CN112863994B - Device and method for modifying pectin by using dielectric barrier discharge cold plasma - Google Patents

Device and method for modifying pectin by using dielectric barrier discharge cold plasma Download PDF

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CN112863994B
CN112863994B CN202110118813.0A CN202110118813A CN112863994B CN 112863994 B CN112863994 B CN 112863994B CN 202110118813 A CN202110118813 A CN 202110118813A CN 112863994 B CN112863994 B CN 112863994B
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pectin
chamber
cold plasma
solution
control
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CN112863994A (en
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孙大文
潘雅雯
成军虎
韩忠
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South China University of Technology SCUT
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South China University of Technology SCUT
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32Gas-filled discharge tubes
    • H01J37/32009Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
    • H01J37/32348Dielectric barrier discharge
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/20Reducing nutritive value; Dietetic products with reduced nutritive value
    • A23L33/21Addition of substantially indigestible substances, e.g. dietary fibres
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

Abstract

The invention belongs to the technical field of preparation of bioactive polysaccharides, and discloses a device for modifying pectin by using dielectric barrier discharge cold plasma, which comprises: consecutive first control room, solution prepare room, cold plasma processing chamber, drying chamber and second control room, wherein: the first control chamber is used for controlling the solution preparation chamber to prepare uniform pectin solution with specified concentration; the solution preparation chamber is provided with a first electric stirrer, and the uniformly stirred and dispersed pectin solution flows to the cold plasma treatment chamber through a control valve; the cold plasma chamber comprises a cold plasma generating device, a filter screen and a second electric stirrer, the cold plasma processing chamber is connected with a second control chamber, and the second control chamber is used for controlling the working parameters of the cold plasma generating device in the cold plasma processing chamber and lifting the filter screen. The modified pectin device has the advantages of greenness, safety, high efficiency, low cost and the like. The invention also provides a method for modifying pectin by using the dielectric barrier discharge cold plasma.

