CN108452035A - A kind of extracting method of peony petal polyphenol - Google Patents

A kind of extracting method of peony petal polyphenol Download PDF

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CN108452035A
CN108452035A CN201810605376.3A CN201810605376A CN108452035A CN 108452035 A CN108452035 A CN 108452035A CN 201810605376 A CN201810605376 A CN 201810605376A CN 108452035 A CN108452035 A CN 108452035A
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polyphenol
petal
peony petal
peony
extracting method
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陈刚
马晓
陈雅君
罗青
王国霞
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Zhengzhou Normal University
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/65Paeoniaceae (Peony family), e.g. Chinese peony
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
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    • A61K2236/15Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K2236/17Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization

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Abstract

This application discloses a kind of extracting methods of peony petal polyphenol, including pretreatment of raw material, the extraction of polyphenol and thick liquid centrifugation step, peony petal is dried, powder processed, after sieving, the ethanol solution for taking peony petal fine powder to be 50~90% with volume fraction is uniformly mixed according to 30: 1~50: 1 liquid ratio, and peony petal fine powder and ethanol solution mixed liquor are placed in supersonic wave cleaning machine and carry out ultrasonic extraction, and petal is obtained after ultrasonic extraction and extracts thick liquid;Petal extraction crude-liquid filtering centrifuges up to polyphenolic extract;The recovery rate of the extracting method of the application peony petal polyphenol is high, it is that raw material extracts polyphenol active material to select the peony petal resource generally as waste, improve the output value of peony petal, further extend tree peony industrial chain, this method can be applied to industrialized production, method is reliable, has preferable application value.

Description

A kind of extracting method of peony petal polyphenol
Technical field
This application involves plant petals extractive technique field more particularly to a kind of extracting methods of peony petal polyphenol.
Background technology
Polyphenol be found in plant food, with it is potential promote health benefit bioactive substance polyphenol have Stronger anti-oxidation efficacy adjusts endocrine confusion, boosts metabolism, improves cardiovascular and cerebrovascular, slow down aging etc., to chronic disease With preferable prevention effect.
For the utilization of tree peony plant tree peony is also often used other than its root skin (moutan bark) is a kind of important Chinese medicine Seed makes peony seed oil or peony essential oil, the rest part of tree peony plant, as tree peony root, stem, leaf, petal are used as waste more Directly abandon;But in fact, equally contain polyphenol in the root, stem, leaf, petal of tree peony, annual a large amount of tree peony roots, stem, leaf, flower it is straight Discarding is connect, undoubtedly a kind of waste of resource.
Ultrasound assisted extraction technique is the fortune for increasing medium molecule using the mechanical effect, cavitation effect and fuel factor of ultrasonic wave Dynamic speed, increases the penetration power of medium to extract biological effective components, with common solvent extraction, supercritical extract and high pressure Rapid extraction technology is compared, and ultrasonic extraction has the spies such as easy to operate, safe, at low cost, extraction time is short, recovery rate is high Point, at present extensive utilization to various plants for example grape, pomegranate, apple, Chinese chestnut specific organization's polyphenol extraction.
Response phase method is that a kind of optimization of maturation several factors are combined to reach the maximized common method of response, Has preferable application in the Optimized Extraction Process research of the polyphenol such as dandelion, Ramulus Juglandis, Radix Notoginseng, cape jasmine.
' Feng Dan ' tree peony is to squeeze one of common kind of peony seed oil.
The polyphenol of plant extracts, and what is mostly used is the method for the ethyl alcohol extracted many times in thermostat water bath, when having extraction Between long, the features such as recovery rate is low.
Invention content
The object of the present invention is to provide a kind of safe operation, extraction time is short, recovery rate is high peony petal polyphenol to carry Take method.
