CN107692230A - Health products containing resveratrol and cyanidenon and its preparation method and application - Google Patents

Health products containing resveratrol and cyanidenon and its preparation method and application Download PDF

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Publication number
CN107692230A
CN107692230A CN201710946012.7A CN201710946012A CN107692230A CN 107692230 A CN107692230 A CN 107692230A CN 201710946012 A CN201710946012 A CN 201710946012A CN 107692230 A CN107692230 A CN 107692230A
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China
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resveratrol
cyanidenon
extract
health products
extraction
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Inventor
刘展眉
程杏安
蒋旭红
林贤伟
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Zhongkai University of Agriculture and Engineering
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Zhongkai University of Agriculture and Engineering
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Publication of CN107692230A publication Critical patent/CN107692230A/en
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/105Plant extracts, their artificial duplicates or their derivatives
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/02Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation containing fruit or vegetable juices
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/52Adding ingredients
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C37/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
    • C07C37/004Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by obtaining phenols from plant material or from animal material
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D311/00Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D311/04Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/22Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
    • C07D311/26Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
    • C07D311/28Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only
    • C07D311/30Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only not hydrogenated in the hetero ring, e.g. flavones
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D311/00Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D311/04Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/22Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
    • C07D311/26Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
    • C07D311/40Separation, e.g. from natural material; Purification
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

Abstract

The invention discloses a kind of health products containing resveratrol and cyanidenon and its preparation method and application.In the health products, including by resveratrol extract and the mixture of cyanidenon extract, especially the two is 1 according to mass ratio:The mixture of 1 composition, further obtains health products in good taste with cloudy mulberry juice, citric acid, D-sorbite and/or edible glycerol interworking.The health products not only have comprehensive healthcare function, have fragrance, and delicious taste, drink conveniently, meet consumer taste demand.

Description

Health products containing resveratrol and cyanidenon and its preparation method and application
Technical field
The present invention relates to health product technology field, in particular it relates to a kind of health products containing resveratrol and cyanidenon And its preparation method and application.
Background technology
Resveratrol is polyphenol compound, is mainly derived from the plants such as peanut, grape (red wine), giant knotweed, mulberry fruit. Resveratrol is a kind of biological very strong natural polyphenol class material, also known as resvertrol, is the chemopreventive agent of tumour, and To reducing platelet aggregation, prevention and treatment atherosclerosis, the chemopreventive agent of cardiovascular and cerebrovascular disease.United States Department of Agriculture Result of study shows that peanut red coat in benevolence with also containing considerable resveratrol.2014, scientist took in white lamb's-quarters to human body General mortality rate caused by the horizontal and various chronic disease of reed alcohol is researched and analysed, and is as a result found, dietary int ake resveratrol and Longevity, inflammation, cancer and cardiovascular health do not have obvious correlation.
Cyanidenon, it is present in more in the form of glucosides in various plants, these plants are with dragonhead, capsicum, mother chrysanthemum Flower, honeysuckle, purple perilla content are higher.With antibechic and phlegm-dispelling functions.According to current research, respiratory symptom cough, expectoration, asthma Breath, it is relevant with chronic airway inflammation.Such as bronchial astehma, COPD, chronic pharyngitis, allergic rhinitis are drawn Play cough, expectoration, pant, be all considered to, the presence of inflammation so that the immune response of air flue mix relevant with the inflammatory infiltration of part Disorderly, often there is airway reactivity and increased in patient.The means for the treatment of should eliminate the chronic inflammation infiltration of air flue first.It is conventional at present Glucocorticoid, to eliminate airway inflammation.But the side effect of glucocorticoid is more, unsuitable prolonged application.Research shows, sweet-scented osmanthus Careless element suppresses macrophage phosphorylation, suppresses transcription factor NF-kB activity, can suppress the macrophage of lipopolysaccharides (LPS) induction Cell cytokine production IL-6, TNF-a.In addition, research also indicate that, reseda be known as suppress uric acid generation into promote uric acid The effect of excretion.Latter two cell factor plays the part of very important role in inflammation mechanism, is the sensitivity for reflecting degree of inflammation Index.Cyanidenon can also improve IFN-γ, reduce specific Ig-E, reduce the infiltration of eosinophil.In addition, reseda Element also has in addition to anti-inflammatory, anti-allergic effects and suppresses PDE, anti-SARS, inhibition of HIV characteristic, the reason for this is that suppressing SARS diseases The activity of malicious Pre-S protein, so as to prevent it from entering host cell.For treat COPD, bronchial astehma and chronic pharyngitis, Chronic cough caused by allergic rhinitis etc..
