CN113245343B - Efficient utilization method of squeezed peony residues - Google Patents
Efficient utilization method of squeezed peony residues Download PDFInfo
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- CN113245343B CN113245343B CN202110453651.6A CN202110453651A CN113245343B CN 113245343 B CN113245343 B CN 113245343B CN 202110453651 A CN202110453651 A CN 202110453651A CN 113245343 B CN113245343 B CN 113245343B
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/028—Flow sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B5/00—Operations not covered by a single other subclass or by a single other group in this subclass
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B2101/00—Type of solid waste
- B09B2101/02—Gases or liquids enclosed in discarded articles, e.g. aerosol cans or cooling systems of refrigerators
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Enzymes And Modification Thereof (AREA)
Abstract
The invention provides a high-efficiency utilization method of squeezed peony flower residues, which mainly comprises squeezing, enzymolysis of the peony flower residues, extraction of hydrolysate of the peony flower residues, enzymolysis of peony flower water A, decoloring and enzyme deactivation of peony flower water B and sterilization; in the extraction process of the flower residue zymolyte, closed low-temperature low-pressure extraction is adopted; when the peony flower water A is subjected to enzymolysis, a gradient enzymolysis mode is adopted. The peony water finished product obtained by the utilization method has the advantages of strong free radical removing capability and good stability, the extraction efficiency of the peony water in the flower residue by the method reaches 78%, the squeezed peony residue is reasonably and comprehensively utilized, the utilization rate of peony resources is improved, and the environment is protected.
Description
Technical Field
The invention relates to the technical field of comprehensive utilization of squeezed flower residues, and particularly relates to a high-efficiency utilization method of squeezed peony flower residues.
Background
In recent years, with the industrialization of oil peonies, the planting area of the peonies is rapidly expanded, and people find that the yield of fresh flowers of the peonies is also considerable while harvesting a large amount of peony seeds. 150kg of fresh petals can be harvested per mu averagely in the full-bearing period; because the peony belongs to self-pollination, the petals collected by adopting the standard operation method not only do not influence the seed production, but also are beneficial to improving the pollination rate and the seed production. In order to utilize the peony flower resources, researchers begin to explore various extraction methods for active ingredients of the peony flowers, and the current extraction method comprises CO 2 Supercritical extraction, steam distillation, solvent extraction, ultrasonic microwave-assisted extraction, mechanical squeezing, etc.; the mechanical squeezing method has the advantages of low investment, low operation cost, low technical threshold and the like, so that the method is more and more popularized and applied. However, after the fresh flower water is extracted from the peony by squeezing, the residual flower residue still contains a large amount of water (the water content is determined to be 82.3%), and the flower residue is also rich in functional components such as polyphenol, flavone, polysaccharide and anthocyanin, and if the flower residue is directly discarded, resources are wasted and the environment is polluted.
The patent documents on the aspect of water extraction of peony flowers are not so many, and especially the technical data on the further comprehensive utilization of squeezed peony flower residues are still blank.
Patent publication No. CN103142431B discloses a peony hydrolat, which is prepared by pickling fresh peony petals, adding water for distillation, collecting distillate, namely a peony petal extract, and mixing the petal extract and the peony root bark extract according to a certain volume ratio. The defect of the patent technology is that the peony extract obtained by the steam distillation method only contains volatile aroma components, and rich mineral elements, amino acids, polyphenol, flavone, anthocyanin and other antioxidant components are remained in the distilled petal mud, so that the finished peony water has weak capacities of resisting oxidation and removing free radicals; in addition, the residual petal mud causes environmental pollution in the process of discarding, and is not beneficial to energy conservation and environmental protection.
The patent publication No. 109730948 discloses a method for extracting cell water of peony flower from peony flower and its application, which comprises squeezing peony flower, performing vacuum distillation on the residue to obtain distillate 1, adding 6-8 times of water into the residue, performing simple enzymolysis, distilling to obtain distillate 2, and mixing the squeezed liquid with the distillate 1 and the distillate 2 to obtain the final product. The patent technique is not enough in that the color of the squeezed liquid is dark, the color of the peony flower water is poor after the squeezed liquid is mixed with twice distillate, and microorganisms and the like exist in the squeezing process, so that the stability of the product quality is not facilitated.
Therefore, the method for efficiently utilizing the squeezed flower residues is significant.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the efficient utilization method of the squeezed peony flower residue, the peony flower water finished product obtained by the utilization method has the advantages of strong free radical removing capability and good stability, the extraction efficiency of the peony flower water in the flower residue reaches 78%, the squeezed peony flower residue is reasonably and comprehensively utilized, the peony resource utilization rate is improved, and the environment is protected.