To achieve the above object, technical solution used by the application is:
A kind of extracting method of peony petal polyphenol, the extracting method of the peony petal polyphenol include the following steps:
Pretreatment of raw material:It takes peony petal to be placed in 80 DEG C of thermostatic drying chambers after drying to constant weight, takes described after drying Peony petal is milled into peony petal coarse powder through cyclone type crushing mill, sieves with 100 mesh sieve the peony petal coarse powder to obtain tree peony Petal fine powder saves backup after sealing the peony petal fine powder shading in 4 DEG C of refrigerators;
Polyphenol extracts:It is 50~90% by the peony petal fine powder obtained in feed pretreatment step and volume fraction Ethanol solution according to 30: 1~50: 1 liquid ratio (mL/g) in container after mixing, will be equipped with peony petal fine powder with The container of ethanol solution mixed liquor, which is placed in supersonic wave cleaning machine, carries out ultrasonic extraction, and ultrasonic time is 5~65 minutes, ultrasound temperature Degree is 25~50 DEG C, and ultrasonic power is 60~100W, and petal is obtained after ultrasonic extraction and extracts thick liquid;
Thick liquid centrifugation:It is transferred to centrifuge tube after the petal obtained in polyphenol extraction step is extracted crude-liquid filtering, it will The centrifuge tube that thick liquid is extracted equipped with the petal is put into centrifuge and is centrifuged, and takes the supernatant of the petal crude extract after centrifugation Obtain polyphenolic extract.
Further, in a kind of extracting method of peony petal polyphenol, the second for the use of volume fraction being 70~90% Alcoholic solution extracts the peony petal fine powder.
Further, in a kind of extracting method of peony petal polyphenol, the second for the use of volume fraction being 60~70% Alcoholic solution extracts the peony petal fine powder.
Further, in a kind of extracting method of peony petal polyphenol, the ethyl alcohol for the use of volume fraction being 63% is molten Liquid extracts the peony petal fine powder.
Further, in a kind of extracting method of peony petal polyphenol, the peony petal fine powder and ethyl alcohol is molten Liquid is mixed according to 40: 1~50: 1 liquid ratio (mL/g).
Further, in a kind of extracting method of peony petal polyphenol, the peony petal fine powder and ethyl alcohol is molten Liquid is mixed according to 43: 1 liquid ratio (mL/g).
Further, in a kind of extracting method of peony petal polyphenol, the peony petal fine powder and ethyl alcohol is molten Liquid is mixed according to 40: 1 liquid ratio (mL/g).
Further, in a kind of extracting method of peony petal polyphenol, the ultrasonic time is 30~40 minutes.
Further, in a kind of extracting method of peony petal polyphenol, the ultrasonic time is 30 minutes.
Further, in a kind of extracting method of peony petal polyphenol, the ultrasonic time is 35 minutes.
Further, in a kind of extracting method of peony petal polyphenol, the ultrasonic temperature is 50 DEG C.
Further, in a kind of extracting method of peony petal polyphenol, the ultrasonic power is 70~80W.
Further, in a kind of extracting method of peony petal polyphenol, the ultrasonic power is 72W.
Further, in a kind of extracting method of peony petal polyphenol, the peony petal fine powder and ethanol solution Mixed liquid ratio 43.05: 1mL/g, ultrasonic time are 29.9 minutes, ultrasonic power 71.5W, volume fraction of ethanol 62.9%, ultrasonic temperature is 50 DEG C.
Further, in a kind of extracting method of peony petal polyphenol, the peony petal fine powder and ethanol solution Mixed liquid ratio is 43: 1mL/g, and ultrasonic time is 30 minutes, ultrasonic power 72W, volume fraction of ethanol 63%, ultrasound Temperature is 50 DEG C.
Further, a kind of extracting method of peony petal polyphenol further includes crude extract concentration step:Polyphenol is thick Extract is concentrated with Rotary Evaporators, is removed solvent, is obtained polyphenol concentrate.
The application has the following effects that:
The present invention extracts polyphenol, preferably extracting parameter using ultrasonic wave assisted extraction method, and recovery rate is high;Select general make Peony petal resource for waste is raw material extraction polyphenol active material, improves the output value of peony petal, further extends Tree peony industrial chain, realizes agricultural production and gardening watches the recycling of waste.
For the extracting method of peony petal polyphenol of the present invention by verification, extraction is reliable, can be applied to industrialized production, produces Required reagent is few with equipment, and production cost is low, and using ethanol solution as extracting solution, reagent safety has preferable application Value.
' Feng Dan ' tree peony is to squeeze one of common kind of peony seed oil, and the present invention selects ' Feng Dan ' tree peony as raw material, Adequately theoretical and data support is provided for the high efficiency of polyphenol in ' Feng Dan ' peony petal in production, is taken in the present invention The response surface model quadratic regression equation of the technological parameter and foundation that obtain extracts processor for tree peony or laboratory is directly joined According to using, R&D costs are reduced, accelerate research and development progress.