As the improvement of people's living standards, its health care consciousness also gradually steps up, and in future, need of the people for health products Asking will be further urgent and strong.If using resveratrol and cyanidenon as main active component, it is prepared with guarantor The Foods or drinkses of strong effect, it will be expected to obtain the health products containing natural antioxidant, there is good development prospect.
Roots of Peanut, stem shell are the discarded object after autumn harvest again in China's wide material sources, as extraction resveratrol and wood The raw material of rhinoceros grass element, Yin Gen and stem had both been avoided to mitigate in giant knotweed, grape etc. again because useless burning causes a large amount of environmental pollutions The use pressure of medicinal material or fruits and vegetables.
The extraction process of existing resveratrol and cyanidenon there is no the resveratrol and sweet-scented osmanthus of high-purity, high activity Careless element, operation is more complicated, and recovery rate is also not high enough, limits the activity application of resveratrol and cyanidenon to a certain extent And the research application of relevant healthcare product.
The content of the invention
The technical problem to be solved in the present invention is the health products for the active component containing resveratrol and cyanidenon A kind of technical deficiency, there is provided health products containing resveratrol and cyanidenon.
Another technical problem to be solved by the present invention is that provide the preparation method of the health products.
A present invention also technical problems to be solved are to provide the application of the health products.
The purpose of the present invention is achieved by technical scheme once:
A kind of health products containing resveratrol and cyanidenon are provided, in the health products, including are extracted by resveratrol The mixture of thing and cyanidenon extract composition.
Preferably, in the health products, including by resveratrol extract and cyanidenon extract it is according to mass ratio 1:The mixture of 1 composition.
It is further preferred that in the health products, in addition to appropriate cloudy mulberry juice, citric acid, D-sorbite and/or edible Glycerine.
It is highly preferred that in the health products containing resveratrol and cyanidenon, by resveratrol extract, cyanidenon Extract, cloudy mulberry juice, citric acid, D-sorbite and edible glycerol are according to 0.075 part:0.075 part:30 parts:0.3 part:0.5 part: 0.5 part of mass ratio composition.
The preparation method of the health products is that each component mixing is shaken up into homogeneous to produce.
Preferably, the trans-resveratrol contained in the resveratrol extract is 0.083% or more.
Preferably, the preparation method of the resveratrol extract comprises the following steps:
S01. peanut rhizome is selected, is crushed;
S02. liquid ratio 25 is pressed:1 by crushing peanuts rhizome be immersed in concentration of volume percent be 65~75% it is edible In level ethanol, multiple lucifuge extraction, gained extract solution rotary evaporated to dryness, resveratrol extract is obtained.
Preferably, peanut rhizome described in step S01 is the rhizome of the peanut of Guangdong Zengcheng production.Further preferably it is planted in wide The rhizome of the peanut of eastern Zengcheng.
Preferably, it is to be crushed to 100 mesh sieves to be crushed described in step S01.
Preferably, the volume ratio percent concentration of ethanol described in step S02 is 70%.
Preferably, the temperature extracted described in step S02 is 50 DEG C, and each extraction time is 1h.
Preferably, step S02 is by liquid ratio 25:Crushing peanuts rhizome is immersed in concentration of volume percent as 65 by 1 In~75% food grade ethanol, then regulation system is extracted to faintly acid, then repeatedly.
It is further preferred that the pH value that the faintly acid is system is 4.8.