Description

Device and method for modifying pectin by using dielectric barrier discharge cold plasma
Technical Field
The invention belongs to the technical field of preparation of bioactive polysaccharides, and relates to a device and a method for modifying pectin by using dielectric barrier discharge cold plasma.
Background
Pectin is a kind of plant polysaccharide substance, and the source of the pectin is very wide, and the pectin is usually present in a large amount in peels of oranges, apples, grapefruits and the like, and is the most abundant source of the pectin. The FAO/WHO combined food additive committee recommended citrus pectin as a safe natural food additive and did not limit its daily allowable intake. At present, pectin is widely applied to the fields of food, cosmetics, chemical industry, textile, medicine and the like, and has various physiological and nutritional effects of reducing blood sugar, serum cholesterol, stimulating macrophages, resisting inflammation, preventing cancers and the like as a dietary fiber. The annual demand for pectin is now around 4 million tons worldwide and is growing every year. In China, the annual consumption of pectin is about 5000 tons, and 80% of pectin depends on import.
The natural pectin has large molecular weight and is not easy to digest, thereby limiting the application of the natural pectin in various aspects such as biological function and the like, and has higher requirements on the esterification degree, the molecular weight and the galacturonic acid content of the pectin in the medical and health care industries. Therefore, the demand for modified pectin is a hot topic in recent years. The modification of pectin is a structural modification method mainly aiming at reducing the molecular weight and the esterification degree. The existing pectin modification methods comprise chemical modification (adjusting pH and temperature conditions), enzyme modification and thermal modification (adjusting temperature and air pressure conditions and the like). Most of pectin on the market is prepared by a chemical modification method, but the preparation method is complex and has great harm to the environment, complex process and long time consumption, and the enzyme modification method is unstable and expensive and has high dependence on the specificity, purity and activity of the enzyme. The thermal modification method has high production cost due to high requirements on equipment. In recent years, ultrasonic-assisted modified pectin is also researched, but compared with a plasma technology, the operation is still more complicated and time-consuming, ultrasonic treatment is required for 30-150min, pH is adjusted, ethanol is used for precipitation and dialysis, and then freeze drying is carried out. Thus, the existing pectin modification methods have more or less considerable disadvantages.
Disclosure of Invention
Aiming at the defects and shortcomings in the prior art, the invention provides a device for modifying pectin by using dielectric barrier discharge cold plasma, belonging to a novel pectin physical modification device.
The invention also provides a method for modifying pectin by using the dielectric barrier discharge cold plasma.
The device for modifying pectin by using dielectric barrier discharge cold plasma is realized by adopting the following technical scheme:
a device for modifying pectin by using dielectric barrier discharge cold plasma comprises: consecutive first control room, solution prepare room, cold plasma processing chamber, drying chamber and second control room, wherein:
the first control chamber is used for controlling the solution preparation chamber to prepare uniform pectin solution with specified concentration; the solution preparation chamber is provided with a first electric stirrer, and the uniformly stirred and dispersed pectin solution flows to the cold plasma treatment chamber through a control valve;
the cold plasma chamber comprises a cold plasma generating device, a filter screen and a second electric stirrer, wherein: the cold plasma generating device comprises a lifting platform, two electrode plates and a medium plate, wherein the lifting platform is used for adjusting the proper discharge distance between the two electrode plates according to the concentration of the pectin solution; the second electric stirrer enables the cold plasma treatment to be more uniform, after the treatment is finished, the filter screen is lifted, and the treated pectin solution flows to the drying chamber through the pipeline after being filtered;
the cold plasma processing chamber is connected with a second control chamber, and the second control chamber is used for controlling the working parameters of the cold plasma generating device in the cold plasma processing chamber and lifting the filter screen.
Preferably, the first control chamber is provided with a first control disc and a second control disc, the first control disc controls the injection amount of the deionized water, and the second control disc controls the addition amount of the pectin.
Preferably, the discharge distance between the two electrode plates is 0-5 cm.
Preferably, the processing voltage of the cold plasma generating device is 30-70kV, and the processing time is 1-4 min.
The method for modifying pectin by using dielectric barrier discharge cold plasma is realized by adopting the following technical scheme:
a method for modifying pectin by using dielectric barrier discharge cold plasma comprises the following steps:
the method comprises the steps of preparing uniform pectin solution with specified concentration in a solution preparation chamber by controlling the content of pectin and deionized water in a first control chamber, starting a first electric stirrer to uniformly mix the pectin solution, introducing the uniformly mixed pectin solution into a cold plasma treatment chamber through a valve, adjusting the discharge distance between two electrode plates and fixing the height.
And setting the treatment voltage and treatment time of the cold plasma treatment chamber through the second control chamber, starting the second electric stirrer, lifting the filter screen after treatment, closing the plasma treatment chamber equipment after filtration, lowering the filter screen, and introducing the pectin solution into the drying chamber through a pipeline for drying to obtain the modified pectin.
Preferably, the pectin is a high methoxyl pectin having a degree of esterification greater than 50% and a galacturonic acid content greater than or equal to 74%.