Specific implementation mode
With reference to embodiment, the present invention is described further.
Embodiment 1
A kind of extracting method of peony petal polyphenol, the extracting method of peony petal polyphenol include the following steps:
Pretreatment of raw material:It takes peony petal to be placed in 80 DEG C of thermostatic drying chambers after drying to constant weight, takes the tree peony after drying Petal is milled into peony petal coarse powder through cyclone type crushing mill, and peony petal coarse powder is sieved with 100 mesh sieve to obtain peony petal fine powder, After peony petal fine powder shading is sealed, saved backup in 4 DEG C of refrigerators;
Polyphenol extracts:The second for being 50~90% by the peony petal fine powder obtained in feed pretreatment step and volume fraction Alcoholic solution according to 30: 1~50: 1 liquid ratio (mL/g) in container after mixing, peony petal fine powder and ethyl alcohol will be housed The container of solution mixed liquor, which is placed in supersonic wave cleaning machine, carries out ultrasonic extraction, and ultrasonic time is 5~65 minutes, and ultrasonic temperature is 25~50 DEG C, ultrasonic power is 60~100W, and petal is obtained after ultrasonic extraction and extracts thick liquid;
Thick liquid centrifugation:The petal obtained in polyphenol extraction step is extracted into thick liquid and is transferred to centrifugation after quantitative filter paper filters Pipe, the centrifuge tube that thick liquid is extracted equipped with petal is put into centrifuge and is centrifuged, in 10000 revs/min 4 DEG C of centrifuge speed Under the conditions of lower centrifugation 10 minutes, take the supernatant of the petal crude extract after centrifugation to obtain polyphenolic extract.
Optionally, a kind of extracting method of peony petal polyphenol further includes crude extract concentration step:Thick liquid is centrifuged The polyphenolic extract obtained in step is concentrated with Rotary Evaporators, is removed solvent, is obtained polyphenol concentrate.
' Feng Dan ' peony petal polyphenol is extracted using the Parameter Conditions in the present embodiment 1, the polyphenol content of extraction For 43.13~51.64mg/g.
Embodiment 2
A kind of extracting method of peony petal polyphenol, peony petal polyphenol extracting method include the following steps:
Pretreatment of raw material:It takes peony petal to be placed in 80 DEG C of thermostatic drying chambers after drying to constant weight, takes the tree peony after drying Petal is milled into peony petal coarse powder through cyclone type crushing mill, and peony petal coarse powder is sieved with 100 mesh sieve to obtain peony petal fine powder, After peony petal fine powder shading is sealed, saved backup in 4 DEG C of refrigerators;
Polyphenol extracts:The second for being 70~90% by the peony petal fine powder obtained in feed pretreatment step and volume fraction Alcoholic solution according to 40: 1~50: 1 liquid ratio (mL/g) in container after mixing, peony petal fine powder and ethyl alcohol will be housed The container of solution mixed liquor, which is placed in supersonic wave cleaning machine, carries out ultrasonic extraction, and ultrasonic time is 30~40 minutes, ultrasonic temperature It it is 35~50 DEG C, ultrasonic power is 70~80W, and petal is obtained after ultrasonic extraction and extracts thick liquid;
Thick liquid centrifugation:The petal obtained in polyphenol extraction step is extracted into thick liquid and is transferred to centrifugation after quantitative filter paper filters Pipe, the centrifuge tube that thick liquid is extracted equipped with petal is put into centrifuge and is centrifuged, in 10000 revs/min 4 DEG C of centrifuge speed Under the conditions of lower centrifugation 10 minutes, take the supernatant of the petal crude extract after centrifugation to obtain polyphenolic extract.
' Feng Dan ' peony petal polyphenol is extracted using the Parameter Conditions in the present embodiment 2, the polyphenol content of extraction For 45.20~51.64mg/g.