Further, the regulation system to faintly acid is to use concentration to be adjusted for 0.1mol/L hydrochloric acid solution Section.
The optimal extracting method of the resveratrol extract is prepared using extract by solvents, described ethanol Concentration of volume percent is 70%, liquid ratio 25:1, Extracting temperature:50 DEG C, extraction time 1h, carry out second extraction, time And 1h.Under the extraction conditions optimized herein, the recovery rate of resveratrol is 0.25%.
It is further preferred that the preparation method of the resveratrol extract also includes following purification step:
S03. resveratrol extract step S02 extracted, by methanol dissolving that may be less;
S04. the mixture after step S03 is dissolved is adsorbed with DA-201 macroreticular resins, then with 60%~100% Food grade ethanol resveratrol is eluted, collect various concentrations section eluent, rotary evaporation recovery eluant, eluent, obtain Resveratrol Primary purification product;
S05. by chromatographic column on resveratrol Primary purification product obtained by step S04, filler is compound adsorbent, is washed It is de-, eluent is collected, obtains resveratrol eluent;The preferred ZK-606 of compound adsorbent (molecularly imprinted polymer) and 400 The mixture of mesh silica gel (presses 1:1 mixing).
S06. after resveratrol eluent obtained by step S05 is concentrated, filtered after adding charcoal absorption, then use stone Oily ether carries out sorption extraction, collects petroleum ether extraction liquid, freeze-drying, obtains the resveratrol extract that purity is more than 98% Sterling.
Preferably, elution described in step S04 is that resveratrol is carried out with the ethanol that volume by volume concentration is 70%~100% Elution.
It is further preferred that it is tracked detection with thin-layer chromatography and high performance liquid chromatography during the elution.
Eluant, eluent described in step S05 is chloroform:The mixture of methanol different volumes ratio, chloroform:Methanol=2:1、3:1、 4:1、5:1、6:1、7:1 or 8:1;It is preferred that use chloroform:Methanol=5:1 mixture.Elution process thin-layer chromatography with efficiently Liquid chromatography is tracked detection.
Resveratrol purity after the eluent freeze-drying being prepared under the conditions of present invention extraction and purifying process For more than 98%.
Preferably, the preparation method of the cyanidenon extract comprises the following steps:
S11. using peanut shell as raw material, peanut shell is crushed;It is preferred that cross 50 mesh sieves;
S12. by the peanut shell that step S11 is crushed using 60%~80% food grade ethanol as extract solution, liquid ratio 25: 1, soak extraction 24h under conditions of being 4.8 in 80 DEG C, pH value, collect extract solution, and filter residue soaks 2~3h and carries out second extraction again Rotary evaporation.Produce cyanidenon extract.
Present invention determine that the optimal extraction process of cyanidenon is:The volumetric concentration of ethanol is 70%, pH value 4.8, Liquid ratio is 25:1, Extracting temperature:70 DEG C, extraction time 1h, carry out second extraction, time 1h.The recovery rate of cyanidenon For:0.20%.The superiority of present invention process is demonstrated with design orthogonal test through experiment of single factor.
It is further preferred that the preparation method of the cyanidenon extract also includes following purification step:
S13. cyanidenon extract step S12 extracted, by methanol dissolving that may be less;
S14. the mixture after step S13 is dissolved is adsorbed with DA-201 macroreticular resins, then with 60%~100% Food grade ethanol cyanidenon is eluted, collect various concentrations section eluent, rotary evaporation recovery eluant, eluent, obtain Cyanidenon Primary purification product;
Preferably, the peanut shell described in step S11 is the shell for the peanut for being planted in Guangdong Zengcheng.
It is that peanut shell powder was broken into 40~60 mesh sieves to be crushed described in step S11, preferably crosses 50 mesh sieves.
Preferably, elution described in step S14 is to reseda with the food grade ethanol that volume by volume concentration is 70%~100% Element is eluted.
It is further preferred that it is tracked detection with thin-layer chromatography and high performance liquid chromatography during the elution.
