CN109691673A - A kind of extract and preparation method thereof containing plant polyphenol - Google Patents

A kind of extract and preparation method thereof containing plant polyphenol Download PDF

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Publication number
CN109691673A
CN109691673A CN201811488503.2A CN201811488503A CN109691673A CN 109691673 A CN109691673 A CN 109691673A CN 201811488503 A CN201811488503 A CN 201811488503A CN 109691673 A CN109691673 A CN 109691673A
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China
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pear skin
mixture
pear
preparation
ultrasonic
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郭巍
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Dawan Hanwei (guangzhou) Pharmaceutical Science And Technology Group Co Ltd
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Dawan Hanwei (guangzhou) Pharmaceutical Science And Technology Group Co Ltd
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Priority to CN201811488503.2A priority Critical patent/CN109691673A/en
Publication of CN109691673A publication Critical patent/CN109691673A/en
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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/105—Plant extracts, their artificial duplicates or their derivatives
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs

Abstract

The invention discloses a kind of extract and preparation method thereof containing plant polyphenol.Preparation method of the present invention include the following steps: (1) by pear skin, solvent, composite plant hydrolase, pH adjusting agent and antioxidant mix mixture A, the mixture A pH be 2-5；(2) by step (1) the mixture A vacuum ultrasonic, filter to get filtrate B；(3) by liquor B described in step (2) through macroporous resin adsorption, elution, freeze-drying.The present invention extracts plant polyphenol using the pear skin discarded in food industry, realizes the effective use of raw material, the content of the plant polyphenol extracted in every gram of raw material is up to 25.78-32.14mg, extraction efficiency is high, and extracting method simple process, it is environmentally protective, it is suitable for industrialized large-scaled production.

Description

A kind of extract and preparation method thereof containing plant polyphenol
Technical field
The present invention relates to a kind of extract and preparation method thereof containing plant polyphenol.
Background technique
Pears are the third-largest fruit in China, and area and yield are only second to apple and citrus.Due to its contain there are many as chlorogenic acid, The substances of classifying such as vanillic aldehyde, myricetrin, have the function of certain anti-oxidation health more.Anli pear category autumn pear (Pyrus Ussuriensis Maxim), it is commonly called as sour pears.For the ancient local fruit of one kind that North China or the Northeast produce, it is mainly distributed on The southern and Yanshan mountain range region of Northeast China.Fruit is round or oblate, pericarp yellow green or golden yellow, fruit compared with Small, about about 200 grams of weight, lithocyte is more, and after sufficiently mature, sour and sweet palatability, strong fragrance, pure and fresh refreshing people, fruit is rich in The nutrition of a variety of needed by human body, containing sugar 8.78%, containing acid 1.27%, l.54% vitamin, is rich in soluble solid.Peace Pear tree lasts a long time, and in Qianxi, the old sour pear tree of one band reaches 100 years or so, if management is proper, single plant yield is up to 500 public affairs Jin.
According to analysis, plant polyphenol is rich in the anli pear of Hebei.Plant polyphenol is widely present in plant, is had anti- The different physiological roles such as scorching, anti-oxidant, antitumor, protection liver.But polyphenol substance is simultaneously unstable, especially in fruit extraction process In, easily by polyphenol oxidase oxydasis, original bioactivity is lost, and extracting solution blackening is made to turn yellow, influences product quality and outer It sees.
Summary of the invention
The technical problem to be solved by the present invention is to the extraction processes in order to overcome plant polyphenol in the prior art Or there are problems that plant polyphenol is easily oxidized to lose bioactivity during the extraction process, or exist because of material It crushes imperfect or plant cell wall to be crushed insufficient and cannot sufficiently discharge polyphenol substance, leads to the problem of extraction efficiency difference, The extract for thus providing a kind of preparation method of the extract containing plant polyphenol and its being prepared.Preparation side of the invention Method simple process, it is environmentally protective, it is suitable for industrialized large-scaled production；The extract that the preparation method is prepared through the invention In, the polyphenol recovery rate of the plant polyphenol is up to 25.78-32.14mg/g.
For avoid it is above-mentioned refer to all kinds of problems, present inventor by further investigation, creatively using enzyme process with Cryogenic vacuum ultrasonic extracting process combines, and dissolves out the polyphenol substance in pear skin adequately, and polyphenol is prevented to be oxidized, after Using membrane technology filtering and impurity removing, ethanol elution is used again after macroporous resin adsorption, it is freeze-dried, it can obtain preferable more Phenol extraction rate.
The present invention is to solve above-mentioned technical problem by following technical proposals.
The present invention provides a kind of preparation methods of extract containing plant polyphenol comprising following steps:
(1) pear skin, solvent, composite plant hydrolase, pH adjusting agent and antioxidant are mixed into obtain mixture A, it is described mixed The pH for closing object A is 2-5；
(2) by step (1) the mixture A vacuum ultrasonic, filter to get filtrate B；
(3) by liquor B described in step (2) through macroporous resin adsorption, elution, freeze-drying.
In step (1), the pear skin can be the pericarp of pears described in the routine of this field, may be derived from anli pear (Pyrus ussuriensis Maxim)。
In step (1), the solvent is ethanol water；The concentration of the ethanol water is 40-70%, such as 45%-60% or 60%, the percentage are mass percent of the ethyl alcohol in ethanol water.
In step (1), the dosage of the solvent can be for used in the such preparation method routine in this field, the specifically pear skin Mass volume ratio with the solvent can be 1/3 (kg/L).
In step (1), the composite plant hydrolase can be concretely fine for used in the such preparation method routine in this field Tie up plain enzyme and/or pectase.
In step (1), the dosage of the composite plant hydrolase is the specially 2%-5% not less than 2%, or can be 3%-4%, such as 2.5%-3.5%, the percentage are matter of the composite plant hydrolase in the mixture A Measure percentage.
In step (1), the type of the pH adjusting agent can be that used in the such preparation method routine in this field, specifically may be selected One of hydrochloric acid, phosphoric acid, nitric acid, sulfuric acid, glacial acetic acid are a variety of, such as glacial acetic acid.
In step (1), the dosage of the pH adjusting agent is the pH 2-5 for making the mixture A, concretely 2.5-4 or 3-3.5, such as 4.5.
In step (1), the type of the antioxidant can specifically can be selected from for used in the such preparation method routine in this field One of vitamin C, vitamin E, lycopene, astaxanthin, grape seed extract are a variety of, such as vitamin C.
In step (1), the dosage of the antioxidant is the specially 0.05-0.15% not less than 0.05%, such as 0.06%-0.10% or 0.07%-0.08%, the percentage refer to quality of the antioxidant in the mixture A Percentage.
In step (1), the mixed precedence is not required to specifically be limited.
In step (1), can by the pear skin pre-process after again with the solvent, the pH adjusting agent and the antioxidant Mixing.Wherein, the pretreated mode can be used in the such preparation method routine in this field, such as to rub.
In step (1), after the mixing, the mixture A can be also crushed；The broken mode can be ability Used in the such preparation method routine in domain, as colloid mill is broken.Wherein, the broken degree can be to be crushed to 200 mesh.
In step (1), the mixture A can the compound plant as described in the pear skin, 40-70% ethanol water, 2%-5% The vitamin C of object hydrolase, glacial acetic acid and 0.05%-0.15% forms, and the pH of the mixture A is 2-5.
In step (1), the mixture A can the compound plant as described in the pear skin, 45-60% ethanol water, 3%-4% The vitamin C of object hydrolase, glacial acetic acid and 0.06%-0.10% forms, and the pH of the mixture A is 2.5-4.
In step (1), the mixture A can be hydrolyzed by the pear skin, 60% ethanol water, 3% composite plant Enzyme, glacial acetic acid and 0.08% vitamin C composition, the pH of the mixture A is 4.
In step (2), the vacuum ultrasonic can be for used in the such preparation method routine in this field, specifically can be in vacuum ultrasonic It is ultrasonic in wave reaction kettle.Wherein,
The vacuum degree of the ultrasound is 60Pa-120Pa, specially 80Pa-100Pa；
The temperature of the reaction kettle is 8 DEG C -20 DEG C, specially 10 DEG C -15 DEG C；
The power of the ultrasound is preferably 300-600W；
The tranmitting frequency of the ultrasound is preferably 20-30KHz；
The pulse cycle frequency of the ultrasound is preferably 10-20 times/second；
The velocity of sound of the ultrasound is preferably 800-1600 meter per second；
The liquid surface sound pressure level of the ultrasound is preferably 20-40 °；
The time of the ultrasound is not shorter than 40min, specially 40min-100min, such as 60min-80min preferably.
