CN113383851A - Method for extracting peony protein isolate for oil - Google Patents

Method for extracting peony protein isolate for oil Download PDF

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CN113383851A
CN113383851A CN202110752411.6A CN202110752411A CN113383851A CN 113383851 A CN113383851 A CN 113383851A CN 202110752411 A CN202110752411 A CN 202110752411A CN 113383851 A CN113383851 A CN 113383851A
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oil
peony
protein
extraction
extracting
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CN113383851B (en
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袁文鹏
鹿杰
黄志强
王惠敏
赵雷振
魏永峰
程丹丹
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Heze Branch Of Shandong Academy Of Sciences
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23JPROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
    • A23J1/00Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites
    • A23J1/14Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from leguminous or other vegetable seeds; from press-cake or oil-bearing seeds
    • A23J1/142Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from leguminous or other vegetable seeds; from press-cake or oil-bearing seeds by extracting with organic solvents
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23JPROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
    • A23J1/00Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites
    • A23J1/14Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from leguminous or other vegetable seeds; from press-cake or oil-bearing seeds
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23JPROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
    • A23J3/00Working-up of proteins for foodstuffs
    • A23J3/14Vegetable proteins
    • 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

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  • Chemical & Material Sciences (AREA)
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Abstract

A method for extracting peony protein for oil comprises the following steps: the method comprises the following steps: shelling oil peony seeds, pressing cake or crushing peony seed meal (hydraulic pressure), granulating, and extracting butane at low temperature for 1-4 times to obtain defatted oil peony seed meal; step two: extracting the peony seed meal obtained in the step one with alcohol for 1-3 times to obtain peony seed meal without alcohol extract; step three: and D, carrying out alkali extraction on the peony seed meal without the alcohol extract obtained in the step two, carrying out acid precipitation on the supernatant obtained after the alkali extraction under the conditions of pH3-5 and time of 1-4 h, centrifuging, washing with water to be neutral, and carrying out spray drying to obtain the peony protein isolate for oil. According to the invention, butane is adopted for low-temperature extraction, so that the protein is prevented from being denatured under the action of high temperature, the content of oil and fat in the meal is reduced to the minimum, and the protein purity is improved; the peony pulp is treated by alcohol extraction, and the protein obtained by alkali extraction and acid precipitation is light yellow after the step, and is purple red if the step is not carried out; the extraction rate and purity of the protein can be highest under the alkali extraction and acid precipitation process, the extraction rate is 51.62 percent, and the purity is 94 percent.