Cyanidenon purity after the eluent freeze-drying being prepared under the conditions of present invention extraction and purifying process For more than 40%.
In the health products containing resveratrol extract and cyanidenon extract, in the resveratrol extract The purity of resveratrol is 98% or more, and the purity of cyanidenon is 40% or more in the cyanidenon extract.
Also containing pros-and-cons type resveratrol, pros-and-cons type polydatin, cyanidenon in the health products.
The resveratrol extract and cyanidenon extract system being prepared using extraction preparation method of the present invention In standby health products, according to weight/mass percentage composition meter, containing formal resveratrol 0.0167%, trans-resveratrol 0.083%, and Cyanidenon 0.150%.
The beneficial effects of the invention are as follows:
The invention provides a kind of health products with health role (beverage), due to containing science ratio group in extract Into resveratrol and cyanidenon, the two plays good synergistic function, forms a kind of natural antioxidant, can be clear Except interior free yl, the anti-aging gene of activating human body, anti-aging, recover the normal function of physiology, antifatigue, the activating cell of strength Recover young vigor;Moreover, also containing cupreol in peanut rhizome extract, it has the obvious work(for reducing serum cholesterol Effect.It is sticky that health products of the present invention can reduce blood, suppresses coagulating platelets and vasodilation, keeps blood Channel Group, can be pre- The generation and development of anti-cancer.
Invention further provides the technical scheme of optimization, with resveratrol extract, cyanidenon extract, sorosis Juice, citric acid, D-sorbite, edible glycerol compatibility.Under the conditions of the technical scheme of optimization, the health products not only have comprehensive Healthcare function, and there is fragrance, delicious taste, drink conveniently, meet consumer taste demand.
On this basis, present invention optimizes the preparation method of resveratrol extract and cyanidenon extract, adopt Resveratrol extract and cyanidenon extract are prepared with extract by solvents, the process conditions of solvent extraction method is optimized, has Effect, which reduces, prepares cost, and obtains preferable recovery rate.
Present invention determine that optimal Extraction Process of Resveratrol From Ploygonum is:The volumetric concentration of ethanol is 70%, liquid ratio 25:1, Extracting temperature:50 DEG C, extraction time 1h, second extraction is carried out, the time is also 1h.The recovery rate of resveratrol is:0.25%.Through Experiment of single factor demonstrates the superiority of present invention process with design orthogonal test.
In terms of extraction, in order to improve recovery rate and under reducing the double effectses guaranteed conditions of production cost, the present invention Using the solvent extraction method of optimization, the recovery rate of resveratrol is 0.25%, and preparation process is simple, is also walked for subsequent purification Rapid simplification lays the first stone.In the crude separation of resveratrol, we are purified with DA-201 to the crude extract of resveratrol, In loading flow velocity 1.00mL/min, elution flow rate 1.60mL/min, volume fraction of ethanol 80%, its after purification resveratrol Rate is (83.13 ± 0.01) %, and 40% can be reached by detecting its purity through HPLC.In terms of using column chromatography purifying, the present invention Filler is compound adsorbent (ZK-606+400 mesh silica gel), is eluted, and collects eluent, obtains resveratrol eluent, is added Filtered after charcoal absorption, then sorption extraction is carried out with petroleum ether, collect petroleum ether extraction liquid, freeze-drying, obtaining purity is More than 98% resveratrol extract sterling, better assure that the beneficial effect of health products of the present invention.
Present invention determine that the optimal extraction process of cyanidenon is:The volumetric concentration of ethanol is 70%, pH value 4.8, Liquid ratio is 25:1, Extracting temperature:70 DEG C, extraction time 1h, carry out second extraction, time 1h.The recovery rate of cyanidenon For:0.20%.The superiority of present invention process is demonstrated with design orthogonal test through experiment of single factor.
Brief description of the drawings
The HPLC chromatogram of Fig. 1 resveratrol standard specimens.
The HPLC chromatogram of Fig. 2 Zengchengs peanut rhizome resveratrol extract.