The specific scheme of the invention is as follows:
a method for efficiently utilizing squeezed peony flower residue mainly comprises squeezing, performing enzymolysis on the peony flower residue, extracting hydrolysate of the peony flower residue, performing enzymolysis on peony flower water A, performing decolorization and enzyme deactivation on peony flower water B, and sterilizing;
in the extraction process of the flower residue zymolyte, closed low-temperature low-pressure extraction is adopted;
when the peony flower water A is subjected to enzymolysis, a gradient enzymolysis mode is adopted, so that the water solubility and the stability of a finished peony flower water product are improved.
A high-efficiency utilization method of squeezed peony flower residues comprises the following specific steps:
(1) squeezing: carrying out enzyme deactivation treatment on fresh flower petals to prevent peroxidase and polyphenol oxidase in the petals from browning and blackening cell juice in the squeezing process, then crushing the flower petals into flower mud by using a crusher, and delivering the flower mud into a squeezer for squeezing to obtain flower residues;
(2) flower residue enzymolysis: uniformly spraying a cellulase solution on the flower residue, and then stacking and performing enzymolysis on the flower residue, wherein the enzymolysis temperature is 30-37 ℃, and the stacking and enzymolysis time is 8-12h, so as to obtain a flower residue zymolyte; through enzyme treatment, cell walls of flower residue cells can be degraded, and leaching of petal cell sap is promoted;
(3) carrying out closed low-temperature low-pressure extraction on the flower residue zymolyte: carrying out closed low-temperature extraction on the flower residue zymolyte in an extraction tank, wherein the extractant is methyl ether, the weight (g/g) ratio of the flower residue zymolyte to the methyl ether is 1:1.5-2.5, the extraction temperature is 20-50 ℃, the pressure is 0.30-1.2MPa, the extraction time is 20-50min, the extraction frequency is 3 times, after the extraction is finished, pouring the mixed solution of the extract and the extractant into an evaporation tank, the evaporation temperature of the recovered solvent is 30-50 ℃, obtaining peony flower water A in the evaporation tank after evaporation, and obtaining dry flower residue in the extraction tank;
(4) and (3) enzymolysis of peony water A: adding pectinase into the peony flower water A obtained in the step (3), wherein the adding amount of the pectinase is 300-; heating the primary enzymolysis liquid to 60-63 ℃, adding glucoamylase into the primary enzymolysis liquid, wherein 5-10 wu of glucoamylase is added into each kilogram of the primary enzymolysis liquid, and the enzymolysis time is 30-50min, so as to obtain peony flower water B; because the components of the peony flower water A are extremely complex, and particularly certain macromolecular substances in the peony flower water A can generate the phenomena of precipitation, agglomeration and the like when the peony flower water A is placed for a long time, and the stability of the product is influenced, the two-step enzymolysis method is adopted to degrade certain macromolecules and colloidal substances, so that the water solubility of molecules in the peony flower water B is increased, the clarity and transparency of the peony flower water B are greatly improved, and the stability of the product is ensured;
(5) and (3) decolorizing and inactivating enzyme of peony flower water B: decoloring the peony flower water B obtained in the step (4), and then inactivating enzyme in a decoloring solution to obtain peony flower water C;
(6) primary filtering: filtering the peony water C by adopting a 200-500-mesh filter screen to obtain peony water D;
(7) high-temperature instantaneous sterilization: carrying out ultrahigh-temperature instantaneous sterilization on the peony water D at the temperature of 121-;
(8) fine filtering: performing fine filtration on the peony flower water E by using a sterile filter with the filter screen aperture of 2000-3000 meshes to obtain a finished product; in the fine filtration process, undegraded micro-polymers separated out due to high-temperature sterilization can be filtered;
(9) packaging and storing: packaging the product with food-grade sterile plastic container or aluminum container, and storing at 2-10 deg.C.
Preferably, in the step (1), the fresh petals are picked in the early morning of the rainy day and before and after the rainy day at 6-10 o' clock, and the blooming period is full bloom; after picking, the fresh flowers are frozen at the temperature of-10 to 20 ℃ so that the fresh flower petals can keep bright colors; the frozen flower petals are completely thawed before squeezing and then enzyme deactivated.
Preferably, in the step (1), the enzyme deactivation mode is microwave enzyme deactivation or ultrasonic enzyme deactivation.
