CN113354755A - High-efficiency pectin extraction process - Google Patents
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Abstract
The invention provides a high-efficiency pectin extraction process, and relates to the technical field of pectin extraction. The high-efficiency pectin extraction process mainly comprises the following steps: pretreating raw materials, mixing plant chelating peptides, boiling, freezing and melting, performing enzymolysis treatment, performing centrifugal filtration, decoloring and concentrating, freezing, drying and crushing and the like. The method overcomes the defects of the prior art, effectively improves the efficiency of extracting pectin from pomace and the final yield of the pectin by re-melting the phytochelatin, various enzymes and freezing steam, reduces the use of special solvents, and is safe and environment-friendly.
Description
Technical Field
The invention relates to the technical field of pectin extraction and processing, and particularly relates to a high-efficiency pectin extraction process.
Background
Pectin is one of the plant cell wall components, is present in the intercellular layer between adjacent cell walls, and plays a role in binding cells together. The natural pectins are widely present in fruits, roots, stems and leaves of plants in the form of protopectin, pectin and pectic acid, are one of the components of cell walls, and exist along with cellulose to form an interlayer adhesive of adjacent cells, so that plant tissue cells are tightly bonded together. Protopectin is insoluble in water, but can be converted into water-soluble pectin by hydrolysis under the action of chemical reagents such as acid, alkali and salt and enzyme. Pectin is essentially a linear polysaccharide polymer containing from several hundred to about 1000 anhydrogalacturonic acid residues with corresponding average relative molecular masses of 50000-150000.
Most of the existing pectin production methods adopt acid extraction or alcohol extraction, but the acid extraction solution has high viscosity and slow filtration, and is usually matched with diatomite for filtration, so that the production period is long and the efficiency is low; the extraction conditions have a great influence on the extraction effect and influence on the product quality and yield. The method has the advantages that the ethanol extraction yield is high (20% -30%), but a large amount of ethanol is needed, the environment is polluted, a matched component organic solvent recovery, distillation and reutilization system is usually needed, the operation is complex, the patent with the patent number of CN201110071940.6 discloses a method for continuously preparing high-purity pectin by using an enzymolysis-ultrafiltration concentration-spray drying process, the pectin is extracted by combining the modes of enzymolysis, ultrafiltration concentration, spray drying and the like, the ethanol is not used, meanwhile, the pectin yield can reach 19.4%, but certain defects are still formed in the yield to a certain extent.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the high-efficiency pectin extraction process, which effectively improves the efficiency of extracting pectin from pomace and the final yield of the pectin by re-melting the phytochelatin, various enzymes and freezing steam, reduces the use of special solvents, and is safe and environment-friendly.
In order to achieve the above purpose, the technical scheme of the invention is realized by the following technical scheme:
a high-efficiency pectin extraction process comprises the following steps:
(1) pretreatment of raw materials: selecting fresh pomace, adding deionized water, grinding into slurry, ultrasonically homogenizing, and then placing in a high-pressure reaction kettle at 85-95 ℃ under the pressure of 14-18MPa for enzyme deactivation treatment to obtain enzyme-deactivated homogenized slurry for later use;
(2) mixing phytochelatin: adding the enzyme-deactivated homogeneous slurry into plant chelating peptide, stirring uniformly, and stirring for 1-3h at the water bath temperature of 30-45 ℃ to obtain a mixture for later use;
(3) boiling treatment: adding deionized water into the mixture, heating and boiling for 10-20min, and taking out to obtain boiled slurry for later use;
(4) freezing and re-melting: placing the boiled pulp in a liquid nitrogen environment for quick freezing, then placing the boiled pulp in a reaction kettle, and introducing high-temperature hot steam inwards for melting treatment to obtain melted pulp for later use;
(5) and (3) enzymolysis treatment: adding cellulase, hemicellulase, glycosidase and amylase into the melted slurry, stirring uniformly, adjusting pH to 4.0-5.0, and placing in a water bath at 30-50 deg.C for enzymolysis for 2-4h to obtain an enzymolysis solution for later use;
(6) centrifugal filtration: placing the enzymolysis liquid in a centrifuge for high-speed centrifugation, and removing precipitates to obtain a pectin liquid for later use;
(7) and (3) decoloring and concentrating: decolorizing the pectin solution with macroporous cation resin, and vacuum concentrating in a vacuum concentrating device to obtain concentrated solution;
(8) freeze-drying and crushing: freeze-drying the concentrated solution at low temperature, taking out, recovering to normal temperature, grinding, and pulverizing to obtain pectin.