The HPLC chromatogram of the resveratrol standard specimen of Fig. 3 embodiments 4.
The HPLC chromatogram of the resveratrol standard specimen of Fig. 4 ZhongKai Agriculture Engineering Academy general plantings.
Fig. 5 embodiment 5DA-201 macroporous resin adsorption results.
Fig. 6 embodiments 5 elute result.
The testing result of the gained resveratrol extract sterling of Fig. 7 embodiments 5.
The HPLC chromatogram of the cyanidenon standard specimen of Fig. 8 embodiments 6.
The HPLC chromatogram of the extract of the peanut shell of Fig. 9 Guangdong Zengcheng plantation.
The external anticancer of carry out of Figure 10 peanut rhizome resveratrol extracts and peanut shell cyanidenon extract mixtures Experimental result (blank and medication 24 hours).
The external anticancer of carry out of Figure 11 peanut rhizome resveratrol extracts and peanut shell cyanidenon extract mixtures Experimental result (blank and medication 48 hours).
The external anticancer of carry out of Figure 12 peanut rhizome resveratrol extracts and peanut shell cyanidenon extract mixtures Experimental result (blank and medication 72 hours).
Embodiment
The inventive method is further illustrated with reference to specific embodiment.Following being given for example only property of embodiment explanations, no It is understood that as limitation of the present invention.Unless stated otherwise, biomaterial, the reagent raw material used in following embodiments is conventional The biomaterial and reagent raw material that purchased in market or commercial sources obtain, unless stated otherwise, the method that is used in following embodiments and Equipment is method and apparatus commonly used in the art.
Embodiment 1
S01. the rhizome of the peanut of Guangdong Zengcheng plantation is selected, crushed after being dried crosses 100 mesh sieves;
S02. liquid ratio 25 is pressed:1 is immersed in crushing peanuts rhizome in 65% food grade ethanol, 50 DEG C of multiple lucifuges Extraction, extraction 1 hour, merges gained extract solution rotary evaporated to dryness, obtains resveratrol extract every time.
Embodiment 2
S01. the rhizome of the peanut of Guangdong Zengcheng plantation is selected, crushed after being dried crosses 100 mesh sieves;
S02. liquid ratio 25 is pressed:1 is immersed in crushing peanuts rhizome in 70% food grade ethanol, 50 DEG C of multiple lucifuges Extraction, extraction 1 hour, merges gained extract solution rotary evaporated to dryness, obtains resveratrol extract every time.
Embodiment 3
S01. the rhizome of the peanut of Guangdong Zengcheng plantation is selected, crushed after being dried crosses 50 mesh sieves;
S02. liquid ratio 25 is pressed:1 is immersed in crushing peanuts rhizome in 75% food grade ethanol, 50 DEG C of multiple lucifuges Extraction, extraction 1 hour, merges gained extract solution rotary evaporated to dryness, obtains resveratrol extract every time.
Any gained resveratrol extract of Example 1 to 3 carries out HPLC detections.Fig. 1 is resveratrol standard specimen HPLC chromatogram, Fig. 2 are the HPLC chromatogram that the present invention uses Zengcheng peanut rhizome resveratrol extract, as seen from the figure, this Resveratrol containing high level in invention extract.
Embodiment 4
S01. select general planting peanut rhizome (by ZhongKai Agriculture Engineering Academy plantation peanut exemplified by illustrate, but The species of peanut is not limited), crushed after being dried crosses 50 mesh sieves;
S02. liquid ratio 25 is pressed:1 is immersed in crushing peanuts rhizome the food grade second that concentration of volume percent is 70% In alcohol, 50 DEG C of multiple lucifuge extractions, extraction 1 hour, merges gained extract solution rotary evaporated to dryness, obtains resveratrol and carry every time Take thing.
The gained resveratrol extract of Example 4 carries out HPLC detections.Fig. 3 is the HPLC chromatogram of resveratrol standard specimen Figure, Fig. 4 are the HPLC chromatogram that the present embodiment uses Zengcheng peanut rhizome resveratrol extract.