In step (2), the condition of the vacuum ultrasonic further may be used specifically: vacuum degree 80Pa-100Pa, 10 DEG C of temperature- 15 DEG C, ultrasonic power 300-600W, tranmitting frequency 20-30KHz, the 10-20 times/second of pulse cycle frequency, 800-1600 meters of the velocity of sound/ Second, 20-40 ° of liquid surface sound pressure level and ultrasonic time 40-100min.
In step (2), the condition of the vacuum ultrasonic further may be used specifically: vacuum degree 60Pa-120Pa, 8 DEG C of temperature- 20 DEG C, ultrasonic power 300-600W, tranmitting frequency 20-30KHz, the 10-20 times/second of pulse cycle frequency, 800-1600 meters of the velocity of sound/ Second, 20-40 ° of liquid surface sound pressure level and ultrasonic time 60-80min.
In step (2), the mixture A after the vacuum ultrasonic is through circulating pump discharging, filtering；The pressure of the circulating pump Can be for used in the such preparation method routine in this field, concretely 0.5-1MPa；The filtering can be the such preparation side in this field Used in method routine, ultrafiltration membrance filter specifically can be used, the ultrafiltration membrane can be used in the such preparation method routine in this field, specifically Its molecular cut off of ground can be ten thousand Dalton molecular weight of 5-15.
In step (3), the macroporous resin adsorption is that liquor B described in step (2) is carried out to macroporous resin adsorption, described Macroreticular resin concretely D101 resin.
In step (3), the elution can carry out for ethyl alcohol used in the such preparation method routine in this field, specifically can be used Elution, the concentration of the ethyl alcohol can be 40-60%.
In step (3), the freeze-drying is the operation of this field normal freeze-drying.
The present invention still further provides made from a kind of preparation method as the above-mentioned extract containing plant polyphenol containing planting The extract of object polyphenol.
In the present invention, unless otherwise instructed, the polyphenol recovery rate (mg/g)=C × V × N/m；
In formula, C is polyphenol mass concentration (mg/mL) in extracting solution；
V is extracting liquid volume (mL)；
N is extension rate；
M is pear skin quality (g).
In the present invention, unless otherwise instructed, the room temperature is 20-25 DEG C.
On the basis of common knowledge of the art, above-mentioned each optimum condition, can any combination to get each preferable reality of the present invention Example.
The reagents and materials used in the present invention are commercially available.
The positive effect of the present invention is that:
(1) extract containing plant polyphenol extracted using the method for extraction plant polyphenol of the invention, wherein more Phenol extraction rate is up to 25.78-32.14mg/g.
(2) present invention extracts plant polyphenol using the pear skin discarded in food industry, realizes the effective use of raw material, saves About resource.
(3) extracting method simple process of the invention, it is environmentally protective, it is suitable for industrialized large-scaled production.
Specific embodiment
The present invention is further illustrated below by the mode of embodiment, but does not therefore limit the present invention to the reality It applies among a range.In the following examples, the experimental methods for specific conditions are not specified, according to conventional methods and conditions, or according to quotient The selection of product specification.
It in following embodiment and comparative examples, is such as not specifically noted, used fresh anli pear (Pyrus Ussuriensis Maxim) exocarp of fruit is 500g, and the place of production is Hebei province Qinglong County；Used reagent is state Analytical reagents is produced, producer is Sinopharm Chemical Reagent Co., Ltd.；Vacuum ultrasonic reaction kettle is purchased from Nanjing elder generation Europe instrument Manufacturing Co., Ltd.
Each operating procedure, is such as not specifically noted in following embodiments, each means and operates at room temperature.
Embodiment 1 extracts active constituent plant polyphenol from fruit pear skin
1) exocarp of fresh anli pear (Pyrus ussuriensis Maxim) fruit is taken, silt, residual leaf, corruption are removed Equal sundries, are put into rinse bath, three times with clean tap water cleaning, add deionized water cleaning once, pull out and drain the water Point, obtain pear skin.Start meat grinder, pear skin is all rubbed, the pear skin after rubbing is collected in stainless steel barrel, and 3 times of weight are added , it is final concentration of that quality is added with glacial acetic acid adjustment endpoint pH for 5 than the ethanol water for 40% in volumetric concentration 0.05% Vc, the composite plant hydrolase of quality final concentration of 2%, is thoroughly mixed, and forms broken pear skin mixed liquor.It opens Dynamic colloid mill, setting fineness are 200 mesh, and the feeding inlet that broken pear skin mixed liquor gradually puts into colloid mill is ground, and are exported Feed liquid ground repeatedly with the same manner again once, be always co-mulled and made into twice, finally ground after pear skin slurry.
2) the pear skin slurry prepared is inputted in vacuum ultrasonic reaction kettle, is evacuated to 120Pa, control temperature in the kettle 20 DEG C, the power for adjusting ultrasonic transmitter is 300W, sets ultrasonic wave tranmitting frequency as 20KHz, pulse cycle frequency 20 times/ Second, 800 meter per second of acoustic beam, liquid surface sound pressure level is 20o, starts ultrasonic wave program, controls ultrasonic intensity, produces pear skin slurry Raw obvious vortex.Ultrasonication 80 minutes, obtain pear skin active component extract.By pear skin active component extract, use Circulating pump sets circulating pump conveying pressure as 0.5MPa, and liquid phase feed liquid is made to pass through the ultrafiltration of 50,000 dalton of molecular cut off Film removes solid phase impurity.Efflux after collecting ultrafiltration.
3) by above-mentioned efflux, at room temperature by D101 macroreticular resin chromatographic column, flow control 10cm/min, later Chromatographic column is cleaned with the distilled water of 5 column volumes, then is eluted with the ethanol water that volume ratio is 40%, elution is collected Liquid.Above-mentioned eluent is dried in vacuo, control drying temperature is 20 DEG C, vacuum degree 120Pa, until it is dry complete, as The plant polyphenol extract object P1 of extraction.Polyphenol content (Jiang Lifang, Chinese pear pear skin are measured in Folin-Ciocalteu method Polyphenol content measurement, chemical engineering and equipment, the 12nd phase in 2011,168-172 pages), it is converted to the list relative to pear skin raw material Position weight extracted amount (being shown in Table 1).
Embodiment 2 extracts active constituent plant polyphenol from fruit pear skin
1) exocarp of fresh anli pear (Pyrus ussuriensis Maxim) fruit is taken, silt, residual leaf, corruption are removed Equal sundries, are put into rinse bath, three times with clean tap water cleaning, add deionized water cleaning once, pull out and drain the water Point, obtain pear skin.Start meat grinder, pear skin is all rubbed, the pear skin after rubbing is collected in stainless steel barrel, and 3 times of weight are added , it is final concentration of that quality is added with glacial acetic acid adjustment endpoint pH for 4 than the ethanol water for 60% in volumetric concentration 0.08% Vc, the composite plant hydrolase of quality final concentration of 3%, is thoroughly mixed, and forms broken pear skin mixed liquor.It opens Dynamic colloid mill, setting fineness are 200 mesh, and the feeding inlet that broken pear skin mixed liquor gradually puts into colloid mill is ground, and are exported Feed liquid ground repeatedly with the same manner again once, be always co-mulled and made into twice, finally ground after pear skin slurry.
2) the pear skin slurry prepared is inputted in vacuum ultrasonic reaction kettle, is evacuated to 100Pa, control temperature in the kettle 15 DEG C, the power for adjusting ultrasonic transmitter is 450W, sets ultrasonic wave tranmitting frequency as 25KHz, pulse cycle frequency 15 times/ Second, 1200 meter per second of acoustic beam, liquid surface sound pressure level is 30 °, starts ultrasonic wave program, controls ultrasonic intensity, produces pear skin slurry Raw obvious vortex.Ultrasonication 60 minutes, obtain pear skin active component extract.By pear skin active component extract, use Circulating pump sets circulating pump conveying pressure as 0.8MPa, and liquid phase feed liquid is made to pass through the ultrafiltration of 100,000 dalton of molecular cut off Film removes solid phase impurity.Efflux after collecting ultrafiltration.
3) by above-mentioned efflux, at room temperature by D101 macroreticular resin chromatographic column, flow control 10cm/min, later Chromatographic column is cleaned with the distilled water of 5 column volumes, then is eluted with the ethanol water that volume ratio is 50%, elution is collected Liquid.Above-mentioned eluent is dried in vacuo, control drying temperature is 20 DEG C, vacuum degree 120Pa, until it is dry complete, as The plant polyphenol extract object P2 of extraction.Polyphenol content is measured in Folin-Ciocalteu method, is converted to relative to pear skin original The Unit Weight extracted amount (being shown in Table 1) of material.