Preferably, in the step (1), the press is a belt press or a screw press, and the pattern mud is pressed twice in the pressing process.
Preferably, in step (2), the concentration of the cellulase solution is 4-7% (v/v); the volume-to-weight (ml/g) ratio of the cellulase solution to the flower residue is 4-8: 100.
Preferably, in the step (2), the enzymolysis temperature is 32-35 ℃, and the volume-to-weight (ml/g) ratio of the cellulase solution to the flower residue is 5-7: 100.
Preferably, in step (3), the recovery temperature of the extractant is 30 to 50 ℃.
Preferably, in the step (5), activated carbon is used as a decolorizing agent, and the weight-to-volume (g/ml) ratio of the activated carbon to the peony flower water B is 2-5: 100; the enzyme inactivating temperature is 70-80 deg.C, and the time is 20-50 min.
Preferably, in the step (3), the dried flower residues in the extraction tank are aired to further volatilize the solvent, so that filler flower residues are obtained, and the filler flower residues are used for pillows; the water content of the filling flower residue is less than 2 percent.
Compared with the prior art, the invention has the beneficial effects that:
1. by using the method, the peony flower water in the flower residue can be effectively extracted, the extraction rate of the peony flower water in the flower residue reaches 77.5%, and the aims of changing waste into valuable, saving energy and protecting environment are fulfilled.
2. The peony flower water finished product obtained by the method is rich in antioxidant components (such as polyphenol, flavone, anthocyanin and the like) in peony flowers, so that the finished product has good free radical scavenging capacity and antioxidant performance; meanwhile, the finished product is rich in volatile aroma components in the peony, and no organic solvent residue exists in the finished product.
3. In the method, secondary enzymolysis is firstly disclosed to the peony flower water A, so that macromolecules which are easy to generate precipitates, mucilage and flocculation and influence the stability of the product are degraded, the problem that precipitates such as the precipitates and the flocculation are easy to generate when the product obtained by the process is placed for a long time is solved, the clarity and the transparency of the finished peony flower water are improved, and the quality and the stability of the product are ensured.
Detailed Description
In order to make those skilled in the art better understand the technical solutions in the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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
(1) Squeezing: carrying out enzyme deactivation treatment on fresh flower petals to prevent peroxidase and polyphenol oxidase in the petals from browning and blackening cell juice in the squeezing process, then crushing the flower petals into flower mud by using a crusher, and delivering the flower mud into a squeezer for squeezing to obtain flower residues;
wherein, fresh flower petals are picked in the early morning between 6-10 o' clock before and after grain rain, and the flowering period is full bloom; freezing at-10-20 deg.C after picking to keep fresh flower petal with bright color; before crushing and squeezing, completely unfreezing frozen fresh flower petals and then inactivating enzymes;
the enzyme deactivation mode is microwave enzyme deactivation;
the squeezer is a belt squeezer, and the flower pulp is squeezed twice in the squeezing process; the water yield is 34.6%, the water content of the flower residue is 82.3%, and the squeezing process flow is as follows: unfreezing frozen petals, feeding the unfrozen petals into a hammer crusher by using a raw material conveyor to be crushed to obtain flower mud, feeding the flower mud into a belt type squeezer from a low-position storage tank through a screw pump propeller to be squeezed twice, feeding the squeezed liquid into a vibrating screen, feeding the squeezed liquid into a bag type filter to obtain squeezed flower water, and collecting flower dregs from a spiral residue conveyor;
(2) flower residue enzymolysis: preparing a cellulase solution with the concentration of 4% (v/v); uniformly spraying 100kg of freshly squeezed flower residues with a cellulase solution according to the volume-to-weight (ml/g) ratio of 5:100 of the cellulase solution to the flower residues, and then carrying out stacking enzymolysis on the flower residues at the enzymolysis temperature of 30 ℃ for 11h to obtain flower residue zymolyte; through enzyme treatment, cell walls of flower residue cells can be degraded, and leaching of petal cell sap is promoted;
(3) carrying out closed low-temperature low-pressure extraction on the flower residue zymolyte: carrying out closed low-temperature extraction on the flower residue zymolyte in an extraction tank, wherein an extractant is methyl ether, the weight (g/g) ratio of the flower residue zymolyte to the methyl ether is 1:1.5, the extraction temperature is 30 ℃, the pressure is 0.30MPa, the extraction time is 50min, the extraction times are 3 times, a water phase is collected to be peony water A, after the extraction is finished, a mixed solution of an extraction liquid and the extractant is poured into an evaporation tank, the evaporation temperature of a recovered solvent is 30 ℃, the peony water A is in the evaporation tank after the evaporation, and dry flower residue is in the extraction tank;
(4) and (3) enzymolysis of peony water A: adding pectinase into the peony flower water A obtained in the step (3), wherein the adding amount of the pectinase is 300u per kg of the flower water, the temperature of the flower water is 40 ℃, the enzymolysis time is 60min, and once enzymolysis is finished to obtain a first enzymolysis liquid;
