitator (Changzhou Ao Hua Instrument Ltd.), under 90rpm/min rotating speed, 60 DEG C of water-bath concussion 2.5h, then by this concussion liquid centrifugal (8000g under room temperature, 10min), filtered by supernatant through No. 2 qualitative filter papers, gained filtrate is the Fructus Mori polyphenol lixiviating solution that conventional method extracts.
After testing, comparative example 3 routinely in method gained Fructus Mori extracting solution the content of total phenols and total anthocyanidin be respectively 39.73mgGAE/gdw and 10.82mgcyd ?3 ?glu/gdw.In embodiment 2 gained extracting solution the content of total phenols and total anthocyanidin be respectively 175.96mgGAE/gdw and 87.67mgcyd ?3 ?glu/gdw.In addition, brightness value L * and the red chrominance value a* of embodiment 2 gained extracting solution are respectively 42.76 and 32.96, and this value is significantly higher than (L*=19.37, the a*=25.03) that comparative example 3 conventional method extracts.And embodiment 2 is extract obtained show stronger suppression a ?the ability of glucosidase activity, suppression ratio is 57.46%, and the suppression ratio of corresponding comparative example 3 gained extracting solution is 26.3%.In addition, the ORAC value of embodiment 2 gained extracting solution is 8496.27 μm of olTrolox/gdw, and the ORAC value of comparative example 3 conventional method gained extracting solution is 975.27 μm of olTrolox/gdw
Microwave is combined with steam by the present invention, realizes deactivation polyphenol oxidase and other catabolic enzyme classes at short notice on the one hand, and this heat treatment has also softened morular cell tissue on the other hand, facilitates the release of phenolic component in born of the same parents.In conventional method, the enzyme be not inactivated all can decompose phenolic component in extracting solution in normal temperature unfreezing and follow-up impregnation stage, causes its concentration and active reduction.In addition, in organic reagent immersion process, the supersaturation of solution causes the extracted amount of phenolic compound can not increase with the prolongation of extraction time.When ul-trasonic irradiation is in lixiviate material, make the fracture of the broken even chemical bond of material particles based on hyperacoustic cavitation corrosion effect (cavitationeffect), this phenomenon facilitates those are combined phenolic component (insoluble phenols) comparatively closely release with Fructus Mori substrate.In addition, generation (the ManuelPinelo of the phenolic compound that the organic reagent of high concentration can cause non-natural to exist, AnisArnousandAnneS.Meyer.2007, Upgradingofgrapeskins:Significanceofplantcell ?wallstructuralcomponentsandextractiontechniquesforphenol release.TrendsinFoodScience & Technology, 17,579 ?590).To sum up, method of the present invention, under the prerequisite of low concentration organic reagent (10 ?25%) use amount, achieves the more excellent extraction to reactive phenolic component in Fructus Mori raw material.
Embodiment 3 (contrasting with conventional Ultrasound method)
Getting a freezing Fructus Mori is raw material, direct microwave deactivating enzyme (in packaging bag reserved steam vent) (500W, 4min), then through secondary steam enzyme denaturing (1min), then with 2 times of frozen water dilution mixture, in colloid mill (JM ?65, Shanghai multi-source Mechanology Inc.) in broken 5min, by gained slag slurry mixed liquor centrifugal (8000g, 20min), supernatant collection, for subsequent use.Remaining residue is mixed (by 1:15 solid-liquid ratio with 25% food grade acidulant ethanol (citric acid containing 0.7%), w/v, by mass unit be kilogram, volume unit calculates for rising), by the ultrasonic (500W of this mixture lucifuge, 30KHz) 2.5h, with temperature of charge in the tap water circulated maintenance ultrasonic procedure at 28 ± 2 DEG C.By centrifugal for supersound extraction liquid (3000g, 10min), supernatant is under 35 DEG C of conditions, and concentrating under reduced pressure 30min, obtains the Fructus Mori slag polyphenol extracting solution without alcohol.Under room temperature, merge supernatant and Fructus Mori slag supersound extraction liquid, by this amalgamation liquid with 290rmin
?1the peristaltic pump of running is that power is delivered to hollow fiber ultrafiltration film (JM ?S0522W, 3000MWCO), collects the Fructus Mori polyphenol extracting solution that filtrate obtains purification.