Preferably, the fresh pomace in the step (1) is apple peel or citrus peel pomace.
Preferably, the mass ratio of the fresh pomace to the deionized water in the step (1) is 1: 3, the ultrasonic homogenization frequency is 40kHz, the homogenization time is 10min, and the enzyme deactivation time is 1-5 s.
Preferably, the mass ratio of the enzyme-deactivated homogeneous slurry and the phytochelatin in the step (2) is 100: 0.01-0.03, and the rotation speed of the heat-preservation stirring is 40-60 r/min.
Preferably, the rotation speed of 20-40r/min is required to be adopted to continuously stir the pulp in the cooking process in the step (3).
Preferably, the temperature of the high-temperature steam in the step (4) is 110-120 ℃, and the time for introducing the hot steam is 30-40 min.
Preferably, the mass ratio of the melted slurry mixed with the cellulase, the hemicellulase, the glycosidase and the amylase in the step (5) is 100: 0.06-0.08: 0.1-0.14: 0.02-0.06: 0.1-0.2.
Preferably, the rotation speed of the centrifugation in the step (6) is 4000-.
Preferably, the concentrated solution obtained in the step (7) is 1/5-1/8 in volume.
Preferably, the temperature of low-temperature freeze-drying in the step (8) is 5 ℃ below zero to 10 ℃ below zero, and the pectin after grinding is sieved by a 80-mesh sieve.
The invention provides a high-efficiency pectin extraction process, which has the advantages compared with the prior art that:
(1) according to the invention, the enzyme is deactivated at high pressure and high temperature, so that the pectinase in the pomace is effectively and rapidly deactivated, the pectin components in the original pomace are further retained, and meanwhile, the high-temperature and high-pressure treatment can make the pomace components looser, thereby facilitating the treatment of various enzymes in the later period and improving the production efficiency;
(2) according to the invention, the heat preservation treatment is carried out on the phytochelatin, then the cooking is carried out, and then the heat preservation enzymolysis of cellulase, hemicellulase, glycosidase and amylase is carried out, so that the corresponding enzymolysis is effectively carried out on the components of the pomace, and the yield of later pectin is improved;
(3) the method provided by the invention can be used for freezing the fruit residues after medium treatment at low temperature and then melting the fruit residues with hot steam, so that the plant tissues in the fruit residues are further damaged, the pectin is further dissolved out under the condition of not using a special solvent, and the final pectin yield is improved.
Description of the drawings:
FIG. 1: the pectin product obtained in example 3 of the present application is shown in the figure.