heating the primary enzymolysis liquid to 60-63 ℃, adding glucoamylase into the primary enzymolysis liquid, and carrying out secondary enzymolysis; adding glucoamylase in an amount of 7 wu per kg of the primary enzymolysis liquid, wherein the enzymolysis time is 50min, and obtaining peony flower water B;
because the components of the peony flower water A are extremely complex, particularly certain macromolecular substances in the peony flower water A can generate precipitation, agglomeration and other phenomena when the peony flower water A is placed for a long time, and the stability of a product is influenced, the two-step enzymolysis method is adopted to degrade certain macromolecules and colloidal substances, so that the water solubility of molecules in the peony flower water B is increased, the clarity and transparency of the peony flower water B are greatly improved, and the stability of the product is ensured;
(5) and (3) decolorizing and inactivating enzyme of peony flower water B: decoloring the peony flower water B obtained in the step (4) by using activated carbon, wherein the weight-volume (g/ml) ratio of the activated carbon to the peony flower water B is 3: 100; inactivating enzyme in the decolorized solution at 80 ℃ for 50min to obtain peony water C;
(6) primary filtering: filtering the peony flower water C by adopting a 400-mesh filter screen to obtain peony flower water D;
(7) high-temperature instantaneous sterilization: carrying out ultrahigh-temperature instantaneous sterilization on the peony flower water D at 121 ℃ for 10s to obtain peony flower water E;
(8) fine filtering: finely filtering the peony flower water E by using an aseptic filter with the filter screen aperture of 2500 meshes to obtain a finished product; in the fine filtration process, undegraded micro-polymers precipitated by high-temperature sterilization can be filtered;
(9) packaging and storing: packaging the product in food-grade sterile plastic container, and storing at 2-10 deg.C.
Example 2
(1) Flower residue enzymolysis: preparing a cellulase solution with the concentration of 6% (v/v); uniformly spraying 100kg of freshly squeezed flower residues in the embodiment 1 on the flower residues according to the volume-weight (ml/g) ratio of the cellulase solution to the flower residues of 4:100, and then stacking the flower residues for enzymolysis at the enzymolysis temperature of 33 ℃ for 11h to obtain flower residue zymolyte; through enzyme treatment, cell walls of flower residue cells can be degraded, and leaching of petal cell sap is promoted;
(2) carrying out closed low-temperature low-pressure extraction on the flower residue zymolyte: carrying out closed low-temperature extraction on the flower residue zymolyte in an extraction tank, wherein an extractant is methyl ether, the weight (g/g) ratio of the flower residue zymolyte to the methyl ether is 1:2, the extraction temperature is 45 ℃, the pressure is 1.0MPa, the extraction time is 45min, the extraction times are 3 times, a water phase is collected to be peony water A, after the extraction is finished, a mixed solution of an extraction liquid and the extractant is poured into an evaporation tank, the evaporation temperature of a recovered solvent is 45 ℃, the peony water A is in the evaporation tank after the evaporation, and dry flower residue is in the extraction tank;
(3) and (3) enzymolysis of peony water A: adding pectinase into the peony flower water A, wherein the adding amount of the pectinase is 450u per kilogram of the flower water, the temperature of the flower water is 45 ℃, the enzymolysis time is 45min, and once enzymolysis liquid is obtained after one enzymolysis is finished;
heating the primary enzymolysis liquid to 60-63 ℃, adding glucoamylase into the primary enzymolysis liquid, and carrying out secondary enzymolysis; adding glucoamylase in an amount of 7.5 wu per kg of the primary enzymolysis liquid, and performing enzymolysis for 45min to obtain peony flower water B;
because the components of the peony flower water A are extremely complex, and particularly certain macromolecular substances in the peony flower water A can generate the phenomena of precipitation, agglomeration and the like when the peony flower water A is placed for a long time, and the stability of the product is influenced, the two-step enzymolysis method is adopted to degrade certain macromolecules and colloidal substances, so that the water solubility of molecules in the peony flower water B is increased, the clarity and transparency of the peony flower water B are greatly improved, and the stability of the product is ensured;
(4) and (3) decolorizing and inactivating enzyme of peony flower water B: decoloring the peony flower water B by using activated carbon, wherein the weight-volume (g/ml) ratio of the activated carbon to the peony flower water B is 4: 100; inactivating enzyme in the decolorized solution at 75 ℃ for 45min to obtain peony water C;
(5) primary filtering: filtering the peony flower water C by adopting a 300-mesh filter screen to obtain peony flower water D;
(6) high-temperature instantaneous sterilization: carrying out ultrahigh-temperature instantaneous sterilization on the peony flower water D at the sterilization temperature of 131 ℃ for 5s to obtain peony flower water E;
(7) fine filtering: finely filtering the peony flower water E by using a sterile filter with the filter screen aperture of 2000 meshes to obtain a finished product; in the fine filtration process, undegraded micro-polymers precipitated by high-temperature sterilization can be filtered;
(8) packaging and storing: packaging the product in food-grade sterile plastic container, and storing at 2-10 deg.C.