Comparative example 4
Get a freezing Fructus Mori (quality is identical with embodiment 3), after thawed at room temperature, with 25% ethanol (by 1:3 solid-liquid ratio, w/v, by mass unit be kilogram, volume unit calculates for rising) mixing, mixture is broken (2.0Kw) 5min in colloid mill (JM ?65, Shanghai multi-source Mechanology Inc.).Colloid mill broken gained Fructus Mori mixed serum is directly placed in ultrasonic reactor ultrasonic (500W, 30KHz) and extracts 2.5h.Then by this mixture centrifugal (8000g, 10min) under room temperature, collect supernatant, filtered by supernatant through No. 2 qualitative filter papers, gained filtrate is the Fructus Mori polyphenol lixiviating solution that conventional method extracts.
After testing, in conventional Ultrasound method gained Fructus Mori extracting solution the content of total phenols and total anthocyanidin be respectively 42.69mgGAE/gdw and 17.57mgcyd ?3 ?glu/gdw.By the content of total phenols and total anthocyanidin in method gained extracting solution of the present invention be respectively 261.13mgGAE/gdw and 125.10mgcyd ?3 ?glu/gdw.In addition, be respectively 65.41 and 49.72 by the brightness value L * of method gained extracting solution of the present invention and red scale value a*, this value is significantly higher than (L*=25.79, the a*=30.14) that conventional method extracts.And method of the present invention is extract obtained show stronger suppression a ?the ability of glucosidase activity, namely to a ?glucosidase activity suppression ratio be 70.34%, the suppression ratio of corresponding conventional method gained extracting solution is 32.2%.Method of the present invention and conventional Ultrasound method gained extracting solution ORAC value are respectively 8724.16 μm of olTrolox/gdw and 1092.35 μm olTrolox/gdw.
Compared with conventional Ultrasound extraction method, embodiment 3 only carries out supersound process to the residue of the first water extraction of Fructus Mori, but not the direct supersound extraction of whole materials in conventional method.Ultrasonic cavitation corrosion effect (cavitationeffect) is although accelerate the release of internal batch active component, active component concentration in Extraction medium is promoted, but in liquid environment, the huge energy that hyperacoustic cavitation corrosion effect produces can cause water-molecule dissociation, produce a large amount of free radicals (as H, OH, O
2and oxygen atom), these free radicals cause the oxidative degradation of the phenolic compound in Extraction medium, cause the concentration of phenolic compound in extracting solution to reduce.In addition, the molecule strenuous exercise that ultrasound wave causes, also accelerate the intensification of Extraction medium, high temperature also promotes the degraded of Heat sensitive active phenolic compound, and ultrasonic under light protected environment, effectively reduce the photodissociation of phenolic component in extracting solution.Twice lixiviate of the present invention, only takes supersound process to Fructus Mori marc, and ultrasonic procedure maintains room temperature state, has effectively evaded the factor that Fructus Mori phenolic compound is degraded.In addition, after ultrafilter membrane purification process, the impurity that extracting solution middle-molecular-weihydroxyethyl is greater than 3000 is excluded, and refined solution small molecular phenolic compound is able to enrichment, make this extracting solution present stronger a ?glucosidase inhibitory active.