Preferably, the pectin source is citrus, apple or grapefruit.
Preferably, the pectin solution has a concentration of 0.1% to 0.5%.
Preferably, the discharge distance between the two electrode plates is 0-5 cm; the processing voltage of the cold plasma generating device in the cold plasma processing chamber is 30-70kV, and the processing time is 1-4 min.
Preferably, the pectin solution is passed into a drying chamber and the drying process comprises vacuum drying, freeze drying and spray drying.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the invention innovatively provides a novel modified pectin obtained by modifying pectin by using a dielectric barrier discharge cold plasma method, researches on galacturonic acid, esterification degree and molecular weight change of the pectin, and provides more theoretical supports for the pectin research field.
(2) The dielectric barrier discharge cold plasma method adopted by the invention is a novel non-thermal physical processing method, is green, safe and efficient, has less energy consumption and low cost. The method can obtain enough samples by processing the samples, and has the advantages of lower cost, environmental friendliness, simple and convenient operation and rapidness compared with the traditional processing method.
(3) The average molecular weight of the modified pectin prepared by the method is 20-70kDa, the lowest esterification degree is 38 percent, and the highest uronic acid content is 94 percent, which indicates that the invention is an economic and efficient pectin modification method. The obtained modified pectin has good application potential in the fields of medicine, health food and the like.
(4) Compared with the existing chemical method, enzymatic method and thermal modification method, the method has the advantages of short reaction time, simple and convenient operation, no pollution and environmental friendliness.
(5) The prior art can not simultaneously realize two degradation targets of pectin molecular weight degradation and pectin deesterification, or deesterification is not considered; the preparation method of the invention can simultaneously realize two modification targets of pectin degradation and degreasing, and improve the functional property of pectin.
(6) The method of the invention is different from the existing pectin modification method, although the existing modification method can meet the requirements, the chemical method is time-consuming, environment-friendly and the subsequent treatment is complicated; the enzyme method is expensive, has strong specificity and is difficult to control, thereby limiting the application of the enzyme method in industry. The method has the advantages of short treatment time, environmental friendliness, simple subsequent treatment and low cost.
(7) The method of the invention is different from the prior physical modification method of pectin, and the prior physical modification method has long reaction time and limited effect. The method of the invention greatly shortens the reaction time, reduces the molecular weight and the esterification degree of the product, and improves the content of galacturonic acid.
Drawings
FIG. 1 is a schematic structural diagram of an embodiment of an apparatus for cold plasma modification of pectin using dielectric barrier discharge.
Fig. 2 is a left side view of a dielectric barrier discharge cold plasma processing chamber in one embodiment.
Fig. 3 is a cross-sectional view of a dbd cold plasma processing chamber according to an embodiment, where fig. 3(a) shows a filter screen in a lowered state and fig. 3(b) shows a filter screen in a raised state.
FIG. 4 is a graph showing the change in the galacturonic acid content of a dielectric barrier discharge cold plasma treated pectin solution in one embodiment; the treatment time of FIG. 4(a) was 2 minutes; the processing voltage of fig. 4(b) was 40 KV.
FIG. 5 is a graph showing the variation of the degree of esterification in a dielectric barrier discharge cold plasma treated pectin solution in one embodiment; the treatment time of FIG. 5(a) was 2 minutes; the processing voltage of FIG. 5(b) was 40 kV.
Detailed Description
The following describes specific embodiments of the present invention with reference to examples, but the embodiments of the present invention are not limited thereto.
A device for modifying pectin by using dielectric barrier discharge cold plasma, as shown in figures 1-3, comprises: a solution preparation chamber 1, a cold plasma processing chamber 2, a drying chamber 3, a first control chamber 9 and a second control chamber 6, wherein:
the solution preparation chamber 1 is provided with a first electric stirrer 4, a first control chamber 9 is used for preparing a uniform pectin solution with a designated concentration, the first control chamber 9 is provided with a first control disk 10 and a second control disk 11, the first control disk 10 controls the injection amount of deionized water, and the second control disk 11 controls the addition amount of pectin. The evenly stirred and dispersed pectin solution flows to the cold plasma processing chamber 2 through a control valve 5.
The cold plasma chamber 2 comprises a cold plasma generating device, a filter screen 12 and a second electric stirrer 7, wherein: the cold plasma generating device comprises a lifting platform 13, two electrode plates 14 and a medium plate 15, wherein the lifting platform 13 is used for adjusting the proper discharge distance between the two electrode plates according to the concentration of the pectin solution; the second electric stirrer 7 enables the cold plasma treatment to be more uniform, after the treatment is finished, the filter screen 12 is lifted, and the treated pectin solution flows to the drying chamber 3 through the pipeline 8 after being filtered.
The cold plasma processing chamber 2 is connected with a second control chamber 6, and the second control chamber 6 is used for controlling the working parameters of the cold plasma generating device in the cold plasma processing chamber and lifting the filter screen 12.
A method for modifying pectin by using dielectric barrier discharge cold plasma comprises the following steps:
the method comprises the steps of preparing uniform pectin solution with specified concentration in a solution preparation chamber by controlling the content of pectin and deionized water in a first control chamber, starting a first electric stirrer to uniformly mix the pectin solution, introducing the uniformly mixed pectin solution into a cold plasma treatment chamber through a valve, adjusting the discharge distance between two electrode plates and fixing the height.