Example 3
(1) Squeezing: the difference from the step (1) in example 1 is that the enzyme deactivation mode is ultrasonic enzyme deactivation, and the squeezing machine is a screw-type squeezing machine; the water yield of the squeezed flower water is 34.3 percent, and the water content of the flower residue is 82.5 percent;
(2) flower residue enzymolysis: preparing a cellulase solution with the concentration of 6% (v/v); uniformly spraying 100kg of freshly squeezed flower residues with a cellulase solution according to the volume-to-weight (ml/g) ratio of the cellulase solution to the flower residues of 8:100, and then carrying out stacking enzymolysis on the flower residues at the enzymolysis temperature of 37 ℃ for 8h to obtain flower residue zymolyte; through enzyme treatment, cell walls of flower residue cells can be degraded, and leaching of petal cell sap is promoted;
(3) carrying out closed low-temperature low-pressure extraction on the flower residue zymolyte: carrying out closed low-temperature extraction on the flower residue zymolyte in an extraction tank, wherein an extractant is methyl ether, the weight (g/g) ratio of the flower residue zymolyte to the methyl ether is 1:2.5, the extraction temperature is 50 ℃, the pressure is 1.2MPa, the extraction time is 20min, the extraction times are 3 times, a water phase is collected to be peony water A, after the extraction is finished, a mixed solution of an extraction liquid and the extractant is poured into an evaporation tank, the evaporation temperature of a recovered solvent is 50 ℃, the peony water A is in the evaporation tank after the evaporation, and dry flower residue is in the extraction tank;
(4) and (3) carrying out enzymolysis on peony water A: adding pectinase into the peony flower water A, wherein the adding amount of the pectinase is 500u per kilogram of the flower water, the temperature of the flower water is 50 ℃, the enzymolysis time is 30min, and once enzymolysis liquid is obtained after one enzymolysis is finished;
heating the primary enzymolysis liquid to 60-63 ℃, adding glucoamylase into the primary enzymolysis liquid, and carrying out secondary enzymolysis; adding 10 ten thousand of glucoamylase into each kilogram of primary enzymolysis liquid, wherein the enzymolysis time is 30min, and obtaining peony flower water B;
because the components of the peony flower water A are extremely complex, and particularly certain macromolecular substances in the peony flower water A can generate the phenomena of precipitation, agglomeration and the like when the peony flower water A is placed for a long time, and the stability of the product is influenced, the two-step enzymolysis method is adopted to degrade certain macromolecules and colloidal substances, so that the water solubility of molecules in the peony flower water B is increased, the clarity and transparency of the peony flower water B are greatly improved, and the stability of the product is ensured;
(5) and (3) decolorizing and inactivating enzyme of peony flower water B: decolorizing peony water B by using activated carbon, wherein the weight-volume (g/ml) ratio of the activated carbon to the peony water B is 5: 100; inactivating enzyme in the decolorized solution at 80 ℃ for 20min to obtain peony water C;
(6) primary filtering: filtering the peony flower water C by adopting a 500-mesh filter screen to obtain peony flower water D;
(7) high-temperature instantaneous sterilization: carrying out ultrahigh-temperature instantaneous sterilization on the peony flower water D at 135 ℃ for 5s to obtain peony flower water E;
(8) fine filtering: finely filtering the peony flower water E by using an aseptic filter with a filter screen aperture of 3000 meshes to obtain a finished product; in the fine filtration process, undegraded micro-polymers separated out due to high-temperature sterilization can be filtered;
(9) packaging and storing: packaging the product in aluminum container, and storing at 2-10 deg.C.