Embodiment 4 (compared with the conventional Ultrasound extraction method of conventional juice extractor fragmentation)
Getting a freezing Fructus Mori is raw material, direct microwave deactivating enzyme (in packaging bag reserved steam vent) (700W, 1min), then through secondary steam enzyme denaturing (5min).With the Fructus Mori of 9 times of frozen water mixing enzyme denaturing, precrushing 10min in colloid mill (JM ?65, Shanghai multi-source Mechanology Inc.).By broken for colloid mill gained slag slurry mixed liquor centrifugal (3000g, 10min), supernatant collection.The extractant of respective residue polyphenol is made (by 1:4 solid-liquid ratio with 15% food grade acidulant ethanol water (citric acid containing 0.15%), m/v by mass unit is kilogram, volume unit calculates for rising), ultrasonic (the 500W of this mixture lucifuge, 50KHz) 0.5h, temperature 25 DEG C.By the Fructus Mori residue water mixed liquid centrifugal (3000g, 10min) after supersound process, supernatant is under 50 DEG C of conditions, and concentrating under reduced pressure 20min, obtains the Fructus Mori slag polyphenol extracting solution without alcohol.Under room temperature, respectively the supernatant of juice extractor and milling treatment of colloid gained and Fructus Mori slag polyphenol extracting solution are merged, and with 500rmin
?1the peristaltic pump of running is power, respectively each amalgamation liquid is conducted through hollow fiber ultrafiltration film (JM ?S0522W, 10000MWCO), collects filter liquor, obtains the Fructus Mori phenols extracting solution that method of the present invention is extracted.
Comparative example 5
Get a freezing Fructus Mori (quality is identical with embodiment), after thawed at room temperature, (by 1:3 solid-liquid ratio, w/v, by mass unit is kilogram with 15% food grade acidulant ethanol water (citric acid containing 0.15%), volume unit calculates for rising) mixing, mixture is broken 10min in juice extractor (JYL ?C63V, nine sun), and the broken grinding residue-pulp mixed liquor of gained is placed in ultrasonic pond, lucifuge ultrasonic (500W, 50KHz) 0.5h.By the Fructus Mori residue water mixed liquid centrifugal (3000g, 10min) after supersound process, supernatant is under 50 DEG C of conditions, and concentrating under reduced pressure 20min, obtains the Fructus Mori slag polyphenol crude extract without alcohol.Under room temperature, and with 500rmin
?1the peristaltic pump of running is power, this crude extract is conducted through hollow fiber ultrafiltration film (JM ?S0522W, 10000MWCO), collects filter liquor.
After testing, in comparative example 5 juice extractor process gained extracting solution the content of total phenols and total anthocyanidin be respectively 55.53mgGAE/gdw and 14.28mgcyd ?3 ?glu/gdw.In embodiment 4 gained extracting solution the content of total phenols and total anthocyanidin be respectively 392.17mgGAE/gdw and 63.28mgcyd ?3 ?glu/gdw.In addition, brightness value L * and the red scale value a* of embodiment 4 gained extracting solution are respectively 70.82 and 55.49, and this value is significantly higher than (L*=31.18, the a*=24.21) that comparative example 5 conventional method extracts.And method of the present invention is extract obtained show stronger suppression a ?the ability of glucosidase activity, namely to a ?glucosidase activity suppression ratio be 76.89%, the suppression ratio of corresponding conventional method gained extracting solution is 29.43%.In addition, the ORAC value of embodiment 4 gained extracting solution is 6742.93 μm of olTrolox/gdw, and the ORAC value of comparative example 5 conventional method gained extracting solution is 782.69 μm of olTrolox/gdw
At food-processing industry, colloid mill is widely used in the emulsification procedure of high oils and fats liquid, and juice extractor is then mainly used in the fragmentation of fruit and vegerable class.But inventor finds, colloid mill also can be applicable to thaw mulberry fruit break process and make the granularity of Fructus Mori reach micron order (granule table volume D [4,3] value is 319 μm), the granule of miniaturization increases the mass transfer rate of leaching process, promotes phenolic component release.In addition, find after testing, the Fructus Mori granule table volume D [4 of juice extractor fragmentation, 3] value is 672 μm, this granularity is much larger than through milling treatment of colloid, and found by electron-microscope scanning, juice extractor process (accompanying drawing 1,2) interface that in residue obtained, still reserve part is complete, but the Fructus Mori of milling treatment of colloid, its granule comparatively disperses, and particle surface presents serious " incoherent " phenomenon, also namely milling treatment of colloid (accompanying drawing 3, the 4) fragmentation to Fructus Mori raw material is more thorough.When ul-trasonic irradiation is when the tiny material of fragmentation, ultrasonic cavitation corrosion effect (cavitationeffect) can be given full play to, make granule the cracking even fracture of material chemical bond, promote the further release (document) of phenolic component in substrate.The present invention, under the prerequisite reducing Fructus Mori grain graininess and integrity, makes full use of the ultrasonic positive role to extract, realizes the content of active phenol in gained extracting solution and activity thereof and is better than that the fragmentation of conventional juice extractor extracts.Also illustrate, colloid mill, except being applied to the emulsification procedure of high fat liquid, also can be applied to the Refinement operation of the berries materials such as Fructus Mori simultaneously.