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 are clearly and completely described below in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all 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:
a high-efficiency pectin extraction process comprises the following steps:
(1) pretreatment of raw materials: selecting fresh citrus pomace, adding deionized water with the mass of 3 times, grinding into slurry, ultrasonically homogenizing for 10min at the frequency of 40kHz, placing the slurry in a high-pressure reaction kettle under the pressure of 14MPa and at the temperature of 85 ℃, and carrying out enzyme deactivation treatment for 1s to obtain enzyme deactivation homogenized slurry for later use;
(2) mixing phytochelatin: adding phytochelatin into the enzyme-inactivated homogeneous slurry according to the mass ratio of 100: 0.01, uniformly stirring, and stirring at the water bath temperature of 30 ℃ for 1h at the rotating speed of 40-60r/min to obtain a mixture for later use;
(3) boiling treatment: adding deionized water into the mixture, heating and boiling for 10min, continuously stirring the slurry at a rotating speed of 20r/min in the boiling process, and taking out to obtain boiled slurry for later use;
(4) freezing and re-melting: placing the boiled pulp in a liquid nitrogen environment for quick freezing, then placing the boiled pulp in a reaction kettle, and introducing high-temperature hot steam with the temperature of 110 ℃ for 30min to carry out melting treatment to obtain melted pulp for later use;
(5) and (3) enzymolysis treatment: mixing the melted slurry with cellulase, hemicellulase, glycosidase and amylase according to the mass ratio of 100: 0.06: 0.1: 0.02: 0.1, uniformly stirring, adjusting the pH to 4.0, and performing enzymolysis for 2 hours at the water bath temperature of 30 ℃ to obtain an enzymolysis liquid for later use;
(6) centrifugal filtration: placing the enzymolysis solution in a centrifuge, centrifuging at a high speed of 4000r/min for 10min, and removing precipitate to obtain pectin solution for later use;
(7) and (3) decoloring and concentrating: decolorizing the pectin solution with macroporous cation resin, and vacuum concentrating in a vacuum concentrating device to 1/5 of the original volume to obtain concentrated solution;
(8) freeze-drying and crushing: freeze-drying the concentrated solution at-5 deg.C, taking out, recovering to normal temperature, grinding, pulverizing, and sieving with 80 mesh sieve to obtain pectin.
Example 2:
a high-efficiency pectin extraction process comprises the following steps:
(1) pretreatment of raw materials: selecting fresh citrus pomace, adding deionized water with the mass of 3 times, grinding into slurry, ultrasonically homogenizing for 10min at the frequency of 40kHz, placing the slurry in a high-pressure reaction kettle under the pressure of 18MPa and at the temperature of 95 ℃, and carrying out enzyme deactivation treatment for 5s to obtain enzyme deactivation homogenized slurry for later use;
(2) mixing phytochelatin: adding phytochelatin into the enzyme-deactivated homogeneous slurry according to the mass ratio of 100: 0.03, uniformly stirring, and stirring for 3 hours at the water bath temperature of 45 ℃ at the rotating speed of 60r/min to obtain a mixture for later use;
(3) boiling treatment: adding deionized water into the mixture, heating and boiling for 20min, continuously stirring the slurry at a rotating speed of 40r/min in the boiling process, and taking out to obtain boiled slurry for later use;
(4) freezing and re-melting: placing the boiled pulp in a liquid nitrogen environment for quick freezing, then placing the boiled pulp in a reaction kettle, and introducing high-temperature hot steam of 120 ℃ for 40min inwards for melting treatment to obtain melted pulp for later use;
(5) and (3) enzymolysis treatment: mixing the melted slurry with cellulase, hemicellulase, glycosidase and amylase according to the mass ratio of 100: 0.08: 0.14: 0.06: 0.2, uniformly stirring, adjusting the pH to 5.0, and performing enzymolysis for 4 hours at the water bath temperature of 50 ℃ to obtain an enzymolysis liquid for later use;
(6) centrifugal filtration: placing the enzymolysis solution in a centrifuge, centrifuging at high speed of 5000r/min for 15min, and removing precipitate to obtain pectin solution;
(7) and (3) decoloring and concentrating: decolorizing the pectin solution with macroporous cation resin, and vacuum concentrating in a vacuum concentrating device to 1/8 of the original volume to obtain concentrated solution;
(8) freeze-drying and crushing: freeze-drying the concentrated solution at a low temperature of-10 ℃, taking out the concentrated solution, recovering to normal temperature, grinding, crushing and sieving with a 80-mesh sieve to obtain the pectin.