Description

Method for extracting peony protein isolate for oil
Technical Field
The invention belongs to the research field of peony protein isolate, and particularly relates to a method for extracting peony protein isolate for oil.
Background
The oil peony mainly comprises paeonia ostii and paeonia rockii, and has the characteristics of large seed yield, high oil content, excellent quality, strong resistance and the like, 60-70% of peony cake meal is generated after oil is pressed from the oil peony seeds, and the peony cake meal contains abundant nutritional ingredients such as protein, polysaccharide, flavone and the like, wherein the protein content accounts for about 20-33% of the weight of the cake meal, the amino acid proportion is balanced, and the peony protein isolate has the functional characteristics of good water absorption, oil retention, emulsifying property, emulsion stability, foaming property, foam stability and the like, and is free of cholesterol, is easier to digest and absorb by a human body, has a liver function protection effect, is favorable for preventing cardiovascular diseases, and is a plant protein with high commercial development value.
The industrial production of vegetable protein is usually carried out by alkali extraction and acid precipitation, taking soybean protein as an example, the process is roughly as follows: soybean → pressing → defatted cake → alkali extraction → centrifugal separation → supernatant liquid to adjust pH to isoelectric point → centrifugal separation → precipitate water washing to neutrality → drying → protein. Alkali extraction and acid precipitation are the only way for extracting plant protein isolate, but the process methods are different, and the extracted and prepared protein isolate has great difference in purity, color, physicochemical properties and the like, which directly determines the quality of the protein isolate. At present, few reports about extraction of oil peony protein isolate are reported, and the problems of low quality of extracted protein isolate, difficulty in scale production, industrialization and the like exist in the existing method.
For example, CN108887461A discloses "peony seed protein and its extraction method", comprising the steps of: after the peony seeds are unshelled, separating shells and kernels, crushing and preheating the kernels, separating peony seed oil by using a supercritical extraction method, wherein the rest part is peony seed meal, drying and crushing the separated peony seed meal, adding distilled water in a certain mass ratio, homogenizing at a high speed, adding a NaOH solution to adjust the pH value to a proper value, stirring and leaching for a certain time at 40-60 ℃, centrifuging the leaching solution, collecting supernatant to obtain a peony protein solution, adjusting the pH value of the peony protein solution to acidity by using an HCl solution to obtain precipitated peony protein, centrifuging, washing to be neutral, and drying to obtain the peony seed protein. The method adopts the steps of separating shells from kernels, preheating the kernels, and separating peony seed oil by using a supercritical extraction method, wherein the method comprises the preheating treatment, and the preheating treatment is easy to generate local high temperature in large-scale implementation, so that protein is denatured; in addition, the supercritical extraction has limited treatment capacity, the treatment capacity of each batch is not more than 200kg, the production capacity is extremely limited, and the large-scale production cannot be realized.
CN110226664A discloses a method for preparing peony seed protein powder, which comprises the following steps: taking degreased peony seed cake powder as a raw material, mixing the pulp with alkaline oxidation potential water, and vacuumizing and soaking under negative pressure; ultrasonic low-temperature extraction; centrifugally separating the protein extracting solution from peony seed residues; taking supernatant, regulating the pH value to be near the isoelectric point of protein by hydrochloric acid; centrifuging to separate out protein; after washing, neutralizing and size mixing; spray drying to obtain the peony protein powder product. The method adopts alkaline oxidation potential water for size mixing, still adopts a mode of alkaline protein extraction, and is characterized in that vacuum pumping and negative pressure soaking are adopted, because peony protein isolate is dissolved under an alkaline condition, whether negative pressure is used has no direct influence on the protein extraction rate, and other impurities are mixed in the peony protein isolate when negative pressure is used for extracting seed meal, and the separated protein can adsorb other impurities in an acid precipitation process, so that the obtained protein isolate has low extraction rate and poor color, and the requirement of the market on high-quality protein isolate is difficult to meet.
Disclosure of Invention
The invention provides a method for extracting peony protein isolate for oil, which is used for overcoming the defects in the prior art.
The invention is realized by the following technical scheme:
a method for extracting peony protein isolate for oil comprises the following steps:
the method comprises the following steps: carrying out shelling, cake pressing or hydraulic treatment on oil peony seeds, crushing and granulating, and extracting for 1-4 times by using butane as an extracting agent under the conditions of pressure of 0.3-0.8 mpa and extraction temperature of 20-50 ℃ to obtain degreased oil peony seed meal with the oil content of less than or equal to 1.5%;
step two: and (2) carrying out treatment on the peony seed meal for the degreased oil obtained in the step one by using methanol or ethanol as a solvent, wherein the alcohol concentration is 50-95%, and the material-liquid ratio is 1: 5-1: 15, extracting for 1-3 times at the extraction temperature of 40-50 ℃ for 1-3 h to obtain the peony seed meal for the degreased oil without the alcohol extract;
step three: and (3) carrying out separation on the degreased oil without the alcohol extract obtained in the step two by using peony seed meal at the temperature of 30-50 ℃ and the material-liquid ratio of 1: 15-1: 25, performing alkali extraction at the pH of 10-11(0.005mol/L-0.01mol/L) for 2h-5h, centrifuging to obtain an alkali extraction supernatant, performing acid precipitation on the alkali extraction supernatant at the pH of 3-5 for 1h-4h, centrifuging, washing the obtained protein to neutrality, and performing spray drying to obtain the peony protein isolate for oil.
The method for extracting the peony protein isolate for oil comprises the step one, wherein the peony seed meal in the step one is the peony seed meal after shelling, cake pressing or hydraulic pressing.
The method for extracting peony protein for oil comprises the step two, wherein the alcohol extract obtained in the step two is an alcohol extract obtained after the solvent is volatilized, and the alcohol extract contains flavone and paeoniflorin.
The invention has the advantages that:
(1) the method adopts butane to extract the peony seeds or the peony seed meal at low temperature (hydraulic pressure), so that the method has the advantages of large one-time treatment capacity, low cost, realization of large-scale production and far better supercritical extraction method; secondly, low-temperature extraction is ensured, the protein property is intact and is not damaged, the twin-screw pressing method generates high temperature in the pressing process to denature the protein, the influence on the physicochemical property, the biochemical property and the like of the protein is great, although the hydraulic method has low temperature, the content of residual oil of the obtained degreased seed meal is still very high, and therefore, the residual oil still needs to be removed by butane low-temperature extraction.
(2) According to the invention, the peony seed meal is treated by methanol or ethanol, the obtained alcohol extract is brown yellow as shown in figure 2, and the components such as flavone and paeoniflorin are preliminarily analyzed. Through the step, the protein color after alkali extraction and acid precipitation is light yellow, if direct alkali extraction and acid precipitation is not carried out in the step, the obtained protein color is purple red (see figure 3), the step is a key step for removing the protein color which is discovered for the first time and is the greatest characteristic of the invention, and the obtained alcohol extract contains effective components such as flavone and paeoniflorin, and can be purified and used in other fields such as cosmetics and the like subsequently, so that the full utilization of resources is realized.