Embodiment 3 extracts active constituent plant polyphenol from fruit pear skin
1) exocarp of fresh anli pear (Pyrus ussuriensis Maxim) fruit is taken, silt, residual leaf, corruption are removed Equal sundries, are put into rinse bath, three times with clean tap water cleaning, add deionized water cleaning once, pull out and drain the water Point, obtain pear skin.Start meat grinder, pear skin is all rubbed, the pear skin after rubbing is collected in stainless steel barrel, and 3 times of weight are added , quality final concentration of 0.1% is added with glacial acetic acid adjustment endpoint pH for 3 than the ethanol water for 70% in volumetric concentration Vc, the composite plant hydrolase of quality final concentration of 4% is thoroughly mixed, and forms broken pear skin mixed liquor.Start colloid Mill, setting fineness are 200 mesh, the feeding inlet that broken pear skin mixed liquor gradually puts into colloid mill are ground, the feed liquid of outlet It is ground once, is always co-mulled and made into twice repeatedly with the same manner again, the pear skin slurry after finally being ground.
2) the pear skin slurry prepared is inputted in vacuum ultrasonic reaction kettle, is evacuated to 80Pa, control temperature in the kettle 10 DEG C, the power for adjusting ultrasonic transmitter is 600W, sets ultrasonic wave tranmitting frequency as 30KHz, pulse cycle frequency 10 times/ Second, 1600 meter per second of acoustic beam, liquid surface sound pressure level is 40o, starts ultrasonic wave program, controls ultrasonic intensity, produces pear skin slurry Raw obvious vortex.Ultrasonication 40 minutes, obtain pear skin active component extract.By pear skin active component extract, use Circulating pump sets circulating pump conveying pressure as 1MPa, and liquid phase feed liquid is made to pass through the ultrafiltration membrane of 150,000 dalton of molecular cut off, Remove solid phase impurity.Efflux after collecting ultrafiltration.
3) by above-mentioned efflux, at room temperature by D101 macroreticular resin chromatographic column, flow control 10cm/min, later Chromatographic column is cleaned with the distilled water of 5 column volumes, then is eluted with the ethanol water that volume ratio is 60%, elution is collected Liquid.Above-mentioned eluent is dried in vacuo, control drying temperature is 20 DEG C, vacuum degree 120Pa, until it is dry complete, as The plant polyphenol extract object P3 of extraction.Polyphenol content is measured in Folin-Ciocalteu method, is converted to relative to pear skin original The Unit Weight extracted amount (being shown in Table 1) of material.
Embodiment 4 extracts active constituent plant polyphenol from fruit pear skin
1) exocarp of fresh anli pear (Pyrus ussuriensis Maxim) fruit is taken, silt, residual leaf, corruption are removed Equal sundries, are put into rinse bath, three times with clean tap water cleaning, add deionized water cleaning once, pull out and drain the water Point, obtain pear skin.Start meat grinder, pear skin is all rubbed, the pear skin after rubbing is collected in stainless steel barrel, and 3 times of weight are added , it is final concentration of that quality is added with glacial acetic acid adjustment endpoint pH for 4.5 than the ethanol water for 50% in volumetric concentration 0.07% Vc, the composite plant hydrolase of quality final concentration of 2.5%, is thoroughly mixed, and forms broken pear skin mixed liquor. Start colloid mill, setting fineness is 200 mesh, the feeding inlet that broken pear skin mixed liquor gradually puts into colloid mill is ground, out The feed liquid of mouth is ground with the same manner once repeatedly again, is always co-mulled and made into twice, the pear skin slurry after finally being ground.
2) the pear skin slurry prepared is inputted in vacuum ultrasonic reaction kettle, is evacuated to 90Pa, control temperature in the kettle 17 DEG C, the power for adjusting ultrasonic transmitter is 500W, sets ultrasonic wave tranmitting frequency as 30KHz, pulse cycle frequency 20 times/ Second, 1000 meter per second of acoustic beam, liquid surface sound pressure level is 40 °, starts ultrasonic wave program, controls ultrasonic intensity, produces pear skin slurry Raw obvious vortex.Ultrasonication 50 minutes, obtain pear skin active component extract.By pear skin active component extract, use Circulating pump sets circulating pump conveying pressure as 0.7MPa, and liquid phase feed liquid is made to pass through the ultrafiltration of 150,000 dalton of molecular cut off Film removes solid phase impurity.Efflux after collecting ultrafiltration.
3) by above-mentioned efflux, at room temperature by D101 macroreticular resin chromatographic column, flow control 10cm/min, later Chromatographic column is cleaned with the distilled water of 5 column volumes, then is eluted with the ethanol water that volume ratio is 45%, elution is collected Liquid.Above-mentioned eluent is dried in vacuo, control drying temperature is 20 DEG C, vacuum degree 120Pa, until it is dry complete, as The plant polyphenol extract object P4 of extraction.Polyphenol content is measured in Folin-Ciocalteu method, is converted to relative to pear skin original The Unit Weight extracted amount (being shown in Table 1) of material.
Embodiment 5 extracts active constituent plant polyphenol from fruit pear skin
1) exocarp of fresh anli pear (Pyrus ussuriensis Maxim) fruit is taken, silt, residual leaf, corruption are removed Equal sundries, are put into rinse bath, three times with clean tap water cleaning, add deionized water cleaning once, pull out and drain the water Point, obtain pear skin.Start meat grinder, pear skin is all rubbed, the pear skin after rubbing is collected in stainless steel barrel, and 3 times of weight are added , it is final concentration of that quality is added with glacial acetic acid adjustment endpoint pH for 3.5 than the ethanol water for 45% in volumetric concentration 0.06% Vc, the composite plant hydrolase of quality final concentration of 3.5%, is thoroughly mixed, and forms broken pear skin mixed liquor. Start colloid mill, setting fineness is 200 mesh, the feeding inlet that broken pear skin mixed liquor gradually puts into colloid mill is ground, out The feed liquid of mouth is ground with the same manner once repeatedly again, is always co-mulled and made into twice, the pear skin slurry after finally being ground.
2) the pear skin slurry prepared is inputted in vacuum ultrasonic reaction kettle, is evacuated to 110Pa, control temperature in the kettle 12 DEG C, the power for adjusting ultrasonic transmitter is 400W, sets ultrasonic wave tranmitting frequency as 20KHz, pulse cycle frequency 15 times/ Second, 1400 meter per second of acoustic beam, liquid surface sound pressure level is 20 °, starts ultrasonic wave program, controls ultrasonic intensity, produces pear skin slurry Raw obvious vortex.Ultrasonication 70 minutes, obtain pear skin active component extract.By pear skin active component extract, use Circulating pump sets circulating pump conveying pressure as 0.9MPa, and liquid phase feed liquid is made to pass through the ultrafiltration of 100,000 dalton of molecular cut off Film removes solid phase impurity.Efflux after collecting ultrafiltration.
3) by above-mentioned efflux, at room temperature by D101 macroreticular resin chromatographic column, flow control 10cm/min, later Chromatographic column is cleaned with the distilled water of 5 column volumes, then is eluted with the ethanol water that volume ratio is 55%, elution is collected Liquid.Above-mentioned eluent is dried in vacuo, control drying temperature is 20 DEG C, vacuum degree 120Pa, until it is dry complete, as The plant polyphenol extract object P5 of extraction.Polyphenol content is measured in Folin-Ciocalteu method, is converted to relative to pear skin original The Unit Weight extracted amount (being shown in Table 1) of material.
Embodiment 6 extracts active constituent plant polyphenol from fruit pear skin
1) exocarp of fresh anli pear (Pyrus ussuriensis Maxim) fruit is taken, silt, residual leaf, corruption are removed Equal sundries, are put into rinse bath, three times with clean tap water cleaning, add deionized water cleaning once, pull out and drain the water Point, obtain pear skin.Start meat grinder, pear skin is all rubbed, the pear skin after rubbing is collected in stainless steel barrel, and 3 times of weight are added , it is dense eventually that quality is added with glacial acetic acid and hydrochloric acid adjustment endpoint pH for 2.5 than the ethanol water for 60% in volumetric concentration The Vc that degree is 0.08%, the composite plant hydrolase of quality final concentration of 3% are thoroughly mixed, and form broken pear skin mixing Liquid.Starting colloid mill, setting fineness is 200 mesh, the feeding inlet that broken pear skin mixed liquor gradually puts into colloid mill ground, The feed liquid of outlet is ground with the same manner once repeatedly again, is always co-mulled and made into twice, the pear skin slurry after finally being ground.
2) the pear skin slurry prepared is inputted in vacuum ultrasonic reaction kettle, is evacuated to 100Pa, control temperature in the kettle 15 DEG C, the power for adjusting ultrasonic transmitter is 450W, sets ultrasonic wave tranmitting frequency as 25KHz, pulse cycle frequency 15 times/ Second, 1200 meter per second of acoustic beam, liquid surface sound pressure level is 30 °, starts ultrasonic wave program, controls ultrasonic intensity, produces pear skin slurry Raw obvious vortex.Ultrasonication 60 minutes, obtain pear skin active component extract.By pear skin active component extract, use Circulating pump sets circulating pump conveying pressure as 0.8MPa, and liquid phase feed liquid is made to pass through the ultrafiltration of 100,000 dalton of molecular cut off Film removes solid phase impurity.Efflux after collecting ultrafiltration.