Embodiment 3
A kind of extracting method of peony petal polyphenol, peony petal polyphenol extracting method include the following steps:
Pretreatment of raw material:It takes peony petal to be placed in 80 DEG C of thermostatic drying chambers after drying to constant weight, takes the tree peony after drying Petal is milled into peony petal coarse powder through cyclone type crushing mill, and peony petal coarse powder is sieved with 100 mesh sieve to obtain peony petal fine powder, After peony petal fine powder shading is sealed, saved backup in 4 DEG C of refrigerators;
Polyphenol extracts:The peony petal fine powder obtained in feed pretreatment step is molten for 70% ethyl alcohol with volume fraction Liquid according to 40: 1 liquid ratio (mL/g) in container after mixing, peony petal fine powder and ethanol solution mixed liquor will be housed Container be placed in supersonic wave cleaning machine and carry out ultrasonic extraction, ultrasonic time is 35 minutes, and ultrasonic temperature is 50 DEG C, ultrasonic power For 80W, petal is obtained after ultrasonic extraction and extracts thick liquid;
Thick liquid centrifugation:The petal obtained in polyphenol extraction step is extracted into thick liquid and is transferred to centrifugation after quantitative filter paper filters Pipe, the centrifuge tube that thick liquid is extracted equipped with petal is put into centrifuge and is centrifuged, in 10000 revs/min 4 DEG C of centrifuge speed Under the conditions of lower centrifugation 10 minutes, take the supernatant of the petal crude extract after centrifugation to obtain polyphenolic extract.
' Feng Dan ' peony petal polyphenol is extracted using the Parameter Conditions in the present embodiment 3, the polyphenol content of extraction For 47.71mg/g.
Embodiment 4
A kind of extracting method of peony petal polyphenol, peony petal polyphenol extracting method include the following steps:
Pretreatment of raw material:It takes peony petal to be placed in 80 DEG C of thermostatic drying chambers after drying to constant weight, takes the tree peony after drying Petal is milled into peony petal coarse powder through cyclone type crushing mill, and peony petal coarse powder is sieved with 100 mesh sieve to obtain peony petal fine powder, After peony petal fine powder shading is sealed, saved backup in 4 DEG C of refrigerators;
Polyphenol extracts:The peony petal fine powder obtained in feed pretreatment step is molten for 70% ethyl alcohol with volume fraction Liquid according to 50: 1 liquid ratio (mL/g) in container after mixing, peony petal fine powder and ethanol solution mixed liquor will be housed Container be placed in supersonic wave cleaning machine and carry out ultrasonic extraction, ultrasonic time is 35 minutes, and ultrasonic temperature is 50 DEG C, ultrasonic power For 80W, petal is obtained after ultrasonic extraction and extracts thick liquid;
Thick liquid centrifugation:The petal obtained in polyphenol extraction step is extracted into thick liquid and is transferred to centrifugation after quantitative filter paper filters Pipe, the centrifuge tube that thick liquid is extracted equipped with petal is put into centrifuge and is centrifuged, in 10000 revs/min 4 DEG C of centrifuge speed Under the conditions of lower centrifugation 10 minutes, take the supernatant of the petal crude extract after centrifugation to obtain polyphenolic extract.
' Feng Dan ' peony petal polyphenol is extracted using the Parameter Conditions in the present embodiment 4, the polyphenol content of extraction For 49.47mg/g.
Embodiment 5
A kind of extracting method of peony petal polyphenol, peony petal polyphenol extracting method include the following steps:
Pretreatment of raw material:It takes peony petal to be placed in 80 DEG C of thermostatic drying chambers after drying to constant weight, takes the tree peony after drying Petal is milled into peony petal coarse powder through cyclone type crushing mill, and peony petal coarse powder is sieved with 100 mesh sieve to obtain peony petal fine powder, After peony petal fine powder shading is sealed, saved backup in 4 DEG C of refrigerators;
Polyphenol extracts:The peony petal fine powder obtained in feed pretreatment step is molten for 70% ethyl alcohol with volume fraction Liquid according to 50: 1 liquid ratio (mL/g) in container after mixing, peony petal fine powder and ethanol solution mixed liquor will be housed Container be placed in supersonic wave cleaning machine and carry out ultrasonic extraction, ultrasonic time is 35 minutes, and ultrasonic temperature is 50 DEG C, ultrasonic power For 70W, petal is obtained after ultrasonic extraction and extracts thick liquid;
Thick liquid centrifugation:The petal obtained in polyphenol extraction step is extracted into thick liquid and is transferred to centrifugation after quantitative filter paper filters Pipe, the centrifuge tube that thick liquid is extracted equipped with petal is put into centrifuge and is centrifuged, in 10000 revs/min 4 DEG C of centrifuge speed Under the conditions of lower centrifugation 10 minutes, take the supernatant of the petal crude extract after centrifugation to obtain polyphenolic extract.