(3) At the alkali extraction temperature of 30-50 ℃, the alkali extraction time of 2-5 h, the ratio of alkali extraction liquid to base extraction liquid of 1: 15-1: 25, the pH value of alkali extraction is 10-11(0.005mol/L-0.01mol/L), the acid precipitation time is 1h-4h, the extraction rate and the purity of the protein can be highest under the process condition of the pH value of acid precipitation 3-5, the extraction rate is 51.62 percent, the purity is 94 percent, and the functional properties of protein water absorption, oil retention, emulsibility, emulsion stability, foamability, foam stability and the like are superior to those of the isolated soy protein.
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In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a process flow of the present invention for extracting the peony protein isolate for oil;
FIG. 2 is a picture of the alcohol extract obtained in the present invention;
in the left picture of FIG. 3, the oil peony protein isolate obtained by direct alkali extraction and acid precipitation without methanol or ethanol extraction is shown; the right picture is the peony protein isolate for oil obtained by the invention;
FIG. 4 shows the results of the acid precipitation time optimization according to the present invention;
FIG. 5 shows the pH optimization results of the acid precipitation according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the method comprises the following steps: crushing and granulating the hydraulic peony seed meal, and extracting for 2 times by using butane as an extracting agent under the conditions of the pressure of 0.4mpa and the extraction temperature of 40 ℃ to obtain the peony seed meal for the degreased oil with the oil content of 1.3 percent;
step two: and (2) carrying out treatment on the peony seed meal for the degreased oil obtained in the step one, wherein ethanol is used as a solvent, the concentration of the ethanol is 70%, and the material-liquid ratio is 1: 5, extracting for 2 times at the extraction temperature of 40 ℃ for 1h to obtain the peony seed meal for the degreased oil without the alcohol extract, wherein the yield of the alcohol extract is 10%;
step three: and (3) carrying out separation on the degreased oil without the alcohol extract obtained in the step two by using peony seed meal at the temperature of 40 ℃, the material-liquid ratio of 1: 15, performing alkali extraction and centrifugation under the conditions of pH10(0.005mol/L) and time of 2.5h to obtain an alkali extraction supernatant, performing acid precipitation and centrifugation on the alkali extraction supernatant under the conditions of pH3 and time of 2h to obtain protein, washing the obtained protein to be neutral, and performing spray drying to obtain the peony protein for oil, wherein the protein extraction rate is 41.2%, and the purity is 91%.
Example 2:
the method comprises the following steps: crushing and granulating the hydraulic peony seed meal, and extracting for 4 times by using butane as an extracting agent under the conditions of the pressure of 0.48mpa and the extraction temperature of 50 ℃ to obtain the peony seed meal for the degreased oil with the oil content of 0.94%;
step two: and (2) carrying out treatment on the peony seed meal for the degreased oil obtained in the step one by taking methanol as a solvent, wherein the alcohol concentration is 90%, and the material-liquid ratio is 1: 10, extracting for 3 times at the extraction temperature of 45 ℃ for 3 hours to obtain the peony seed meal for the degreased oil without the alcohol extract, wherein the yield of the alcohol extract is 14%;
step three: and (3) carrying out oil-removing treatment on the degreased oil without the alcohol extract obtained in the step two by using peony seed meal at the temperature of 50 ℃, the material-liquid ratio of 1: 25, performing alkali extraction and centrifugation under the conditions of pH10.5(0.008mol/L) and time of 3.5h to obtain an alkali extraction supernatant, performing acid precipitation and centrifugation on the alkali extraction supernatant under the conditions of pH4.0 and time of 2h, washing the obtained protein to be neutral, and performing spray drying to obtain the peony protein isolate for oil, wherein the protein extraction rate is 51.62%, and the purity is 94%.
Example 3:
the method comprises the following steps: crushing and granulating the hydraulic peony seed meal, and extracting for 3 times by using butane as an extracting agent under the conditions of the pressure of 0.6mpa and the extraction temperature of 45 ℃ to obtain the peony seed meal for the degreased oil with the oil content of 1.15%;
step two: and (2) carrying out treatment on the peony seed meal for the degreased oil obtained in the step one by taking methanol as a solvent, wherein the alcohol concentration is 80%, and the material-liquid ratio is 1: 15, extracting for 1 time at the extraction temperature of 50 ℃ for 2 hours to obtain the peony seed meal for the degreased oil without the alcohol extract, wherein the yield of the alcohol extract is 12%;
step three: and (3) carrying out separation on the degreased oil without the alcohol extract obtained in the step two by using peony seed meal at the temperature of 40 ℃, the material-liquid ratio of 1: 25, performing alkali extraction and centrifugation under the conditions of pH10.5(0.008mol/L) and time of 4h to obtain an alkali extraction supernatant, performing acid precipitation and centrifugation on the alkali extraction supernatant under the conditions of pH5 and time of 3h, washing the obtained protein to be neutral, and performing spray drying to obtain the peony protein isolate for oil, wherein the protein extraction rate is 47.9%, and the purity is 93%.
The peony protein isolate for oil prepared in example 2 was compared functionally with the soy protein isolate, and the results are shown in table 1.
TABLE 1 functional comparison of oil peony protein isolates with soy protein isolates
Figure BDA0003145288580000061
As is clear from the data in table 1, the isolated soy protein obtained in example 2 is superior to the isolated soy protein in functional properties such as water absorption, oil retention, emulsifying property, emulsion stability, foaming property, foam stability, etc.
The invention firstly discovers that the color of the separated protein can be improved after alcohol extraction, and meanwhile, the alcohol extract contains components such as flavone, paeoniflorin and the like, and has high recycling value, so that the application analyzes how the alcohol extract can be effectively and efficiently extracted, and the analysis process is shown in tables 2 and 3.
Table 2 response surface optimization methanol treatment of peony seed meal test results (alcohol extract yield is measured by rutin content)
Figure BDA0003145288580000071
Table 3 response surface optimization ethanol treatment of peony seed meal test results (alcohol extract yield is measured by rutin content)
Figure BDA0003145288580000081
From the data in tables 2 and 3, the ratio of the feed to the liquid is 1: 5-1: 15, the extraction temperature is 40-50 ℃, the extraction time is 1-3 h, and the alcohol extract containing the flavone can be efficiently extracted, so that the quality of the protein isolate is ensured, and the subsequent obtaining and reutilization of the alcohol extract containing the flavone is facilitated.
The method for extracting protein by alkali also carries out optimization test, and the process is shown in table 4.
Table 4 orthogonal experiments to optimize the protocol and results of alkaline protein extraction
Figure BDA0003145288580000082
Figure BDA0003145288580000091
As can be seen from Table 4, the temperature is 40-50 ℃, the time is 2.5-3.5h, the pH is controlled between 10-11, and the ratio of the materials to the liquids is 1: 15-1: 25, the protein isolate with higher purity and yield can be obtained.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (3)