3) by above-mentioned efflux, at room temperature by D101 macroreticular resin chromatographic column, flow control 10cm/min, later Chromatographic column is cleaned with the distilled water of 5 column volumes, then is eluted with the ethanol water that volume ratio is 50%, elution is collected Liquid.Above-mentioned eluent is dried in vacuo, control drying temperature is 20 DEG C, vacuum degree 120Pa, until it is dry complete, as The plant polyphenol extract object C3 of extraction.Polyphenol content is measured in Folin-Ciocalteu method, is converted to relative to pear skin original The Unit Weight extracted amount (being shown in Table 1) of material.
Embodiment 7 extracts active constituent plant polyphenol from fruit pear skin
1) exocarp of fresh anli pear (Pyrus ussuriensis Maxim) fruit is taken, silt, residual leaf, corruption are removed Equal sundries, are put into rinse bath, three times with clean tap water cleaning, add deionized water cleaning once, pull out and drain the water Point, obtain pear skin.Start meat grinder, pear skin is all rubbed, the pear skin after rubbing is collected in stainless steel barrel, and 3 times of weight are added , it is final concentration of that quality is added with glacial acetic acid adjustment endpoint pH for 4 than the ethanol water for 60% in volumetric concentration 0.15% Vc, the composite plant hydrolase of quality final concentration of 3%, is thoroughly mixed, and forms broken pear skin mixed liquor.It opens Dynamic colloid mill, setting fineness are 200 mesh, and the feeding inlet that broken pear skin mixed liquor gradually puts into colloid mill is ground, and are exported Feed liquid ground repeatedly with the same manner again once, be always co-mulled and made into twice, finally ground after pear skin slurry.
2) the pear skin slurry prepared is inputted in vacuum ultrasonic reaction kettle, is evacuated to 100Pa, control temperature in the kettle 15 DEG C, the power for adjusting ultrasonic transmitter is 450W, sets ultrasonic wave tranmitting frequency as 25KHz, pulse cycle frequency 15 times/ Second, 1200 meter per second of acoustic beam, liquid surface sound pressure level is 30 °, starts ultrasonic wave program, controls ultrasonic intensity, produces pear skin slurry Raw obvious vortex.Ultrasonication 60 minutes, obtain pear skin active component extract.By pear skin active component extract, use Circulating pump sets circulating pump conveying pressure as 0.8MPa, and liquid phase feed liquid is made to pass through the ultrafiltration of 100,000 dalton of molecular cut off Film removes solid phase impurity.Efflux after collecting ultrafiltration.
3) by above-mentioned efflux, at room temperature by D101 macroreticular resin chromatographic column, flow control 10cm/min, later Chromatographic column is cleaned with the distilled water of 5 column volumes, then is eluted with the ethanol water that volume ratio is 50%, elution is collected Liquid.Above-mentioned eluent is dried in vacuo, control drying temperature is 20 DEG C, vacuum degree 120Pa, until it is dry complete, as The plant polyphenol extract object C5 of extraction.Polyphenol content is measured in Folin-Ciocalteu method, is converted to relative to pear skin original The Unit Weight extracted amount (being shown in Table 1) of material.
Embodiment 8 extracts active constituent plant polyphenol from fruit pear skin
1) exocarp of fresh anli pear (Pyrus ussuriensis Maxim) fruit is taken, silt, residual leaf, corruption are removed Equal sundries, are put into rinse bath, three times with clean tap water cleaning, add deionized water cleaning once, pull out and drain the water Point, obtain pear skin.Start meat grinder, pear skin is all rubbed, the pear skin after rubbing is collected in stainless steel barrel, and 3 times of weight are added , it is final concentration of that quality is added with glacial acetic acid adjustment endpoint pH for 4 than the ethanol water for 60% in volumetric concentration 0.08% Vc, the composite plant hydrolase of quality final concentration of 5%, is thoroughly mixed, and forms broken pear skin mixed liquor.It opens Dynamic colloid mill, setting fineness are 200 mesh, and the feeding inlet that broken pear skin mixed liquor gradually puts into colloid mill is ground, and are exported Feed liquid ground repeatedly with the same manner again once, be always co-mulled and made into twice, finally ground after pear skin slurry.
2) the pear skin slurry prepared is inputted in vacuum ultrasonic reaction kettle, is evacuated to 100Pa, control temperature in the kettle 15 DEG C, the power for adjusting ultrasonic transmitter is 450W, sets ultrasonic wave tranmitting frequency as 25KHz, pulse cycle frequency 15 times/ Second, 1200 meter per second of acoustic beam, liquid surface sound pressure level is 30 °, starts ultrasonic wave program, controls ultrasonic intensity, produces pear skin slurry Raw obvious vortex.Ultrasonication 60 minutes, obtain pear skin active component extract.By pear skin active component extract, use Circulating pump sets circulating pump conveying pressure as 0.8MPa, and liquid phase feed liquid is made to pass through the ultrafiltration of 100,000 dalton of molecular cut off Film removes solid phase impurity.Efflux after collecting ultrafiltration.
3) by above-mentioned efflux, at room temperature by D101 macroreticular resin chromatographic column, flow control 10cm/min, later Chromatographic column is cleaned with the distilled water of 5 column volumes, then is eluted with the ethanol water that volume ratio is 50%, elution is collected Liquid.Above-mentioned eluent is dried in vacuo, control drying temperature is 20 DEG C, vacuum degree 120Pa, until it is dry complete, as The plant polyphenol extract object C7 of extraction.Polyphenol content is measured in Folin-Ciocalteu method, is converted to relative to pear skin original The Unit Weight extracted amount (being shown in Table 1) of material.
Embodiment 9 extracts active constituent plant polyphenol from fruit pear skin
1) exocarp of fresh anli pear (Pyrus ussuriensis Maxim) fruit is taken, silt, residual leaf, corruption are removed Equal sundries, are put into rinse bath, three times with clean tap water cleaning, add deionized water cleaning once, pull out and drain the water Point, obtain pear skin.Start meat grinder, pear skin is all rubbed, the pear skin after rubbing is collected in stainless steel barrel, and 3 times of weight are added , it is final concentration of that quality is added with glacial acetic acid adjustment endpoint pH for 4 than the ethanol water for 60% in volumetric concentration 0.08% Vc, the composite plant hydrolase of quality final concentration of 3%, is thoroughly mixed, and forms broken pear skin mixed liquor.It opens Dynamic colloid mill, setting fineness are 200 mesh, and the feeding inlet that broken pear skin mixed liquor gradually puts into colloid mill is ground, and are exported Feed liquid ground repeatedly with the same manner again once, be always co-mulled and made into twice, finally ground after pear skin slurry.
2) the pear skin slurry prepared is inputted in vacuum ultrasonic reaction kettle, is evacuated to 60Pa, control temperature in the kettle 15 DEG C, the power for adjusting ultrasonic transmitter is 450W, sets ultrasonic wave tranmitting frequency as 25KHz, pulse cycle frequency 15 times/ Second, 1200 meter per second of acoustic beam, liquid surface sound pressure level is 30 °, starts ultrasonic wave program, controls ultrasonic intensity, produces pear skin slurry Raw obvious vortex.Ultrasonication 60 minutes, obtain pear skin active component extract.By pear skin active component extract, use Circulating pump sets circulating pump conveying pressure as 0.8MPa, and liquid phase feed liquid is made to pass through the ultrafiltration of 100,000 dalton of molecular cut off Film removes solid phase impurity.Efflux after collecting ultrafiltration.
3) by above-mentioned efflux, at room temperature by D101 macroreticular resin chromatographic column, flow control 10cm/min, later Chromatographic column is cleaned with the distilled water of 5 column volumes, then is eluted with the ethanol water that volume ratio is 50%, elution is collected Liquid.Above-mentioned eluent is dried in vacuo, control drying temperature is 20 DEG C, vacuum degree 120Pa, until it is dry complete, as The plant polyphenol extract object C9 of extraction.Polyphenol content is measured in Folin-Ciocalteu method, is converted to relative to pear skin original The Unit Weight extracted amount (being shown in Table 1) of material.