Example 3:
a high-efficiency pectin extraction process comprises the following steps:
(1) pretreatment of raw materials: selecting fresh citrus pomace, adding deionized water with the mass of 3 times, grinding into slurry, ultrasonically homogenizing for 10min at the frequency of 40kHz, placing the slurry in a high-pressure reaction kettle under the pressure of 16MPa and at the temperature of 90 ℃, and carrying out enzyme deactivation treatment for 3s to obtain enzyme deactivation homogenized slurry for later use;
(2) mixing phytochelatin: adding phytochelatin into the enzyme-deactivated homogeneous slurry according to the mass ratio of 100: 0.02, uniformly stirring, and stirring at the water bath temperature of 40 ℃ for 2 hours at the rotating speed of 50r/min to obtain a mixture for later use;
(3) boiling treatment: adding deionized water into the mixture, heating and boiling for 15min, continuously stirring the slurry at a rotating speed of 30r/min in the boiling process, and taking out to obtain boiled slurry for later use;
(4) freezing and re-melting: placing the boiled pulp in a liquid nitrogen environment for quick freezing, then placing the boiled pulp in a reaction kettle, and introducing high-temperature hot steam of 115 ℃ for 35min inwards for carrying out melting treatment to obtain melted pulp for later use;
(5) and (3) enzymolysis treatment: mixing the melted slurry with cellulase, hemicellulase, glycosidase and amylase according to the mass ratio of 100: 0.07: 0.12: 0.04: 0.15, stirring uniformly, adjusting the pH to 5.0, and performing enzymolysis for 3 hours at the water bath temperature of 40 ℃ to obtain an enzymolysis solution for later use;
(6) centrifugal filtration: placing the enzymolysis solution in a centrifuge, centrifuging at a high speed of 4500r/min for 13min, and removing precipitate to obtain pectin solution;
(7) and (3) decoloring and concentrating: decolorizing the pectin solution with macroporous cation resin, and vacuum concentrating in a vacuum concentrating device to 1/7 of the original volume to obtain concentrated solution;
(8) freeze-drying and crushing: freeze-drying the concentrated solution at a low temperature of-8 ℃, taking out the concentrated solution, recovering to normal temperature, grinding, crushing and sieving with a 80-mesh sieve to obtain the pectin.
Comparative example 1:
the pectin extraction process comprises the following steps:
(1) pretreatment of raw materials: selecting fresh citrus pomace, adding deionized water with the mass of 3 times, grinding into slurry, ultrasonically homogenizing for 10min at the frequency of 40kHz, placing the slurry in a high-pressure reaction kettle under the pressure of 16MPa and at the temperature of 90 ℃, and carrying out enzyme deactivation treatment for 3s to obtain enzyme deactivation homogenized slurry for later use;
(2) boiling treatment: adding deionized water into the enzyme-deactivated homogenized pulp, heating and boiling for 15min, continuously stirring the pulp at a rotating speed of 30r/min in the boiling process, and taking out to obtain boiled pulp for later use;
(3) freezing and re-melting: placing the boiled pulp in a liquid nitrogen environment for quick freezing, then placing the boiled pulp in a reaction kettle, and introducing high-temperature hot steam of 115 ℃ for 35min inwards for carrying out melting treatment to obtain melted pulp for later use;
(4) and (3) enzymolysis treatment: mixing the melted slurry with cellulase, hemicellulase, glycosidase and amylase according to the mass ratio of 100: 0.07: 0.12: 0.04: 0.15, stirring uniformly, adjusting the pH to 5.0, and performing enzymolysis for 3 hours at the water bath temperature of 40 ℃ to obtain an enzymolysis solution for later use;
(5) centrifugal filtration: placing the enzymolysis solution in a centrifuge, centrifuging at a high speed of 4500r/min for 13min, and removing precipitate to obtain pectin solution;
(6) and (3) decoloring and concentrating: decolorizing the pectin solution with macroporous cation resin, and vacuum concentrating in a vacuum concentrating device to 1/7 of the original volume to obtain concentrated solution;
(7) freeze-drying and crushing: freeze-drying the concentrated solution at a low temperature of-8 ℃, taking out the concentrated solution, recovering to normal temperature, grinding, crushing and sieving with a 80-mesh sieve to obtain the pectin.