1. A method for extracting peony protein isolate for oil is characterized in that: the method comprises the following steps:
the method comprises the following steps: carrying out shelling, cake pressing or hydraulic treatment on oil peony seeds, crushing and granulating, and extracting for 1-4 times by using butane as an extracting agent under the conditions of pressure of 0.3-0.8 mpa and extraction temperature of 20-50 ℃ to obtain degreased oil peony seed meal with the oil content of less than or equal to 1.5%;
step two: and (2) carrying out treatment on the peony seed meal for the degreased oil obtained in the step one by using methanol or ethanol as a solvent, wherein the alcohol concentration is 50-95%, and the material-liquid ratio is 1: 5-1: 15, extracting for 1-3 times at the extraction temperature of 40-50 ℃ for 1-3 h to obtain the peony seed meal for the degreased oil without the alcohol extract;
step three: and (3) carrying out separation on the degreased oil without the alcohol extract obtained in the step two by using peony seed meal at the temperature of 30-50 ℃ and the material-liquid ratio of 1: 15-1: performing alkali extraction at the pH of 10-11 for 2-5 h, centrifuging to obtain an alkali extraction supernatant, performing acid precipitation on the alkali extraction supernatant at the pH of 3-5 for 1-4 h, centrifuging, washing the obtained protein to neutrality, and performing spray drying to obtain the peony protein isolate for oil.
2. The method for extracting peony protein isolate for oil according to claim 1, wherein: the peony seed meal in the step one is oil peony seeds, and is subjected to shelling, cake pressing treatment or hydraulic pressure.
3. The method for extracting peony protein isolate for oil according to claim 1, wherein: and (3) volatilizing the solvent from the alcohol extract obtained in the step two, wherein the alcohol extract contains flavone and paeoniflorin.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113995046A (en) * 2021-11-26 2022-02-01 山东省科学院菏泽分院 Method for extracting high-emulsibility and oil-absorption peony protein isolate
CN114525169A (en) * 2022-01-19 2022-05-24 西安海斯夫生物科技有限公司 Method for continuously grading peony seeds