In examples 1 to 3, the water content of the flower residue was about 82.3%, and after the treatment, the water content of the dried flower residue obtained by recovering the solvent was about 16.5%; drying the dried flower residue after the solvent is recovered to obtain filler flower residue which can be used as a pillow filler; and drying the dry flower residues in a drying process by adopting an air-blast drying oven at the drying temperature of 55 ℃, and obtaining the filler flower residues when the water content of the dry flower residues is reduced to below 2%.
In the extraction process of the low-temperature low-pressure closed system, various antioxidant components and volatile aroma components in the peony are fully reserved; in the extraction process, methyl ether is used as an extractant, and can be removed during high-temperature instantaneous sterilization treatment, so that no solvent residue exists in the finished product of the peony water.
Comparative example 1
The difference from example 3 is that the enzymatic hydrolysis of the flower residue in step (2) of example 3 was not carried out on the flower residue.
Comparative example 2
The difference from the example 3 is that the peony water A is not subjected to the enzymolysis process of the peony water A in the step (4) in the example 3.
Comparative example 3
The difference from the example 3 is that the peony water A is not subjected to the secondary enzymolysis process (only pectinase enzymolysis) of the peony water A in the step (4) in the example 3.
Comparative example 4
The difference from example 3 is that the peony water A is not subjected to the primary enzymolysis process (only glucoamylase enzymolysis) of the peony water A in step (4) of example 3.
Comparative example 5
Patent publication No. CN103142431B discloses a peony hydrosol, which is prepared by pickling fresh peony petals, adding water for distillation, and collecting distillate, i.e. peony petal extract.
Comparative example 6
The patent publication No. 109730948 discloses a method for extracting cell water of peony flower from peony flower and application thereof, the method comprises squeezing peony flower to obtain squeezed liquid, performing reduced pressure dry distillation on pressed residue flower residue to obtain distillate 1, adding 6-8 times of water into the flower residue after dry distillation for simple enzymolysis, distilling to obtain distillate 2, and mixing the squeezed liquid with the distillate 1 and the distillate 2 to obtain the final product of cell water of peony flower.
And (3) detection:
the extraction rate of peony water and the water content of the dried flower residue in examples 1 to 3 and comparative example 1 were measured and shown in Table 1.
TABLE 1 extraction ratio of peony Water and Water content of dried flower residue
| Name of art | Extraction ratio (%) | Moisture content of dried flower residue (%) |
| Example 1 | 77.0 | 17.0 |
| Example 2 | 78.0 | 16.0 |
| Example 3 | 77.5 | 16.5 |
| Comparative example 1 | 65.0 | 20.5 |
As can be seen by combining the table 1, the water extraction rate of the peony flowers in the embodiments 1-3 of the invention is significantly higher than that of the comparative example 1 which is not subjected to enzymolysis by cellulase; after the extraction and the recovery of methyl ether, the water content of the dried flower residue obtained in the examples 1-3 is lower than that of the comparative example 1, which proves that the extraction rate of the peony flower water is effectively improved after the flower residue is subjected to the enzymolysis by cellulase.
Second, the results of the physical and chemical indicators of the peony water obtained in example 3 and comparative examples 2 to 4 are shown in Table 2.
TABLE 2 physicochemical indices of peony flower water
| Name of art | Total sugar (%) | Total phenols (mg/ml) | Reducing sugar (%) | Dry matter (%) | Protein (%) |
| Example 3 | 8.40 | 3.84 | 7.81 | 9.63 | 0.42 |
| Comparative example 2 | 10.23 | 1.86. | 3.92 | 11.34 | 0.65 |
| Comparative example 3 | 9.52 | 2.33 | 4.65. | 10.45 | 0.52 |
| Comparative example 4 | 9.45 | 2.45 | 5.12 | 10.21 | 0.50 |
As can be seen from Table 2, the difference between the total sugar and the reducing sugar of the extract in example 3 was the smallest, the difference between the total sugar and the reducing sugar of comparative examples 3 and 4 was the next, and the difference between the total sugar and the reducing sugar of comparative example 2 was the largest; the degradation effect of components such as sugar macromolecules in the peony water is most obvious after the secondary enzymolysis, the water solubility of each component in the peony water is enhanced, and the product stability is improved. In addition, the total phenol content of the product is the highest in the example 2, which also shows that the double enzymolysis promotes the generation of the total phenol and improves the oxidation resistance of the product.