Embodiment 10 extracts active constituent plant polyphenol from fruit pear skin
1) exocarp of fresh anli pear (Pyrus ussuriensis Maxim) fruit is taken, silt, residual leaf, corruption are removed Equal sundries, are put into rinse bath, three times with clean tap water cleaning, add deionized water cleaning once, pull out and drain the water Point, obtain pear skin.Start meat grinder, pear skin is all rubbed, the pear skin after rubbing is collected in stainless steel barrel, and 3 times of weight are added , it is final concentration of that quality is added with glacial acetic acid adjustment endpoint pH for 4 than the ethanol water for 60% in volumetric concentration 0.08% Vc, the composite plant hydrolase of quality final concentration of 3%, is thoroughly mixed, and forms broken pear skin mixed liquor.It opens Dynamic colloid mill, setting fineness are 200 mesh, and the feeding inlet that broken pear skin mixed liquor gradually puts into colloid mill is ground, and are exported Feed liquid ground repeatedly with the same manner again once, be always co-mulled and made into twice, finally ground after pear skin slurry.
2) the pear skin slurry prepared is inputted in vacuum ultrasonic reaction kettle, is evacuated to 100Pa, control temperature in the kettle 8 DEG C, the power for adjusting ultrasonic transmitter is 450W, sets ultrasonic wave tranmitting frequency as 25KHz, pulse cycle frequency 15 times/ Second, 1200 meter per second of acoustic beam, liquid surface sound pressure level is 30 °, starts ultrasonic wave program, controls ultrasonic intensity, produces pear skin slurry Raw obvious vortex.Ultrasonication 60 minutes, obtain pear skin active component extract.By pear skin active component extract, use Circulating pump sets circulating pump conveying pressure as 0.8MPa, and liquid phase feed liquid is made to pass through the ultrafiltration of 100,000 dalton of molecular cut off Film removes solid phase impurity.Efflux after collecting ultrafiltration.
3) by above-mentioned efflux, at room temperature by D101 macroreticular resin chromatographic column, flow control 10cm/min, later Chromatographic column is cleaned with the distilled water of 5 column volumes, then is eluted with the ethanol water that volume ratio is 50%, elution is collected Liquid.Above-mentioned eluent is dried in vacuo, control drying temperature is 20 DEG C, vacuum degree 120Pa, until it is dry complete, as The plant polyphenol extract object C11 of extraction.Polyphenol content is measured in Folin-Ciocalteu method, is converted to relative to pear skin The Unit Weight extracted amount (being shown in Table 1) of raw material.
Embodiment 11 extracts active constituent plant polyphenol from fruit pear skin
1) exocarp of fresh anli pear (Pyrus ussuriensis Maxim) fruit is taken, silt, residual leaf, corruption are removed Equal sundries, are put into rinse bath, three times with clean tap water cleaning, add deionized water cleaning once, pull out and drain the water Point, obtain pear skin.Start meat grinder, pear skin is all rubbed, the pear skin after rubbing is collected in stainless steel barrel, and 3 times of weight are added , it is final concentration of that quality is added with glacial acetic acid adjustment endpoint pH for 4 than the ethanol water for 60% in volumetric concentration 0.08% Vc, the composite plant hydrolase of quality final concentration of 3%, is thoroughly mixed, and forms broken pear skin mixed liquor.It opens Dynamic colloid mill, setting fineness are 200 mesh, and the feeding inlet that broken pear skin mixed liquor gradually puts into colloid mill is ground, and are exported Feed liquid ground repeatedly with the same manner again once, be always co-mulled and made into twice, finally ground after pear skin slurry.
2) the pear skin slurry prepared is inputted in vacuum ultrasonic reaction kettle, is evacuated to 100Pa, control temperature in the kettle 15 DEG C, the power for adjusting ultrasonic transmitter is 450W, sets ultrasonic wave tranmitting frequency as 25KHz, pulse cycle frequency 15 times/ Second, 1200 meter per second of acoustic beam, liquid surface sound pressure level is 30 °, starts ultrasonic wave program, controls ultrasonic intensity, produces pear skin slurry Raw obvious vortex.Ultrasonication 100 minutes, obtain pear skin active component extract.By pear skin active component extract, use Circulating pump sets circulating pump conveying pressure as 0.8MPa, and liquid phase feed liquid is made to pass through the ultrafiltration of 100,000 dalton of molecular cut off Film removes solid phase impurity.Efflux after collecting ultrafiltration.
3) by above-mentioned efflux, at room temperature by D101 macroreticular resin chromatographic column, flow control 10cm/min, later Chromatographic column is cleaned with the distilled water of 5 column volumes, then is eluted with the ethanol water that volume ratio is 50%, elution is collected Liquid.Above-mentioned eluent is dried in vacuo, control drying temperature is 20 DEG C, vacuum degree 120Pa, until it is dry complete, as The plant polyphenol extract object C13 of extraction.Polyphenol content is measured in Folin-Ciocalteu method, is converted to relative to pear skin The Unit Weight extracted amount (being shown in Table 1) of raw material.
Comparative example 1 extracts active constituent plant polyphenol from fruit pear skin
1) exocarp of fresh anli pear (Pyrus ussuriensis Maxim) fruit is taken, silt, residual leaf, corruption are removed Equal sundries, are put into rinse bath, three times with clean tap water cleaning, add deionized water cleaning once, pull out and drain the water Point, obtain pear skin.Start meat grinder, pear skin is all rubbed, the pear skin after rubbing is collected in stainless steel barrel, and 3 times of weight are added , it is final concentration of that quality is added with glacial acetic acid adjustment endpoint pH for 4 than the ethanol water for 30% in volumetric concentration 0.08% Vc, the composite plant hydrolase of quality final concentration of 3%, is thoroughly mixed, and forms broken pear skin mixed liquor.It opens Dynamic colloid mill, setting fineness are 200 mesh, and the feeding inlet that broken pear skin mixed liquor gradually puts into colloid mill is ground, and are exported Feed liquid ground repeatedly with the same manner again once, be always co-mulled and made into twice, finally ground after pear skin slurry.
2) the pear skin slurry prepared is inputted in vacuum ultrasonic reaction kettle, is evacuated to 100Pa, control temperature in the kettle 15 DEG C, the power for adjusting ultrasonic transmitter is 450W, sets ultrasonic wave tranmitting frequency as 25KHz, pulse cycle frequency 15 times/ Second, 1200 meter per second of acoustic beam, liquid surface sound pressure level is 30 °, starts ultrasonic wave program, controls ultrasonic intensity, produces pear skin slurry Raw obvious vortex.Ultrasonication 60 minutes, obtain pear skin active component extract.By pear skin active component extract, use Circulating pump sets circulating pump conveying pressure as 0.8MPa, and liquid phase feed liquid is made to pass through the ultrafiltration of 100,000 dalton of molecular cut off Film removes solid phase impurity.Efflux after collecting ultrafiltration.
3) by above-mentioned efflux, at room temperature by D101 macroreticular resin chromatographic column, flow control 10cm/min, later Chromatographic column is cleaned with the distilled water of 5 column volumes, then is eluted with the ethanol water that volume ratio is 50%, elution is collected Liquid.Above-mentioned eluent is dried in vacuo, control drying temperature is 20 DEG C, vacuum degree 120Pa, until it is dry complete, as The plant polyphenol extract object C1 of extraction.Polyphenol content is measured in Folin-Ciocalteu method, is converted to relative to pear skin original The Unit Weight extracted amount (being shown in Table 1) of material.
Comparative example 2 extracts active constituent plant polyphenol from fruit pear skin
1) exocarp of fresh anli pear (Pyrus ussuriensis Maxim) fruit is taken, silt, residual leaf, corruption are removed Equal sundries, are put into rinse bath, three times with clean tap water cleaning, add deionized water cleaning once, pull out and drain the water Point, obtain pear skin.Start meat grinder, pear skin is all rubbed, the pear skin after rubbing is collected in stainless steel barrel, and 3 times of weight are added , it is final concentration of that quality is added with glacial acetic acid adjustment endpoint pH for 4 than the ethanol water for 80% in volumetric concentration 0.08% Vc, the composite plant hydrolase of quality final concentration of 3%, is thoroughly mixed, and forms broken pear skin mixed liquor.It opens Dynamic colloid mill, setting fineness are 200 mesh, and the feeding inlet that broken pear skin mixed liquor gradually puts into colloid mill is ground, and are exported Feed liquid ground repeatedly with the same manner again once, be always co-mulled and made into twice, finally ground after pear skin slurry.
2) the pear skin slurry prepared is inputted in vacuum ultrasonic reaction kettle, is evacuated to 100Pa, control temperature in the kettle 15 DEG C, the power for adjusting ultrasonic transmitter is 450W, sets ultrasonic wave tranmitting frequency as 25KHz, pulse cycle frequency 15 times/ Second, 1200 meter per second of acoustic beam, liquid surface sound pressure level is 30 °, starts ultrasonic wave program, controls ultrasonic intensity, produces pear skin slurry Raw obvious vortex.Ultrasonication 60 minutes, obtain pear skin active component extract.By pear skin active component extract, use Circulating pump sets circulating pump conveying pressure as 0.8MPa, and liquid phase feed liquid is made to pass through the ultrafiltration of 100,000 dalton of molecular cut off Film removes solid phase impurity.Efflux after collecting ultrafiltration.