Embodiment 5
S01. the rhizome of the peanut of Guangdong Zengcheng plantation is selected, crushed after being dried crosses 100 mesh sieves;
S02. liquid ratio 25 is pressed:1 is immersed in crushing peanuts rhizome in 70% food grade ethanol, 50 DEG C of multiple lucifuges Extraction, extraction 1 hour, merges gained extract solution rotary evaporated to dryness, obtains resveratrol extract every time;
S03. by S02 resveratrol extract rotary evaporated to dryness, dissolved with a small amount of methanol, be freeze-dried to doing, obtain Just extraction product;
S04. will just extract product obtained by step S03 to be adsorbed on macroreticular resin, macroreticular resin model used DA-201;Then gradient elution is carried out on macroreticular resin with 60%, 70%, 80%, 90%, 100% ethanol, eluent is used Thin-layered chromatography and high performance liquid chromatography are tracked, and collect the eluent of resveratrol section;By the solution of resveratrol section Concentration and recovery ethanol, obtain the resveratrol semi-finished product that content is 45% or so;Fig. 5 embodiment 5DA-201 macroporous resin adsorptions As a result as shown in accompanying drawing 5, elute shown in result as accompanying drawing 6.
S05. it is compound adsorbent (ZK-606+400 mesh silica gel) by chromatographic column on gained semi-finished product, filler, uses chlorine successively It is imitative:Methanol is 2:1、3:1、4:1、5:1、6:1、7:1、8:1 volume ratio is eluted, with thin-layered chromatography and high-efficient liquid phase color Spectrometry is tracked.Collect the eluent of resveratrol section.
S06. after resveratrol eluent obtained by step S05 is concentrated, filtered after adding charcoal absorption, then use stone Oily ether carries out sorption extraction, collects petroleum ether extraction liquid, freeze-drying, obtains the resveratrol extract that purity is more than 98% Sterling.Shown in testing result as accompanying drawing 7.
Embodiment 6
S11. the shell of the peanut of Guangdong Zengcheng plantation is selected, crushed after being dried crosses 50 mesh sieves;
S12. liquid ratio 25 is pressed:1 is immersed in crushing peanuts shell in 60% food grade ethanol, 60 DEG C of repeatedly extractions, Extraction 24 hours every time, merge gained extract solution rotary evaporated to dryness, obtain cyanidenon extract.
Embodiment 7
S11. the shell of the peanut of Guangdong Zengcheng plantation is selected, crushed after being dried crosses 50 mesh sieves;
S12. liquid ratio 25 is pressed:1 is immersed in crushing peanuts shell in 70% food grade ethanol, 60 DEG C of repeatedly extractions, Extraction 24 hours every time, merge gained extract solution rotary evaporated to dryness, obtain cyanidenon extract.
Embodiment 8
S11. the shell of the peanut of Guangdong Zengcheng plantation is selected, crushed after being dried crosses 50 mesh sieves;
S12. liquid ratio 25 is pressed:1 is immersed in crushing peanuts shell in 75% food grade ethanol, 60 DEG C of repeatedly extractions, Extraction 24 hours every time, merge gained extract solution rotary evaporated to dryness, obtain cyanidenon extract.
As shown in Figure 9, Fig. 8 is cyanidenon to the HPLC chromatogram of any gained cyanidenon extract of embodiment 6 to 8 The HPLC chromatogram of standard specimen.
Embodiment 9
S11. the shell of the peanut of selection selection general planting is (by taking the peanut of ZhongKai Agriculture Engineering Academy plantation as an example, but not Limit the species of peanut), crushed after being dried crosses 50 mesh sieves;
S12. liquid ratio 25 is pressed:1 is immersed in crushing peanuts shell in 100% food grade ethanol, 60 DEG C of repeatedly extractions, Extraction 24 hours every time, merge gained extract solution rotary evaporated to dryness, obtain cyanidenon extract.