And (III) the color and the light transmittance of the peony flower water of the example 3 and the comparative example 6 are detected, and the results are shown in the table 3.
TABLE 3 color and transmittance of peony water
| Sample name | Color | Light transmittance (%) |
| Example 3 | Colorless and colorless | 100 |
| Comparative example 6 | Reddish brown | 92 |
In combination with table 3, it can be seen that: the color and luster and the clarity (light transmittance) of the product obtained in the embodiment 3 are obviously superior to those of the product obtained in the comparative example 6 (patent technology with publication number 109730948).
And (IV) carrying out microbial detection on the peony water obtained in example 3 and comparative example 6, wherein the results are shown in Table 4.
The culture process comprises the following steps: the products of example 3 and comparative example 6 were coated on PDA plate medium, and the samples were stored in a constant temperature and humidity incubator at a set temperature of 30. + -. 1 ℃ and a relative humidity of 75% for 90 days to record the change of each sample.
TABLE 4 microbiological assay results for peony water
| Sample name | Total number of bacteria | Mold and yeast | Conclusion |
| Example 3 | 0 | 0 | Qualified |
| Comparative example 6 | 200cfu/ml | 1000cfu/ml | Fail to be qualified |
As can be seen from Table 4: the detection result of the product microorganism obtained in the embodiment 3 of the invention meets the specification, and the detection result of the product microorganism obtained in the comparative example 6 (the patent technology with the publication number of 109730948) does not meet the standard requirement. The main reason is that the product obtained in comparative example 6 is squeezed flower water which is directly mixed with distilled flower water, and the squeezed flower water has poor color, clarity and sanitation indexes without being treated.
(V) evaluation of microbial condition and sensory condition was carried out on the peony water obtained in example 3 and comparative examples 2 to 6, and the results are shown in Table 5.
The culture process comprises the following steps: the peony water of example 3 and comparative examples 2-6 were applied to PDA plate medium, and the samples were stored for 15 days at a set temperature of 40 + -1 deg.C and a relative humidity of 75% in a constant temperature and humidity incubator to record the change of each sample.
TABLE 5 microbial and organoleptic status of peony Water
| Sample name | Smell(s) | Colour(s) | Turbidity (haze) | Flocculation | Precipitation of | Growth of bacteria |
| Example 3 | Peony flower fragrance | Light yellow | Is composed of | Is free of | Is free of | Is free of |
| Comparative example 2 | Peony flower fragrance | Light yellow | Turbidity | Flocculation | Precipitation of | Is free of |
| Comparative example 3 | Peony flower fragrance | Light yellow | Slight turbidity | Micro flocculation | No precipitation | Is free of |
| Comparative example 4 | Peony flower fragrance | Light yellow | Slight turbidity | Micro flocculation | No precipitation | Is free of |
| Comparative example 5 | Peony flower fragrance | Light yellow | Is free of | Micro flocculation | Is free of | Is free of |
| Comparative example 6 | Musty taste | Reddish brown color | Turbidity (haze) | Flocculation | Precipitation of | Long wool |
From the data in table 5, it can be seen that: after the test is placed for 15 days in an accelerated test, indexes of each proportion have certain changes in different degrees, and particularly, the comparative example 6 shows that the peony flower has poor water stability and serious bacteria growth; and all indexes of the product in the embodiment 3 of the invention are not changed, which shows that the product obtained by the invention has better stability.
Sixthly, the chemical components of the peony water of example 3 and comparative examples 5 to 6 were analyzed, and see table 6.
TABLE 6 detection of chemical composition in peony water
Seventhly, the oxidation resistance of the peony water of example 3 and comparative examples 5 to 6 was tested, and is shown in Table 7.
TABLE 7 measurement of antioxidant capacity in peony water
| Sample name | DPPH clearance (%) | FRAP clearance (%) |
| Example 3 | 92.4 | 88.4 |
| Comparative example 5 | 18.2 | 20.9 |
| Comparative example 6 | 45.8 | 50.2 |
| CO 2 Supercritical extraction | 30.6 | 38.3 |
As can be seen from Table 7, the peony flower of example 3 of the present invention has a strong ability to scavenge free radicals, and thus has a strong antioxidant ability, as confirmed by the results of measurements of the contents of total phenols, flavones, proanthocyanidins and anthocyanins in Table 6. As can be seen from Table 6, the contents of total phenols, flavones, proanthocyanidins and anthocyanins in the peony water of example 3 of the invention are all significantly higher than those of comparative examples 5 and 6, which illustrates that the method of the invention effectively retains the antioxidant compounds in the flower residue.