Comparative example 2:
the pectin extraction process comprises the following steps:
(1) pretreatment of raw materials: selecting fresh citrus pomace, adding deionized water with the mass of 3 times, grinding into slurry, ultrasonically homogenizing for 10min at the frequency of 40kHz, placing the slurry in a high-pressure reaction kettle under the pressure of 16MPa and at the temperature of 90 ℃, and carrying out enzyme deactivation treatment for 3s to obtain enzyme deactivation homogenized slurry for later use;
(2) mixing phytochelatin: adding phytochelatin into the enzyme-deactivated homogeneous slurry according to the mass ratio of 100: 0.02, uniformly stirring, and stirring at the water bath temperature of 40 ℃ for 2 hours at the rotating speed of 50r/min to obtain a mixture for later use;
(3) boiling treatment: adding deionized water into the mixture, heating and boiling for 15min, continuously stirring the slurry at a rotating speed of 30r/min in the boiling process, and taking out to obtain boiled slurry for later use;
(4) and (3) enzymolysis treatment: mixing the boiled pulp with cellulase, hemicellulase, glycosidase and amylase according to the mass ratio of 100: 0.07: 0.12: 0.04: 0.15, uniformly stirring, adjusting the pH to 5.0, and performing enzymolysis for 3 hours at the water bath temperature of 40 ℃ to obtain an enzymolysis liquid for later use;
(5) centrifugal filtration: placing the enzymolysis solution in a centrifuge, centrifuging at a high speed of 4500r/min for 13min, and removing precipitate to obtain pectin solution;
(6) and (3) decoloring and concentrating: decolorizing the pectin solution with macroporous cation resin, and vacuum concentrating in a vacuum concentrating device to 1/7 of the original volume to obtain concentrated solution;
(7) freeze-drying and crushing: freeze-drying the concentrated solution at a low temperature of-8 ℃, taking out the concentrated solution, recovering to normal temperature, grinding, crushing and sieving with a 80-mesh sieve to obtain the pectin.
Comparative example 3:
a high-efficiency pectin extraction process comprises the following steps:
(1) pretreatment of raw materials: selecting fresh citrus pomace, adding deionized water with the mass of 3 times, grinding into slurry, ultrasonically homogenizing for 10min at the frequency of 40kHz, placing the slurry in a high-pressure reaction kettle under the pressure of 16MPa and at the temperature of 90 ℃, and carrying out enzyme deactivation treatment for 3s to obtain enzyme deactivation homogenized slurry for later use;
(2) mixing phytochelatin: adding phytochelatin into the enzyme-deactivated homogeneous slurry according to the mass ratio of 100: 0.02, uniformly stirring, and stirring at the water bath temperature of 40 ℃ for 2 hours at the rotating speed of 50r/min to obtain a mixture for later use;
(3) boiling treatment: adding deionized water into the mixture, heating and boiling for 15min, continuously stirring the slurry at a rotating speed of 30r/min in the boiling process, and taking out to obtain boiled slurry for later use;
(4) freezing and re-melting: placing the boiled pulp in a liquid nitrogen environment for quick freezing, and then carrying out normal-temperature melting treatment to obtain melted pulp for later use;
(5) and (3) enzymolysis treatment: mixing the melted slurry with cellulase, hemicellulase, glycosidase and amylase according to the mass ratio of 100: 0.07: 0.12: 0.04: 0.15, stirring uniformly, adjusting the pH to 5.0, and performing enzymolysis for 3 hours at the water bath temperature of 40 ℃ to obtain an enzymolysis solution for later use;
(6) centrifugal filtration: placing the enzymolysis solution in a centrifuge, centrifuging at a high speed of 4500r/min for 13min, and removing precipitate to obtain pectin solution;
(7) and (3) decoloring and concentrating: decolorizing the pectin solution with macroporous cation resin, and vacuum concentrating in a vacuum concentrating device to 1/7 of the original volume to obtain concentrated solution;
(8) freeze-drying and crushing: freeze-drying the concentrated solution at a low temperature of-8 ℃, taking out the concentrated solution, recovering to normal temperature, grinding, crushing and sieving with a 80-mesh sieve to obtain the pectin.