' Feng Dan ' peony petal polyphenol is extracted using the Parameter Conditions in the present embodiment 5, the polyphenol content of extraction For 51.64mg/g.
Embodiment 6
A kind of extracting method of peony petal polyphenol, peony petal polyphenol extracting method include the following steps:
Pretreatment of raw material:It takes peony petal to be placed in 80 DEG C of thermostatic drying chambers after drying to constant weight, takes the tree peony after drying Petal is milled into peony petal coarse powder through cyclone type crushing mill, and peony petal coarse powder is sieved with 100 mesh sieve to obtain peony petal fine powder, After peony petal fine powder shading is sealed, saved backup in 4 DEG C of refrigerators;
Polyphenol extracts:The second for being 60~70% by the peony petal fine powder obtained in feed pretreatment step and volume fraction Alcoholic solution according to 50: 1 liquid ratio (mL/g) in container after mixing, will be mixed with ethanol solution equipped with peony petal fine powder The container of conjunction liquid, which is placed in supersonic wave cleaning machine, carries out ultrasonic extraction, and ultrasonic time is 35 minutes, and ultrasonic temperature is 50 DEG C, ultrasound Power is 80W, and petal is obtained after ultrasonic extraction and extracts thick liquid;
Thick liquid centrifugation:The petal obtained in polyphenol extraction step is extracted into thick liquid and is transferred to centrifugation after quantitative filter paper filters Pipe, the centrifuge tube that thick liquid is extracted equipped with petal is put into centrifuge and is centrifuged, in 10000 revs/min 4 DEG C of centrifuge speed Under the conditions of lower centrifugation 10 minutes, take the supernatant of the petal crude extract after centrifugation to obtain polyphenolic extract;Preferably, this implementation In example, the volume fraction for the ethanol solution that peony petal polyphenol extracting method uses is 70%.
' Feng Dan ' peony petal polyphenol is extracted using the Parameter Conditions in the present embodiment 6, the polyphenol content of extraction For 51.73~51.95mg/g, when the volume fraction of ethanol solution is 70%, the polyphenol content of extraction is 51.95mg/g.
Embodiment 7
A kind of extracting method of peony petal polyphenol, peony petal polyphenol extracting method include the following steps:
Pretreatment of raw material:It takes peony petal to be placed in 80 DEG C of thermostatic drying chambers after drying to constant weight, takes the tree peony after drying Petal is milled into peony petal coarse powder through cyclone type crushing mill, and peony petal coarse powder is sieved with 100 mesh sieve to obtain peony petal fine powder, After peony petal fine powder shading is sealed, saved backup in 4 DEG C of refrigerators;
Polyphenol extracts:The peony petal fine powder obtained in feed pretreatment step is molten for 63% ethyl alcohol with volume fraction Liquid according to 43: 1 liquid ratio (mL/g) in container after mixing, peony petal fine powder and ethanol solution mixed liquor will be housed Container be placed in supersonic wave cleaning machine and carry out ultrasonic extraction, ultrasonic time is 30 minutes, and ultrasonic temperature is 50 DEG C, ultrasonic power For 72W, petal is obtained after ultrasonic extraction and extracts thick liquid;
Thick liquid centrifugation:The petal obtained in polyphenol extraction step is extracted into thick liquid and is transferred to centrifugation after quantitative filter paper filters Pipe, the centrifuge tube that thick liquid is extracted equipped with petal is put into centrifuge and is centrifuged, in 10000 revs/min 4 DEG C of centrifuge speed Under the conditions of lower centrifugation 10 minutes, take the supernatant of the petal crude extract after centrifugation to obtain polyphenolic extract.
' Feng Dan ' peony petal polyphenol is extracted using the Parameter Conditions in the present embodiment 7, the polyphenol content of extraction For 52.11 ± 1.75mg/g.
The extraction effect of the extracting method of peony petal polyphenol in order to further illustrate the present invention, using response phase method to this The extracting method of peony petal polyphenol is verified, and verification process is as follows:
Using liquid ratio, ultrasonic time, ultrasonic power and volume fraction of ethanol as independent variable, with ' Feng Dan ' tree peony polyphenol content For response, the horizontal response surface analysis experiment of 4 factor of design 3, the code levels of four factors are shown in Table 1.