Although the present invention has been described in detail by referring to the preferred embodiments, the present invention is not limited thereto. Various equivalent modifications or substitutions can be made on the embodiments of the present invention by those skilled in the art without departing from the spirit and scope of the present invention, and these modifications or substitutions are within the scope of the present invention/any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (8)
1. A high-efficiency utilization method of squeezed peony flower residues is characterized by comprising the following specific steps:
(1) squeezing: carrying out enzyme deactivation treatment on the fresh flower petals, then crushing the fresh flower petals into flower mud by using a crusher, and squeezing the flower mud by using a squeezer to obtain flower dregs;
(2) flower residue enzymolysis: uniformly spraying a cellulase solution on the flower residue, and then stacking and performing enzymolysis on the flower residue, wherein the enzymolysis temperature is 30-37 ℃, and the stacking and enzymolysis time is 8-12h, so as to obtain a flower residue zymolyte;
(3) carrying out closed low-temperature low-pressure extraction on the flower residue zymolyte: carrying out closed low-temperature extraction on the flower residue zymolyte in an extraction tank, wherein the extractant is methyl ether, the weight ratio of the flower residue zymolyte to the methyl ether is 1:1.5-2.5, the extraction temperature is 20-50 ℃, the pressure is 0.30-1.2MPa, the extraction time is 20-50min, the extraction frequency is 3 times, after the extraction is finished, pouring the mixed solution of the extraction liquid and the extractant into an evaporation tank, the evaporation temperature of the recovered solvent is 30-50 ℃, obtaining peony flower water A in the evaporation tank after evaporation, and obtaining dry flower residue in the extraction tank;
(4) and (3) enzymolysis of peony water A: adding pectinase into the peony flower water A obtained in the step (3) in a gradient enzymolysis manner, wherein the addition amount of the pectinase is 300-; heating the primary enzymolysis liquid to 60-63 ℃, adding glucoamylase into the primary enzymolysis liquid, wherein 5-10 wu of glucoamylase is added into each kilogram of the primary enzymolysis liquid, and the enzymolysis time is 30-50min, so as to obtain peony flower water B;
(5) and (3) decolorizing and inactivating enzyme of peony flower water B: decoloring the peony flower water B obtained in the step (4), and then inactivating enzyme in a decoloring solution to obtain peony flower water C;
(6) primary filtering: filtering the peony water C by adopting a 200-500-mesh filter screen to obtain peony water D;
(7) high-temperature instantaneous sterilization: carrying out ultrahigh-temperature instantaneous sterilization on the peony water D at the temperature of 121-;
(8) fine filtering: performing fine filtration on the peony flower water E by using a sterile filter with the filter screen aperture of 2000-3000 meshes to obtain a finished product;
(9) packaging and storing: packaging the product with food-grade sterile plastic container or aluminum container, and storing at 2-10 deg.C.
2. The method for efficiently utilizing peony flower dregs according to claim 1, wherein in the step (1), the fresh petals are picked in the early morning between 6 and 10 o' clock before and after the rain, and the blooming period is full bloom period; freezing at-10-20 deg.C after picking; before squeezing, the frozen petals of fresh flowers are completely thawed and then enzyme is deactivated.
3. The efficient utilization method of peony residues as claimed in claim 1, wherein in step (1), said enzyme deactivation manner is microwave enzyme deactivation or ultrasonic enzyme deactivation.
4. The method for efficiently utilizing peony residues according to claim 1, wherein in the step (1), the press is a belt press or a screw press, and the flower mud is pressed twice during the pressing process.
5. The method for efficiently utilizing peony residues according to claim 1, wherein in step (2), the volume concentration of the cellulase solution is 4% -7%; the volume-weight ratio of the cellulase solution to the flower residue is 4-8:100 ml/g.
6. The method for efficiently utilizing peony flower dregs according to claim 1, wherein in the step (2), the enzymolysis temperature is 32-35 ℃, and the volume-to-weight ratio of the cellulase solution to the flower dregs is 5-7:100 ml/g.
7. The method for efficiently utilizing peony residues as claimed in claim 1, wherein, in step (3), the recovery temperature of the extractant is 30-50 ℃.
8. The method for efficiently utilizing peony residues as claimed in claim 1, wherein in step (5), activated carbon is used as a decolorizing agent, and the weight-to-volume ratio of activated carbon to peony flower water B is 2-5:100 g/ml; the enzyme inactivating temperature is 70-80 deg.C, and the time is 20-50 min.
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