And (3) detection:
the yields of extracted pectin obtained in examples 1 to 3 and comparative examples 1 to 3 were measured, respectively, and the results are shown in the following table:
as can be seen from the table above, the addition, low-temperature freezing and high-temperature re-melting of phytochelatin can effectively improve the yield of pectin, and the comprehensive yield can reach the corresponding range of ethanol precipitation.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
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 (10)
1. The high-efficiency pectin extraction process is characterized by comprising the following steps:
(1) pretreatment of raw materials: selecting fresh pomace, adding deionized water, grinding into slurry, ultrasonically homogenizing, and then placing in a high-pressure reaction kettle at 85-95 ℃ under the pressure of 14-18MPa for enzyme deactivation treatment to obtain enzyme-deactivated homogenized slurry for later use;
(2) mixing phytochelatin: adding the enzyme-deactivated homogeneous slurry into plant chelating peptide, stirring uniformly, and stirring for 1-3h at the water bath temperature of 30-45 ℃ to obtain a mixture for later use;
(3) boiling treatment: adding deionized water into the mixture, heating and boiling for 10-20min, and taking out to obtain boiled slurry for later use;
(4) freezing and re-melting: placing the boiled pulp in a liquid nitrogen environment for quick freezing, then placing the boiled pulp in a reaction kettle, and introducing high-temperature hot steam inwards for melting treatment to obtain melted pulp for later use;
(5) and (3) enzymolysis treatment: adding cellulase, hemicellulase, glycosidase and amylase into the melted slurry, stirring uniformly, adjusting pH to 4.0-5.0, and placing in a water bath at 30-50 deg.C for enzymolysis for 2-4h to obtain an enzymolysis solution for later use;
(6) centrifugal filtration: placing the enzymolysis liquid in a centrifuge for high-speed centrifugation, and removing precipitates to obtain a pectin liquid for later use;
(7) and (3) decoloring and concentrating: decolorizing the pectin solution with macroporous cation resin, and vacuum concentrating in a vacuum concentrating device to obtain concentrated solution;
(8) freeze-drying and crushing: freeze-drying the concentrated solution at low temperature, taking out, recovering to normal temperature, grinding, and pulverizing to obtain pectin.
2. The high-efficiency pectin extraction process according to claim 1, characterized by comprising the following steps: the fresh pomace in the step (1) is apple peel or citrus peel pomace.
3. The high-efficiency pectin extraction process according to claim 1, characterized by comprising the following steps: in the step (1), the mixing mass ratio of the fresh pomace to the deionized water is 1: 3, the ultrasonic homogenization frequency is 40kHz, the homogenization time is 10min, and the enzyme deactivation time is 1-5 s.
4. The high-efficiency pectin extraction process according to claim 1, characterized by comprising the following steps: in the step (2), the mass ratio of the enzyme-inactivating homogeneous slurry to the phytochelatin is 100: 0.01-0.03, and the rotation speed of the heat-preservation stirring is 40-60 r/min.
5. The high-efficiency pectin extraction process according to claim 1, characterized by comprising the following steps: and (4) continuously stirring the pulp at a rotating speed of 20-40r/min in the boiling process in the step (3).
6. The high-efficiency pectin extraction process according to claim 1, characterized by comprising the following steps: the temperature of the high-temperature steam in the step (4) is 110-120 ℃, and the time for introducing the hot steam is 30-40 min.
7. The high-efficiency pectin extraction process according to claim 1, characterized by comprising the following steps: the mass ratio of the melted slurry to the cellulase, the hemicellulase, the glycosidase and the amylase in the step (5) is 100: 0.06-0.08: 0.1-0.14: 0.02-0.06: 0.1-0.2.
8. The high-efficiency pectin extraction process according to claim 1, characterized by comprising the following steps: the rotation speed of the centrifugation in the step (6) is 4000-.
9. The high-efficiency pectin extraction process according to claim 1, characterized by comprising the following steps: the concentrated solution obtained in the step (7) is 1/5-1/8 in original volume.
10. The high-efficiency pectin extraction process according to claim 1, characterized by comprising the following steps: the low-temperature freeze-drying temperature in the step (8) is 5-10 ℃ below zero, and the pectin after grinding is sieved by a 80-mesh sieve.
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