Embodiment 10
S11. the shell of the peanut of Guangdong Zengcheng plantation is selected, crushed after being dried crosses 50 mesh sieves;
S12. liquid ratio 25 is pressed:1 is immersed in crushing peanuts shell in 70% food grade ethanol, 60 DEG C of repeatedly extractions, Extraction 24 hours every time, merge gained extract solution rotary evaporated to dryness, obtain cyanidenon extract;
S13. by S02 cyanidenon extract rotary evaporated to dryness, dissolved with a small amount of methanol, be freeze-dried to doing, obtain Just extraction product.
Embodiment 11
The present embodiment provides a kind of health products containing resveratrol and cyanidenon, in the health products, including following matter Measure each component of number:Resveratrol extract made from any example of Example 1 to 5, any example of Example 6 to 10 are made Cyanidenon extract, cloudy mulberry juice purchased in market, citric acid, D-sorbite, edible glycerol, according to the mass fraction shown in table 1 Formula rate, each component is mixed, shaken up, homogeneous produces.
Table 1
Embodiment 12
Detection product A~H's the results are shown in Table shown in 2.Select 10 subjective appreciation composition of personnel evaluation groups, it is desirable to which sense organ is commented Fix the number of workers 12h before evaluation does not drink, and non-smoking, does not eat pungent irritable food of Denging, and 2 samples will be gargled with clear water before and after evaluation Mouthful simultaneously it is spaced 10min, the mode such as taste using range estimation, nasil, mouth carries out subjective appreciation one by one, is allocated as, for optimal number, filling out with 10 Write results of sensory evaluation.Detection and results of sensory evaluation see the table below 2.
Table 2
Embodiment 13
According to mass fraction ratio it is 1 with peanut rhizome resveratrol extract and peanut shell cyanidenon extract:1 After ratio mixing, external anticancer experiment is carried out, it is found that extract plays the role of suppression to cell, as shown in Figure 10 to 12, has attached Scheme visible, cell quantity has obvious difference before and after dosing, a large amount of apoptosis of cell after dosing.
The preparation of the ZK-606 adsorbents of embodiment 14
Therefore the material and instrument that the present embodiment uses as shown in Table 3 and Table 4, but do not limit the scope of the invention.
The experimental drug table of table 3
The laboratory apparatus table of table 4
Molecularly imprinted polymer is prepared using precipitation polymerization method:
S1. a certain amount of template molecule resveratrol and function monomer methacrylic acid (MAA) are weighed, it is molten to be dissolved in methanol In agent;
S2. the cyclotron oscillation prepolymerization 1h in thermostatic control oscillator vibration, crosslinking agent GDMA is added (EGDMA) and 0.1g initiator azodiisobutyronitriles (AIBN), after ultrasonic deoxidation 10min, N is led to210min starvations, it is close Envelope, polymerize 24h in water bath with thermostatic control.
S3. polymer is taken out, the filtering of cloth funnel, dried.With V (methanol):V (acetic acid)=8:2 are used as eluent, rope Formula extracts a week, washes away template molecule, dries, that is, obtains resveratrol imprinted polymer (MIPs), be named as ZK-606. Under conditions of template molecule resveratrol is not added with, blank imprinted polymer (NIPs) is made in the same way.
30mg each 6 parts of ZK-606 (MIPs21) and NIPs21 is weighed respectively, and it is about the white of 1~8mmol/L to add concentration Veratryl alcohol methanol solution, cyclotron oscillation absorption 24h, surveys its adsorbance at room temperature.
ZK-606 Selective adsorption result of the test is shown in Table 4:
Adsorbances of the MIPs of table 4 from NIPs to different substrates

Claims (10)

1. a kind of health products containing resveratrol and cyanidenon, it is characterised in that in the health products, including by resveratrol The mixture of extract and cyanidenon extract composition.
2. the health products containing resveratrol and cyanidenon according to claim 1, it is characterised in that in the health products, Including according to mass ratio being 1 by resveratrol extract and cyanidenon extract:The mixture of 1 composition.