Claims (8)
1. a green method for extraction and purification for Fructus Mori reactive phenolic compounds, is characterized in that comprising the following steps:
(1) raw material enzyme denaturing: through microwave deactivating enzyme and the process of water vapour enzyme denaturing after fresh Fructus Mori are first;
(2) broken: by the Fructus Mori of step (1) enzyme denaturing and frozen water by feed liquid mass volume ratio 1:2 ?1:9 mix, through colloid mill fragmentation, the power of motor of control colloid mill be 1.5 ?2.2Kw, obtain Fructus Mori suspension;
(3) preparation of mulberry fruit polyphenol extracting solution: by the suspension of step (2) gained, centrifugal under room temperature, collects supernatant and residue respectively; Supernatant is the first aqueous extract of Fructus Mori polyphenol;
(4) supersound extraction of Fructus Mori slag polyphenol: using kilogram and rise as quality and volume units, by the residue of step (3) gained and volumetric concentration be 10 ?25% acidic ethanol solution by feed liquid mass volume ratio 1:3 ?1:15 mix, mixture in 25 ?under 40 DEG C of conditions, ultrasound assisted extraction 0.5 ?2.5h; Described ultrasonic power be 500w ?700w, frequency be 30 ?50KHz;
(5) preparation of Fructus Mori slag polyphenol extracting solution: supersound extraction liquid is centrifugal under room temperature, supernatant in 35 ?under 50 DEG C of conditions, reduction vaporization 20 ?50min, obtain the Fructus Mori slag polyphenol extracting solution without alcohol;
(6) Fructus Mori extracting solution purification: the Fructus Mori slag polyphenol extracting solution of the supernatant of step (3) step gained and step (5) step gained is merged, with 200 ?500rmin
?1the peristaltic pump of running is power, this amalgamation liquid is delivered to 3000 ?the hollow fiber ultrafiltration film of 10000 molecular retention amounts, carry out grading purification process, collect penetrating fluid, obtain Fructus Mori active polyphenol extracting solution.
2. the preparation method of Fructus Mori phenolic compound extracting solution according to claim 1, is characterized in that, the microwave power of described microwave deactivating enzyme is 400-700W, and the time is 1-5min; The time of described steam enzyme denaturing is 1-5min.
3. the preparation method of Fructus Mori phenolic compound extracting solution according to claim 1, is characterized in that, described ethanol is food-grade ethanol, and acidic ethanol refers to the food stage citric acid containing 0.1-0.9%.
4. the preparation method of Fructus Mori phenolic compound extracting solution according to claim 1, it is characterized in that, described Mechanical Crushing is through colloid mill, broken under 1.5-2.2Kw condition; Time is 3-10min.
5. the preparation method of Fructus Mori phenolic compound extracting solution according to claim 1, is characterized in that, the centrifugal rotating speed described in step (3) is 3000-8000g, and the time is 10-20min.