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Publication number Priority date Publication date Assignee Title
CN103493968A (en) * 2013-09-23 2014-01-08 河南科技大学 Preparation method of high-purity peony seed protein powder for oil
CN106467861A (en) * 2015-08-17 2017-03-01 洛阳健特生物科技有限公司 Peony seed oil subcritical fluid extraction technique
CN108887461A (en) * 2018-05-25 2018-11-27 常州大学 Peony seeds albumen and its extracting method
CN109593601A (en) * 2018-12-30 2019-04-09 洛阳万景祥牡丹产业科技有限公司 A kind of cold pressing extraction process of peony seed oil production
CN110226664A (en) * 2019-07-16 2019-09-13 山西潞安石圪节智华生物科技有限公司 A kind of preparation method of peony seeds albumen powder

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103493968A (en) * 2013-09-23 2014-01-08 河南科技大学 Preparation method of high-purity peony seed protein powder for oil
CN106467861A (en) * 2015-08-17 2017-03-01 洛阳健特生物科技有限公司 Peony seed oil subcritical fluid extraction technique
CN108887461A (en) * 2018-05-25 2018-11-27 常州大学 Peony seeds albumen and its extracting method
CN109593601A (en) * 2018-12-30 2019-04-09 洛阳万景祥牡丹产业科技有限公司 A kind of cold pressing extraction process of peony seed oil production
CN110226664A (en) * 2019-07-16 2019-09-13 山西潞安石圪节智华生物科技有限公司 A kind of preparation method of peony seeds albumen powder

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113995046A (en) * 2021-11-26 2022-02-01 山东省科学院菏泽分院 Method for extracting high-emulsibility and oil-absorption peony protein isolate
CN114525169A (en) * 2022-01-19 2022-05-24 西安海斯夫生物科技有限公司 Method for continuously grading peony seeds
CN114525169B (en) * 2022-01-19 2022-11-15 西安海斯夫生物科技有限公司 Method for continuously grading peony seeds

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