1 independent variable factor of table encodes and level
According to the independent variable code levels of table 1, design response surface analysis experiment is shown in Table 2, totally 29 testing sites, wherein 5 Centered on point, experiment is repeated 5 times on the basis of each influence factor is zero level, it is other for estimating test error 24 testing sites are factorial point, for analyzing four A liquid ratios, B ultrasound sound time, C ultrasonic powers, D volume fraction of ethanol factors Influence to ' Feng Dan ' peony petal polyphenol content.
2 response surface experiments of table design and result
According to the data of table 2, establish using A, B, C, D as the even experiment design about polyphenol content Y of independent variable, 29 responses in table 2 are fitted with Design-Expert7.0 softwares, obtain following quadratic regression equation:
Y=51.632+1.622A-1.128B+1.839C+1.110D+0.012AB-0.984AC-0.3 02AD+0.929BC +0.140BD-0.029CD-1.130A2-1.370B2-2.967C2-1.514D2
Coefficient of determination R is returned known to regression equation fail-safe analysis2It is 0.9731, illustrates the response surface for having 97.31% Value meets this model, and experimental factor is affected, and correlation is high;Correct coefficient of determination R2 AdjIt is 0.9462, illustrates there is 94.62% Test data variation can be referred to this model;The signal-to-noise ratio of model is 20.664, is more than 4, equation is reasonable;Coefficient of variation CV It is 1.21%, numerical value is smaller, this equation has higher reliability and stability.
3 regression equation coefficient significance test of table
Note:* significant difference (p < 0.05) is indicated;* differences are extremely significantly (p < 0.01).
It can be obtained by table 3, extremely significantly (p < 0.01), it is 0.5806 not notable to lose quasi- item p value to the response surface model, shows this Equation has higher degree of fitting, and test error is small, the A in the first order and quadratic term of the equation2、B2、C2、D2Show Pole significant difference (p < 0.01), factor AC, BC difference is extremely notable (p < 0.01), not notable (the p > of AB, AD, BD, CD difference 0.05);By F values it is found that influence of four factors to ' Feng Dan ' peony petal polyphenol content is followed successively by C (ultrasonic power) > A (liquid Expect ratio) > B (ultrasonic time) > D (volume fraction of ethanol);To sum up this model has application value, can be used for analysis of experiments.
To the quadratic regression equation maximizing of foundation, the theory of ultrasound assisted extraction ' Feng Dan ' peony petal polyphenol is obtained Optimised process is:Liquid ratio 43.05: 1mL/g, ultrasonic time 29.9 minutes, ultrasonic power 71.5W, volume fraction of ethanol 62.9%;With this condition, the theoretical extraction of values of polyphenol is 52.621mg/g;Consider that actual conditions, adjustment above-mentioned parameter obtain The embodiment of the present invention 7, i.e. liquid ratio are 43: 1mL/g, and ultrasonic time is 30 minutes, ultrasonic power 72W, ethyl alcohol volume point Number is 63%, and carries out 5 parallel tests with this process conditions and verified, and the polyphenol content for measuring ' Feng Dan ' peony petal is 52.111 ± 1.752mg/g, the relative error with quadratic regression equation predicted value are 0.969%, therefore male in the present embodiment 7 The extracting method of red petal polyphenol is most preferred process in invention.
Simultaneously, it was demonstrated that the process conditions that response surface optimization obtains are accurate and reliable, can be further used for ' Feng Dan ' peony petal Polyphenol extraction prediction.
It should be noted that the measurement of polyphenol content uses in the present invention《Plant physiology experiment》(ISBN: 9787565506598) assay method of the polyphenol content described in page 133~page 135 is measured
Extracted amount according to the peony petal polyphenol of the present invention is as follows compared with the prior art:
In above table, the prior art is the Chinese patent of application number 201410040798.2《A kind of tree peony flower polyphenol Extraction process》.
By testing above, the extracting method of peony petal polyphenol, the recovery rate of peony petal polyphenol are aobvious according to the present invention It writes and is higher than the prior art;It is that raw material extracts polyphenol active material to select the peony petal resource generally as waste, is improved The output value of peony petal further extends tree peony industrial chain, realizes agricultural production and gardening watches the recycling of waste It utilizes.
For the extracting method of peony petal polyphenol of the present invention by verification, extraction is reliable, can be applied to industrialized production, produces Required reagent is few with equipment, and production cost is low, and using ethanol solution as extracting solution, reagent safety has preferable application Value.