6. the preparation method of Fructus Mori phenolic compound extracting solution according to claim 1, is characterized in that, the centrifugal rotating speed described in step (5) is 3000-8000g, and the time is 10-20min.
7. the preparation method of Fructus Mori phenolic compound extracting solution according to claim 1, is characterized in that, the temperature of described frozen water is 0-4 DEG C.
8. a Fructus Mori reactive phenolic compounds, it is characterized in that its by claim 1 ?extracting method described in 7 any one obtain, in described Fructus Mori extract reactive phenolic compounds content be 120 ?400mgGAE/gdw, anthocyan content be 60 ?90mgcyd ?3 ?glu/gdw, prepared Fructus Mori extracting solution is bright in colour, tool antioxidation and suppress a ?glucosidase activity.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510862706.3A CN105343186B (en) | 2015-11-30 | 2015-11-30 | A kind of mulberries reactive phenolic compounds and its green method for extraction and purification |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510862706.3A CN105343186B (en) | 2015-11-30 | 2015-11-30 | A kind of mulberries reactive phenolic compounds and its green method for extraction and purification |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105343186A true CN105343186A (en) | 2016-02-24 |
| CN105343186B CN105343186B (en) | 2019-08-20 |
Family
ID=55319346
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510862706.3A Active CN105343186B (en) | 2015-11-30 | 2015-11-30 | A kind of mulberries reactive phenolic compounds and its green method for extraction and purification |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105343186B (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106046848A (en) * | 2016-06-06 | 2016-10-26 | 西昌学院 | Method for extracting and purifying anthocyanin from mulberry pomace |
| 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 |
| 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 |
| 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 |
| CN107927784A (en) * | 2017-12-15 | 2018-04-20 | 齐鲁工业大学 | Fruit mulberry soaks warehouse paste manufacture process optimizing research |
| 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 |
| US20190290575A1 (en) | 2018-03-23 | 2019-09-26 | Mary Kay Inc. | Topical compositions and methods |
| CN111789204A (en) * | 2020-08-27 | 2020-10-20 | 蔡晓明 | Mulberry beverage and preparation method thereof |
| US11389392B2 (en) | 2017-06-13 | 2022-07-19 | Mary Kay Inc. | Cosmetic compositions and methods for their use in firming skin |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103610750A (en) * | 2013-11-07 | 2014-03-05 | 李刚 | Method for extracting, separating and purifying glucosidase inhibitor |
| CN103881867A (en) * | 2014-03-24 | 2014-06-25 | 山东省蚕业研究所 | Preparation method of mulberry fruit wine |
| CN103981067A (en) * | 2014-06-05 | 2014-08-13 | 济南国力生物科技有限公司 | Processing technology of mulberry fruit |
| CN104403359A (en) * | 2014-11-14 | 2015-03-11 | 陕西科技大学 | Method for preparation of mulberry pigment by mulberry residue |
-
2015
- 2015-11-30 CN CN201510862706.3A patent/CN105343186B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103610750A (en) * | 2013-11-07 | 2014-03-05 | 李刚 | Method for extracting, separating and purifying glucosidase inhibitor |
| CN103881867A (en) * | 2014-03-24 | 2014-06-25 | 山东省蚕业研究所 | Preparation method of mulberry fruit wine |
| CN103981067A (en) * | 2014-06-05 | 2014-08-13 | 济南国力生物科技有限公司 | Processing technology of mulberry fruit |
| CN104403359A (en) * | 2014-11-14 | 2015-03-11 | 陕西科技大学 | Method for preparation of mulberry pigment by mulberry residue |
Non-Patent Citations (3)
| Title |
|---|
| 吴庆智: "超声波辅助提取桑椹色素的技术研究", 《食品科技》 * |
| 李永春: "微波处理对籽瓜多酚氧化酶活性的影响", 《江苏农业科学》 * |
| 游庭活；等: "应用响应曲面法优化超声波辅助乙醇提取桑椹多酚的工艺技术条件", 《蚕业科学》 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106046848A (en) * | 2016-06-06 | 2016-10-26 | 西昌学院 | Method for extracting and purifying anthocyanin from mulberry pomace |