3) by above-mentioned efflux, at room temperature by D101 macroreticular resin chromatographic column, flow control 10cm/min, later Chromatographic column is cleaned with the distilled water of 5 column volumes, then is eluted with the ethanol water that volume ratio is 50%, elution is collected Liquid.Above-mentioned eluent is dried in vacuo, control drying temperature is 20 DEG C, vacuum degree 120Pa, until it is dry complete, as The plant polyphenol extract object C2 of extraction.Polyphenol content is measured in Folin-Ciocalteu method, is converted to relative to pear skin original The Unit Weight extracted amount (being shown in Table 1) of material.
Comparative example 3 extracts active constituent plant polyphenol from fruit pear skin
1) exocarp of fresh anli pear (Pyrus ussuriensis Maxim) fruit is taken, silt, residual leaf, corruption are removed Equal sundries, are put into rinse bath, three times with clean tap water cleaning, add deionized water cleaning once, pull out and drain the water Point, obtain pear skin.Start meat grinder, pear skin is all rubbed, the pear skin after rubbing is collected in stainless steel barrel, and 3 times of weight are added , it is final concentration of that quality is added with glacial acetic acid adjustment endpoint pH for 6 than the ethanol water for 60% in volumetric concentration 0.08% Vc, the composite plant hydrolase of quality final concentration of 3%, is thoroughly mixed, and forms broken pear skin mixed liquor.It opens Dynamic colloid mill, setting fineness are 200 mesh, and the feeding inlet that broken pear skin mixed liquor gradually puts into colloid mill is ground, and are exported Feed liquid ground repeatedly with the same manner again once, be always co-mulled and made into twice, finally ground after pear skin slurry.
2) the pear skin slurry prepared is inputted in vacuum ultrasonic reaction kettle, is evacuated to 100Pa, control temperature in the kettle 15 DEG C, the power for adjusting ultrasonic transmitter is 450W, sets ultrasonic wave tranmitting frequency as 25KHz, pulse cycle frequency 15 times/ Second, 1200 meter per second of acoustic beam, liquid surface sound pressure level is 30 °, starts ultrasonic wave program, controls ultrasonic intensity, produces pear skin slurry Raw obvious vortex.Ultrasonication 60 minutes, obtain pear skin active component extract.By pear skin active component extract, use Circulating pump sets circulating pump conveying pressure as 0.8MPa, and liquid phase feed liquid is made to pass through the ultrafiltration of 100,000 dalton of molecular cut off Film removes solid phase impurity.Efflux after collecting ultrafiltration.
3) by above-mentioned efflux, at room temperature by D101 macroreticular resin chromatographic column, flow control 10cm/min, later Chromatographic column is cleaned with the distilled water of 5 column volumes, then is eluted with the ethanol water that volume ratio is 50%, elution is collected Liquid.Above-mentioned eluent is dried in vacuo, control drying temperature is 20 DEG C, vacuum degree 120Pa, until it is dry complete, as The plant polyphenol extract object C4 of extraction.Polyphenol content is measured in Folin-Ciocalteu method, is converted to relative to pear skin original The Unit Weight extracted amount (being shown in Table 1) of material.
Comparative example 4 extracts active constituent plant polyphenol from fruit pear skin
1) exocarp of fresh anli pear (Pyrus ussuriensis Maxim) fruit is taken, silt, residual leaf, corruption are removed Equal sundries, are put into rinse bath, three times with clean tap water cleaning, add deionized water cleaning once, pull out and drain the water Point, obtain pear skin.Start meat grinder, pear skin is all rubbed, the pear skin after rubbing is collected in stainless steel barrel, and 3 times of weight are added , it is final concentration of that quality is added with glacial acetic acid adjustment endpoint pH for 4 than the ethanol water for 60% in volumetric concentration 0.03% Vc, the composite plant hydrolase of quality final concentration of 3%, is thoroughly mixed, and forms broken pear skin mixed liquor.It opens Dynamic colloid mill, setting fineness are 200 mesh, and the feeding inlet that broken pear skin mixed liquor gradually puts into colloid mill is ground, and are exported Feed liquid ground repeatedly with the same manner again once, be always co-mulled and made into twice, finally ground after pear skin slurry.
2) the pear skin slurry prepared is inputted in vacuum ultrasonic reaction kettle, is evacuated to 100Pa, control temperature in the kettle 15 DEG C, the power for adjusting ultrasonic transmitter is 450W, sets ultrasonic wave tranmitting frequency as 25KHz, pulse cycle frequency 15 times/ Second, 1200 meter per second of acoustic beam, liquid surface sound pressure level is 30 °, starts ultrasonic wave program, controls ultrasonic intensity, produces pear skin slurry Raw obvious vortex.Ultrasonication 60 minutes, obtain pear skin active component extract.By pear skin active component extract, use Circulating pump sets circulating pump conveying pressure as 0.8MPa, and liquid phase feed liquid is made to pass through the ultrafiltration of 100,000 dalton of molecular cut off Film removes solid phase impurity.Efflux after collecting ultrafiltration.
3) by above-mentioned efflux, at room temperature by D101 macroreticular resin chromatographic column, flow control 10cm/min, later Chromatographic column is cleaned with the distilled water of 5 column volumes, then is eluted with the ethanol water that volume ratio is 50%, elution is collected Liquid.Above-mentioned eluent is dried in vacuo, control drying temperature is 20 DEG C, vacuum degree 120Pa, until it is dry complete, as The plant polyphenol extract object C6 of extraction.Polyphenol content is measured in Folin-Ciocalteu method, is converted to relative to pear skin original The Unit Weight extracted amount (being shown in Table 1) of material.
Comparative example 5 extracts active constituent plant polyphenol from fruit pear skin
1) exocarp of fresh anli pear (Pyrus ussuriensis Maxim) fruit is taken, silt, residual leaf, corruption are removed Equal sundries, are put into rinse bath, three times with clean tap water cleaning, add deionized water cleaning once, pull out and drain the water Point, obtain pear skin.Start meat grinder, pear skin is all rubbed, the pear skin after rubbing is collected in stainless steel barrel, and 3 times of weight are added , it is final concentration of that quality is added with glacial acetic acid adjustment endpoint pH for 4 than the ethanol water for 60% in volumetric concentration 0.08% Vc, the composite plant hydrolase of quality final concentration of 1%, is thoroughly mixed, and forms broken pear skin mixed liquor.It opens Dynamic colloid mill, setting fineness are 200 mesh, and the feeding inlet that broken pear skin mixed liquor gradually puts into colloid mill is ground, and are exported Feed liquid ground repeatedly with the same manner again once, be always co-mulled and made into twice, finally ground after pear skin slurry.
2) the pear skin slurry prepared is inputted in vacuum ultrasonic reaction kettle, is evacuated to 100Pa, control temperature in the kettle 15 DEG C, the power for adjusting ultrasonic transmitter is 450W, sets ultrasonic wave tranmitting frequency as 25KHz, pulse cycle frequency 15 times/ Second, 1200 meter per second of acoustic beam, liquid surface sound pressure level is 30 °, starts ultrasonic wave program, controls ultrasonic intensity, produces pear skin slurry Raw obvious vortex.Ultrasonication 60 minutes, obtain pear skin active component extract.By pear skin active component extract, use Circulating pump sets circulating pump conveying pressure as 0.8MPa, and liquid phase feed liquid is made to pass through the ultrafiltration of 100,000 dalton of molecular cut off Film removes solid phase impurity.Efflux after collecting ultrafiltration.
3) by above-mentioned efflux, at room temperature by D101 macroreticular resin chromatographic column, flow control 10cm/min, later Chromatographic column is cleaned with the distilled water of 5 column volumes, then is eluted with the ethanol water that volume ratio is 50%, elution is collected Liquid.Above-mentioned eluent is dried in vacuo, control drying temperature is 20 DEG C, vacuum degree 120Pa, until it is dry complete, as The plant polyphenol extract object C8 of extraction.Polyphenol content is measured in Folin-Ciocalteu method, is converted to relative to pear skin original The Unit Weight extracted amount (being shown in Table 1) of material.
Comparative example 6 extracts active constituent plant polyphenol from fruit pear skin
1) exocarp of fresh anli pear (Pyrus ussuriensis Maxim) fruit is taken, silt, residual leaf, corruption are removed Equal sundries, are put into rinse bath, three times with clean tap water cleaning, add deionized water cleaning once, pull out and drain the water Point, obtain pear skin.Start meat grinder, pear skin is all rubbed, the pear skin after rubbing is collected in stainless steel barrel, and 3 times of weight are added , it is final concentration of that quality is added with glacial acetic acid adjustment endpoint pH for 4 than the ethanol water for 60% in volumetric concentration 0.08% Vc, the composite plant hydrolase of quality final concentration of 3%, is thoroughly mixed, and forms broken pear skin mixed liquor.It opens Dynamic colloid mill, setting fineness are 200 mesh, and the feeding inlet that broken pear skin mixed liquor gradually puts into colloid mill is ground, and are exported Feed liquid ground repeatedly with the same manner again once, be always co-mulled and made into twice, finally ground after pear skin slurry.