3. the health products according to claim 1 or claim 2 containing resveratrol and cyanidenon, it is characterised in that the health products In, in addition to appropriate cloudy mulberry juice, citric acid, D-sorbite and/or edible glycerol;It is preferred that
In the health products containing resveratrol and cyanidenon, by resveratrol extract, cyanidenon extract, sorosis Juice, citric acid, D-sorbite and edible glycerol are according to 0.075 part:0.075 part:30 parts:0.3 part:0.5 part:0.5 part of quality Than composition.
4. the health products containing resveratrol and cyanidenon according to any one of claims 1 to 3, it is characterised in that described The preparation method of resveratrol extract comprises the following steps:
S01. peanut rhizome is selected, is crushed, sieving;
S02. liquid ratio 25 is pressed:1 is immersed in crushing peanuts rhizome the food grade ethanol that concentration of volume percent is 65~75% In, multiple lucifuge extraction, gained extract solution rotary evaporated to dryness, obtain resveratrol extract.
5. the health products containing resveratrol and cyanidenon according to claim 4, it is characterised in that mistake described in step S01 Sieve was 100 mesh sieves;The concentration of volume percent of food grade ethanol described in step S02 is 70%.
6. the health products containing resveratrol and cyanidenon according to claim 4 or 5, it is characterised in that the white black false hellebore The preparation method of alcohol extracting thing is further comprising the steps of:
S03. resveratrol extract step S02 extracted, use methanol dissolving as few as possible;
S04. the mixture after step S03 is dissolved is adsorbed with DA-201 macroreticular resins, then with 60%~100% it is edible Level ethanol elutes to resveratrol, collects the eluent of various concentrations section, rotary evaporation recovery eluant, eluent, obtains white black false hellebore Alcohol Primary purification product;
S05. by chromatographic column on resveratrol Primary purification product obtained by step S04, filler is compound adsorbent resveratrol point Sub- imprinted polymer ZK-606 and 400 mesh silica-gel mixtures, are eluted, and are collected eluent, are obtained resveratrol eluent;
S06. after resveratrol eluent obtained by step S05 is concentrated, filtered after adding charcoal absorption, then use petroleum ether Sorption extraction is carried out, petroleum ether extraction liquid is collected, freeze-drying, obtains the resveratrol extract sterling that purity is more than 98%.
7. the health products containing resveratrol and cyanidenon according to any one of claims 1 to 3, it is characterised in that described The preparation method of cyanidenon extract comprises the following steps:
S11. using peanut shell as raw material, peanut shell is crushed, sieved;
S12. by the peanut shell that step S11 is crushed using 60%~80% food grade ethanol as extract solution, liquid ratio 25,80 DEG C, pH value be 4.8 under conditions of soak extraction, collect extract solution, filter residue soak again carry out second extraction rotary evaporation, produce wood Rhinoceros grass extract.
8. the health products containing resveratrol and cyanidenon according to claim 7, it is characterised in that mistake described in step S11 Sieve was 50 mesh sieves;The soak extraction time described in step S12 is 24 hours, and soak time is 2~3 hours to filter residue again.
9. the health products containing resveratrol and cyanidenon according to claim 7, it is characterised in that the resveratrol carries Take the preparation method of thing further comprising the steps of:
S13. cyanidenon extract step S12 extracted, use methanol dissolving as few as possible;
S14. the mixture after step S13 is dissolved is adsorbed with DA-201 macroreticular resins, then with 60%~100% it is edible Level ethanol elutes to cyanidenon, collects the eluent of various concentrations section, rotary evaporation recovery eluant, eluent, obtains reseda Plain Primary purification product.
10. the health products containing resveratrol and cyanidenon according to any one of claim 1 to 9, it is characterised in that described In health products, according to weight/mass percentage composition meter, containing formal resveratrol and glycosides 0.0167%, trans-resveratrol and glycosides 0.083% With the % of cyanidenon 0.150.
CN201710946012.7A 2017-10-10 2017-10-10 Health products containing resveratrol and cyanidenon and its preparation method and application Pending CN107692230A (en)

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