| 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 |
| 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 |
| US11389392B2 (en) | 2017-06-13 | 2022-07-19 | Mary Kay Inc. | Cosmetic compositions and methods for their use in firming 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 |
| CN107927784A (en) * | 2017-12-15 | 2018-04-20 | 齐鲁工业大学 | Fruit mulberry soaks warehouse paste manufacture process optimizing research |
| US20190290575A1 (en) | 2018-03-23 | 2019-09-26 | Mary Kay Inc. | Topical compositions and methods |
| US11701322B2 (en) | 2018-03-23 | 2023-07-18 | Mary Kay Inc. | 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105343186B (en) | 2019-08-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105343186A (en) | Mulberry active phenolic compound and pollution-free extraction and purification method thereof | |
| CN101461514B (en) | Bitter melon extract preparation method | |
| CN106243172B (en) | A method of extracting black fruit fructus lycii anthocyanin | |
| CN103478838B (en) | Honeysuckle kudzuvine root beverage and preparation method thereof | |
| CN104342337B (en) | A kind of production technique of Sunset Abelmoschus Root functional health wine | |
| CN101919512B (en) | Production process of highland barley green | |
| CN106281638B (en) | A kind of method that camellia seed oil and oil tea saponin and camellia seed meal feed are extracted from camellia seed kernel | |
| CN103892154B (en) | A kind of method utilizing blueberry residue production blueberry fruit cake | |
| CN111000875A (en) | Extraction method of kelp polyphenol | |
| EP0301956B1 (en) | Method for processing food | |
| CN109096079A (en) | A kind of production technology of rapidly extracting curcumin | |
| CN106699916A (en) | Combined extraction method of polyphenols and polysaccharides from lotus roots | |
| CN103462140B (en) | Low frequency ultrasonic-assisted desugaring and deacidification method for concentrated waxberry juice | |
| CN102807570A (en) | Method for preparing gallogen by platycarya strobilacea fruit | |
| CN108432987A (en) | A kind of preparation method of lotus root juice drink | |
| CN105124689A (en) | Processing method and application of carmine red radish condensed juice products | |
| CN104495754A (en) | Extraction method of algae iodate and composite algae iodate salt additive | |
| CN101070334B (en) | Process for separating tea sapogenin and tea polysaccharide from tea-oil cake | |
| CN1255481C (en) | Process for extracting natural red pigment from purple sweet potato with alcohol | |
| CN116784476A (en) | Composition containing concentrated powder of Aronia melanocarpa fruit, apple, acerola cherry and mulberry, and preparation and application thereof | |
| CN110623179A (en) | Method for extracting mulberry juice | |
| CN112442136A (en) | Method for extracting functional components from tremella | |
| CN103122039B (en) | Process for extracting pectin from acid discharge liquor generated in canned citrus production | |
| CN101433322A (en) | Functional food rich in anthocyanidin and preparation method thereof | |
| CN105685740B (en) | A method of preparing concentration Rabdosia rubescens juice |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 510640 No. five, 381 mountain road, Guangzhou, Guangdong, Tianhe District Patentee after: SOUTH CHINA University OF TECHNOLOGY Patentee after: Guangzhou Zhongmei Pulai Health Technology Co.,Ltd. Address before: 510640 No. five, 381 mountain road, Guangzhou, Guangdong, Tianhe District Patentee before: SOUTH CHINA University OF TECHNOLOGY Patentee before: GUANGZHOU DR. SUGAR Co.,Ltd. |
|
| CP01 | Change in the name or title of a patent holder | ||
| TR01 | Transfer of patent right |
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. |
|
| TR01 | Transfer of patent right |