2) the pear skin slurry prepared is inputted in vacuum ultrasonic reaction kettle, is evacuated to 150Pa, control temperature in the kettle 15 DEG C, the power for adjusting ultrasonic transmitter is 450W, sets ultrasonic wave tranmitting frequency as 25KHz, pulse cycle frequency 15 times/ Second, 1200 meter per second of acoustic beam, liquid surface sound pressure level is 30 °, starts ultrasonic wave program, controls ultrasonic intensity, produces pear skin slurry Raw obvious vortex.Ultrasonication 60 minutes, obtain pear skin active component extract.By pear skin active component extract, use Circulating pump sets circulating pump conveying pressure as 0.8MPa, and liquid phase feed liquid is made to pass through the ultrafiltration of 100,000 dalton of molecular cut off Film removes solid phase impurity.Efflux after collecting ultrafiltration.
3) by above-mentioned efflux, at room temperature by D101 macroreticular resin chromatographic column, flow control 10cm/min, later Chromatographic column is cleaned with the distilled water of 5 column volumes, then is eluted with the ethanol water that volume ratio is 50%, elution is collected Liquid.Above-mentioned eluent is dried in vacuo, control drying temperature is 20 DEG C, vacuum degree 120Pa, until it is dry complete, as The plant polyphenol extract object C10 of extraction.Polyphenol content is measured in Folin-Ciocalteu method, is converted to relative to pear skin The Unit Weight extracted amount (being shown in Table 1) of raw material.
Comparative example 7 extracts active constituent plant polyphenol from fruit pear skin
1) exocarp of fresh anli pear (Pyrus ussuriensis Maxim) fruit is taken, silt, residual leaf, corruption are removed Equal sundries, are put into rinse bath, three times with clean tap water cleaning, add deionized water cleaning once, pull out and drain the water Point, obtain pear skin.Start meat grinder, pear skin is all rubbed, the pear skin after rubbing is collected in stainless steel barrel, and 3 times of weight are added , it is final concentration of that quality is added with glacial acetic acid adjustment endpoint pH for 4 than the ethanol water for 60% in volumetric concentration 0.08% Vc, the composite plant hydrolase of quality final concentration of 3%, is thoroughly mixed, and forms broken pear skin mixed liquor.It opens Dynamic colloid mill, setting fineness are 200 mesh, and the feeding inlet that broken pear skin mixed liquor gradually puts into colloid mill is ground, and are exported Feed liquid ground repeatedly with the same manner again once, be always co-mulled and made into twice, finally ground after pear skin slurry.
2) the pear skin slurry prepared is inputted in vacuum ultrasonic reaction kettle, is evacuated to 100Pa, control temperature in the kettle 25 DEG C, the power for adjusting ultrasonic transmitter is 450W, sets ultrasonic wave tranmitting frequency as 25KHz, pulse cycle frequency 15 times/ Second, 1200 meter per second of acoustic beam, liquid surface sound pressure level is 30 °, starts ultrasonic wave program, controls ultrasonic intensity, produces pear skin slurry Raw obvious vortex.Ultrasonication 60 minutes, obtain pear skin active component extract.By pear skin active component extract, use Circulating pump sets circulating pump conveying pressure as 0.8MPa, and liquid phase feed liquid is made to pass through the ultrafiltration of 100,000 dalton of molecular cut off Film removes solid phase impurity.Efflux after collecting ultrafiltration.
3) by above-mentioned efflux, at room temperature by D101 macroreticular resin chromatographic column, flow control 10cm/min, later Chromatographic column is cleaned with the distilled water of 5 column volumes, then is eluted with the ethanol water that volume ratio is 50%, elution is collected Liquid.Above-mentioned eluent is dried in vacuo, control drying temperature is 20 DEG C, vacuum degree 120Pa, until it is dry complete, as The plant polyphenol extract object C12 of extraction.Polyphenol content is measured in Folin-Ciocalteu method, is converted to relative to pear skin The Unit Weight extracted amount (being shown in Table 1) of raw material.
Comparative example 8 extracts active constituent plant polyphenol from fruit pear skin
1) exocarp of fresh anli pear (Pyrus ussuriensis Maxim) fruit is taken, silt, residual leaf, corruption are removed Equal sundries, are put into rinse bath, three times with clean tap water cleaning, add deionized water cleaning once, pull out and drain the water Point, obtain pear skin.Start meat grinder, pear skin is all rubbed, the pear skin after rubbing is collected in stainless steel barrel, and 3 times of weight are added , it is final concentration of that quality is added with glacial acetic acid adjustment endpoint pH for 4 than the ethanol water for 60% in volumetric concentration 0.08% Vc, the composite plant hydrolase of quality final concentration of 3%, is thoroughly mixed, and forms broken pear skin mixed liquor.It opens Dynamic colloid mill, setting fineness are 200 mesh, and the feeding inlet that broken pear skin mixed liquor gradually puts into colloid mill is ground, and are exported Feed liquid ground repeatedly with the same manner again once, be always co-mulled and made into twice, finally ground after pear skin slurry.
2) the pear skin slurry prepared is inputted in vacuum ultrasonic reaction kettle, is evacuated to 100Pa, control temperature in the kettle 30 DEG C, the power for adjusting ultrasonic transmitter is 450W, sets ultrasonic wave tranmitting frequency as 25KHz, pulse cycle frequency 15 times/ Second, 1200 meter per second of acoustic beam, liquid surface sound pressure level is 30 °, starts ultrasonic wave program, controls ultrasonic intensity, produces pear skin slurry Raw obvious vortex.Ultrasonication 30 minutes, obtain pear skin active component extract.By pear skin active component extract, use Circulating pump sets circulating pump conveying pressure as 0.8MPa, and liquid phase feed liquid is made to pass through the ultrafiltration of 100,000 dalton of molecular cut off Film removes solid phase impurity.Efflux after collecting ultrafiltration.
3) by above-mentioned efflux, at room temperature by D101 macroreticular resin chromatographic column, flow control 10cm/min, later Chromatographic column is cleaned with the distilled water of 5 column volumes, then is eluted with the ethanol water that volume ratio is 50%, elution is collected Liquid.Above-mentioned eluent is dried in vacuo, control drying temperature is 20 DEG C, vacuum degree 120Pa, until it is dry complete, as The plant polyphenol extract object C14 of extraction.Polyphenol content is measured in Folin-Ciocalteu method, is converted to relative to pear skin The Unit Weight extracted amount (being shown in Table 1) of raw material.
Comparative example 9 extracts active constituent plant polyphenol from fruit pear skin
1) exocarp of fresh anli pear (Pyrus ussuriensis Maxim) fruit is taken, silt, residual leaf, corruption are removed Equal sundries, are put into rinse bath, three times with clean tap water cleaning, add deionized water cleaning once, pull out and drain the water Point, obtain pear skin.Start meat grinder, pear skin is all rubbed, the pear skin after rubbing is collected in stainless steel barrel, and 3 times of weight are added , it is final concentration of that quality is added with glacial acetic acid adjustment endpoint pH for 4 than the ethanol water for 60% in volumetric concentration 0.08% Vc, the composite plant hydrolase of quality final concentration of 3%, is thoroughly mixed, and forms broken pear skin mixed liquor.It opens Dynamic colloid mill, setting fineness are 200 mesh, and the feeding inlet that broken pear skin mixed liquor gradually puts into colloid mill is ground, and are exported Feed liquid ground repeatedly with the same manner again once, be always co-mulled and made into twice, finally ground after pear skin slurry.
2) the pear skin slurry that will be prepared is set circulating pump conveying pressure as 0.8MPa, is made liquid phase feed liquid using circulating pump It is the ultrafiltration membrane of 100,000 dalton by molecular cut off, removes solid phase impurity.Efflux after collecting ultrafiltration.
3) by above-mentioned efflux, at room temperature by D101 macroreticular resin chromatographic column, flow control 10cm/min, later Chromatographic column is cleaned with the distilled water of 5 column volumes, then is eluted with the ethanol water that volume ratio is 50%, elution is collected Liquid.Above-mentioned eluent is dried in vacuo, control drying temperature is 20 DEG C, vacuum degree 120Pa, until it is dry complete, as The plant polyphenol extract object C3 of extraction.Polyphenol content is measured in Folin-Ciocalteu method, is converted to relative to pear skin original The Unit Weight extracted amount (being shown in Table 1) of material.