' Feng Dan ' tree peony is to squeeze one of common kind of peony seed oil, and the present invention selects ' Feng Dan ' tree peony as raw material, Adequately theoretical and data support is provided for the high efficiency of polyphenol in ' Feng Dan ' peony petal in production, is taken in the present invention The response surface model quadratic regression equation of the technological parameter and foundation that obtain extracts processor for tree peony or laboratory is directly joined According to using, R&D costs are reduced, accelerate research and development progress.
More than, only the application preferred embodiment, not limiting the application, the common skill of any fields Art personnel within the spirit herein and principle made by all any modification, equivalent and improvement etc. should be included in the application Within the scope of being claimed.

Claims (10)

1. a kind of extracting method of peony petal polyphenol, including pretreatment of raw material, polyphenol extraction and thick liquid centrifugation step, feature It is:In polyphenol extraction step, by the peony petal fine powder obtained in pretreatment of raw material and volume fraction be 50~ 90% ethanol solution according to 30: 1~50: 1 liquid ratio (mL/g) after mixing, by peony petal fine powder and ethanol solution Mixed liquor, which is placed in supersonic wave cleaning machine, carries out ultrasonic extraction, and ultrasonic time is 5~65 minutes, and ultrasonic temperature is 25~50 DEG C, Ultrasonic power is 60~100W, and petal is obtained after ultrasonic extraction and extracts thick liquid.
2. a kind of extracting method of peony petal polyphenol according to claim 1, it is characterised in that:The peony petal is thin The liquid ratio of powder and ethanol solution is 40: 1~50: 1mL/g, and ultrasonic time is 30~40 minutes, and ultrasonic power is 70~80W, Volume fraction of ethanol is 70~90%.
3. a kind of extracting method of peony petal polyphenol according to claim 1, it is characterised in that:By the peony petal The liquid ratio (mL/g) that fine powder is mixed with ethanol solution is 43: 1.
4. a kind of extracting method of peony petal polyphenol according to claim 1, it is characterised in that:The ultrasonic time is 30 minutes or 35 minutes.
5. a kind of extracting method of peony petal polyphenol according to claim 1, it is characterised in that:A kind of peony In the extracting method of valve polyphenol, the ultrasonic power is 72W.
6. a kind of extracting method of peony petal polyphenol according to claim 1, it is characterised in that:The peony petal is thin The liquid ratio of powder and ethanol solution is 50: 1mL/g, and ultrasonic time is 35 minutes, ultrasonic power 70W, and volume fraction of ethanol is 70%, ultrasonic temperature is 50 DEG C.
7. a kind of extracting method of peony petal polyphenol according to claim 1, it is characterised in that:The peony petal is thin The liquid ratio of powder and ethanol solution is 50: 1mL/g, and ultrasonic time is 35 minutes, ultrasonic power 80W, and volume fraction of ethanol is 60~70%, ultrasonic temperature is 50 DEG C.
8. a kind of extracting method of peony petal polyphenol according to claim 1, it is characterised in that:The peony petal is thin The liquid ratio of powder and ethanol solution is 43: 1mL/g, and ultrasonic time is 30 minutes, ultrasonic power 72W, and volume fraction of ethanol is 63%, ultrasonic temperature is 50 DEG C.
9. a kind of extracting method of peony petal polyphenol according to claim 1, it is characterised in that:The thick liquid centrifugation step Centrifuge speed in rapid is 10000 revs/min, centrifuging temperature is 4 DEG C, centrifugation time is 10 minutes.
10. a kind of extracting method of peony petal polyphenol according to claim 1, it is characterised in that:The peony petal The extracting method of polyphenol further includes crude extract concentration step:Polyphenolic extract is concentrated with Rotary Evaporators, removes solvent, Obtain polyphenol concentrate.
CN201810605376.3A 2018-06-04 2018-06-04 A kind of extracting method of peony petal polyphenol Pending CN108452035A (en)

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CN115192638A (en) * 2022-08-31 2022-10-18 北京尚捷优蓝科技有限公司 Peony bloom antioxidant active site and preparation method and application thereof

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Publication number Priority date Publication date Assignee Title
CN115040567A (en) * 2022-05-24 2022-09-13 菏泽学院 Extraction method and application of polyphenol in peony
CN115192638A (en) * 2022-08-31 2022-10-18 北京尚捷优蓝科技有限公司 Peony bloom antioxidant active site and preparation method and application thereof
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Application publication date: 20180828