Effect example 1: the product that above-described embodiment 1-11 and comparative example 1-9 are extracted carries out comparision contents, than It relatively the results are shown in Table 1.
Table 1 extracts the content balance of plant polyphenol using embodiment 1-11 and comparative example 1-9 method from pear skin
From 1 disclosure of table: according to the extraction conditions of embodiment 1-5, the extract plant polyphenol being prepared Content is higher, and the plant polyphenol that every gram of pear skin is extracted is up to 25.78-32.14mg.
1 condition of comparative example is compared with highest 2 condition of embodiment of recovery rate, and only extracting solution concentration of alcohol is become from 60% 30% difference, but extraction efficiency is decreased obviously；
2 condition of comparative example is compared with highest 2 condition of embodiment of recovery rate, and only extracting solution concentration of alcohol is become from 60% 80% difference, extraction efficiency are decreased obviously, although decline is strong not as good as 30% concentration, but excessive ethyl alcohol is unfavorable for improving Recovery rate, and excessive ethyl alcohol causes increased costs；
3 condition of comparative example compared with highest 2 condition of embodiment of recovery rate, only extracting solution pH from 4 become 6 difference, But extraction efficiency is decreased obviously；
4 condition of comparative example is compared with highest 2 condition of embodiment of recovery rate, and only extracting solution VC content is become from 0.08% 0.03% difference, but extraction efficiency is decreased obviously；
5 condition of comparative example is compared with highest 2 condition of embodiment of recovery rate, and only extracting solution complex enzyme content is become by 3% For 1% difference, but extraction efficiency is decreased obviously；
Compared with highest 2 condition of embodiment of recovery rate, only sonic vacuum degree is become 6 condition of comparative example from 100Pa The difference of 150Pa, but extraction efficiency is decreased obviously；
7 condition of comparative example is compared with highest 2 condition of embodiment of recovery rate, and only ultrasonic temperature becomes 25 DEG C from 15 DEG C Difference, but extraction efficiency is decreased obviously；
8 condition of comparative example is compared with highest 2 condition of embodiment of recovery rate, and only ultrasonic time became 30 points from 60 minutes The difference of clock, but extraction efficiency is decreased obviously.

Claims (10)

1. a kind of preparation method of the extract containing plant polyphenol comprising following steps:
(1) pear skin, solvent, composite plant hydrolase, pH adjusting agent and antioxidant are mixed into obtain mixture A, the mixture A PH be 2-5；
(2) by step (1) the mixture A vacuum ultrasonic, filter to get filtrate B；
(3) by liquor B described in step (2) through macroporous resin adsorption, elution, freeze-drying；
In step (1), the solvent is ethanol water；The concentration of the ethanol water is 40-70%, and the percentage is Mass percent of the ethyl alcohol in ethanol water；The dosage of the composite plant hydrolase is the percentage not less than 2% For mass percent of the composite plant hydrolase in the mixture A；The dosage of the antioxidant is not low In 0.05%, the percentage refers to mass percent of the antioxidant in the mixture A；
In step (2), the vacuum ultrasonic is in ultrasonic in vacuum ultrasonic reaction kettle；Wherein, the vacuum degree of the ultrasound is 60Pa-120Pa；The temperature of the reaction kettle is 8 DEG C -20 DEG C；The time of the ultrasound is not to be shorter than 40min.
2. preparation method as described in claim 1, which is characterized in that in step (1),
The pear skin is derived from anli pear；
And/or the concentration of the ethanol water is 45%-60%, the percentage is matter of the ethyl alcohol in ethanol water Measure percentage；
And/or the pear skin and the mass volume ratio of the solvent can be 1/3 (kg/L)；
And/or the composite plant hydrolase is cellulase and/or pectase；
And/or the dosage of the composite plant hydrolase is 2%-5%, the percentage is the composite plant hydrolase Mass percent in the mixture A；
And/or the pH adjusting agent is one of hydrochloric acid, phosphoric acid, nitric acid, sulfuric acid, glacial acetic acid or a variety of；
And/or the dosage of the pH adjusting agent is the pH 2-5 for making the mixture A；
And/or the antioxidant in vitamin C, vitamin E, lycopene, astaxanthin, grape seed extract one Kind is a variety of；
And/or the dosage of the antioxidant is 0.05-0.15%, the percentage refers to the antioxidant described mixed Close the mass percent in object A.
3. preparation method as claimed in claim 2, which is characterized in that in step (1),
The concentration of the ethanol water is 50%, and the percentage is mass percent of the ethyl alcohol in ethanol water；
And/or the dosage of the composite plant hydrolase is 3%-4%, the percentage is the composite plant hydrolase Mass percent in the mixture A；
And/or the pH adjusting agent is glacial acetic acid；
And/or the dosage of the pH adjusting agent is the pH 2.5-4 for making the mixture A；
And/or the antioxidant is selected from vitamin C；
And/or the dosage of the antioxidant is 0.06%-0.10%, the percentage refers to the antioxidant described Mass percent in mixture A.
4. preparation method as claimed in claim 3, which is characterized in that in step (1),
The dosage of the composite plant hydrolase is 2.5%-3.5%, and the percentage is that the composite plant hydrolase exists Mass percent in the mixture A；
And/or the dosage of the pH adjusting agent is the pH 3-3.5 or 4.5 for making the mixture A；
And/or the dosage of the antioxidant is 0.07%-0.08%, the percentage refers to the antioxidant described Mass percent in mixture A.
5. preparation method as described in claim 1, which is characterized in that in step (1),
It will be mixed again with the solvent, the pH adjusting agent and the antioxidant after pear skin pretreatment；Wherein, described pre- The mode of processing is preferably rubbed；
And/or after the mixing, also the mixture A is crushed；The preferred colloid mill of broken mode is broken；Institute It states broken degree and is preferably crushed to 200 mesh.
6. preparation method as described in claim 1, which is characterized in that in step (1),
Mixture A composite plant hydrolase, glacial acetic acid as described in the pear skin, 40-70% ethanol water, 2%-5% It is formed with the vitamin C of 0.05%-0.15%, the pH of the mixture A is 2-5；
Or, the mixture A is by the pear skin, 45-60% ethanol water, the 3.5% composite plant hydrolase, glacial acetic acid It is formed with the vitamin C of 0.06%-0.10%, the pH of the mixture A is 2.5-4；
Or, the mixture A by the pear skin, 60% ethanol water, the 3% composite plant hydrolase, glacial acetic acid and 0.08% vitamin C composition, the pH of the mixture A are 4.
7. preparation method as described in claim 1, which is characterized in that in step (2),
The vacuum degree of the ultrasound is 80Pa-100Pa；
And/or the temperature of the reaction kettle is 10 DEG C -15 DEG C；
And/or the power of the ultrasound is 300-600W；
And/or the tranmitting frequency of the ultrasound is 20-30KHz；
And/or the pulse cycle frequency of the ultrasound is 10-20 times/second；
And/or the velocity of sound of the ultrasound is 800-1600 meter per second；
And/or the liquid surface sound pressure level of the ultrasound is selected as 20-40 °；
And/or the time of the ultrasound is 40min-100min or 60min-80min.
8. preparation method as claimed in claim 7, which is characterized in that in step (2),
The condition of the vacuum ultrasonic are as follows: vacuum degree 80Pa-100Pa, 10 DEG C -15 DEG C of temperature, ultrasonic power 300-600W, transmitting Frequency 20-30KHz, the 10-20 times/second of pulse cycle frequency, velocity of sound 800-1600 meter per second, 20-40 ° of liquid surface sound pressure level and Ultrasonic time 40-100min；Or, vacuum degree 60Pa-120Pa, 8 DEG C -20 DEG C of temperature, ultrasonic power 300-600W, tranmitting frequency 20-30KHz, 10-20 times/second of pulse cycle frequency, velocity of sound 800-1600 meter per second, 20-40 ° of liquid surface sound pressure level and ultrasound Time 60-80min；
And/or the mixture A after the vacuum ultrasonic discharges through circulating pump, filtering；The pressure of the circulating pump is 0.5- 1MPa；The filtering uses ultrafiltration membrance filter, and the molecular cut off of the ultrafiltration membrane is ten thousand Dalton molecular weight of 5-15.
9. preparation method as described in claim 1, which is characterized in that in step (3),
The macroporous resin adsorption is that liquor B described in step (2) is carried out to macroporous resin adsorption, and the macroreticular resin is D101 Resin；
And/or the elution is eluted using ethyl alcohol, the concentration of the ethyl alcohol is 40-60%.
10. a kind of extract containing plant polyphenol being prepared by such as described in any item preparation methods of claim 1-9.
CN201811488503.2A 2018-12-06 2018-12-06 A kind of extract and preparation method thereof containing plant polyphenol Pending CN109691673A (en)

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