And setting the treatment voltage and treatment time of the cold plasma treatment chamber through the second control chamber, starting the second electric stirrer, lifting the filter screen after treatment, closing the plasma treatment chamber equipment after filtration, lowering the filter screen, and introducing the pectin solution into the drying chamber through a pipeline for drying to obtain the modified pectin.
In a preferred embodiment, the pectin is a high methoxyl pectin having a degree of esterification greater than 50% and a galacturonic acid content of 74% or greater. The pectin source is citrus, apple or grapefruit.
The concentration of the pectin solution is 0.1-0.5%.
The discharge interval is 0-5 cm.
The processing voltage of the cold plasma processing chamber is 30-70kV, and the processing time is 1-4 min.
After the pectin solution is introduced into the drying chamber, the drying method comprises vacuum drying, freeze drying and spray drying.
Example 1
And (3) preparing a 0.2% pectin solution through the first control chamber, opening the first electric stirrer, introducing the uniformly mixed pectin solution into the cold plasma treatment chamber through a valve, adjusting the discharge distance between the two electrode plates and fixing the height. Setting the processing voltage of the cold plasma processing chamber to be 40kV and the processing time to be 2min through the second control chamber, starting the second electric stirrer, lifting the filter screen after the processing is finished, closing the plasma equipment after the filtering is finished, lowering the filter screen, introducing the pectin solution into the drying chamber through a pipeline, and selecting freeze drying, wherein the yield of the pectin product is 100%.
The molecular weight of citrus pectin before modification in this example was 700kDa, the uronic acid content was 74%, and the degree of esterification was 55%; the pectin obtained by the modification method has the molecular weight of 100kDa, the uronic acid content of 94 percent and the esterification degree of 38 percent.
Example 2
And (3) preparing a 0.2% pectin solution through the first control chamber, opening the first electric stirrer, introducing the uniformly mixed pectin solution into the cold plasma treatment chamber through a valve, adjusting the discharge distance between the two electrode plates and fixing the height. The processing voltage of the cold plasma processing chamber is set to be 70kV through the second control chamber, the processing time is set to be 2min, and the second electric stirrer is started. After the treatment is finished, the filter screen is lifted, after the filtration is finished, the plasma equipment is closed, the filter screen is lowered, the pectin solution is introduced into the drying chamber through a pipeline, and freeze drying is selected, so that the pectin yield is 90%.
The molecular weight of citrus pectin before modification in this example was 700kDa, the uronic acid content was 74%, and the degree of esterification was 55%; the pectin obtained by the modification method has the molecular weight of 60kDa, the uronic acid content of 84 percent and the esterification degree of 45 percent.
Example 3
And (3) preparing a 0.4% pectin solution through the first control chamber, opening the first electric stirrer, introducing the uniformly mixed pectin solution into the cold plasma treatment chamber through a valve, adjusting the discharge distance between the two electrode plates and fixing the height. The processing voltage of the cold plasma processing chamber is set to be 40kV through the second control chamber, the processing time is set to be 2min, and the second electric stirrer is started. And after the treatment is finished, lifting the filter screen, closing the plasma equipment after the filtration is finished, lowering the filter screen, introducing the pectin solution into a drying chamber through a pipeline, and selectively freeze-drying to obtain the pectin yield of 100%.
The molecular weight of citrus pectin before modification in this example was 700kDa, the uronic acid content was 74%, and the degree of esterification was 55%; the pectin obtained by the modification method has the molecular weight of 200kDa, the uronic acid content of 86 percent and the esterification degree of 43 percent.
Example 4
And (3) preparing a 0.1% pectin solution through the first control chamber, opening the first electric stirrer, introducing the uniformly mixed pectin solution into the cold plasma treatment chamber through a valve, adjusting the discharge distance between the two electrode plates and fixing the height. The processing voltage of the cold plasma processing chamber is set to be 40kV through the second control chamber, the processing time is set to be 2min, and the second electric stirrer is started. And after the treatment is finished, lifting the filter screen, closing the plasma equipment after the filtration is finished, lowering the filter screen, introducing the pectin solution into a drying chamber through a pipeline, and selectively freeze-drying to obtain the pectin yield of 100%.
The molecular weight of citrus pectin before modification in this example was 700kDa, the uronic acid content was 74%, and the degree of esterification was 55%; the pectin obtained by the modification method has the molecular weight of 400kDa, the uronic acid content of 84 percent and the esterification degree of 41 percent.
Description of the drawings: the treatment time of FIG. 4(a) was 2 minutes; the processing voltage of FIG. 4(b) is 40 KV; the treatment time of FIG. 5(a) was 2 minutes; the processing voltage of FIG. 5(b) was 40 kV. The results for uronic acid and degree of esterification mentioned in example 1 and example 2 correspond to the results for the treatment conditions in fig. 4 and fig. 5, respectively, for a pectin concentration of 0.2% (2mg/mL), a treatment time of 2min, and a treatment voltage of 40kV and 70kV, respectively. The results mentioned in example 3 for uronic acid and degree of esterification correspond to the results for the conditions in fig. 4 and 5 for a pectin concentration of 0.4% (4mg/mL), a treatment time of 2min and a treatment voltage of 40 kV.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (7)

1. A device for modifying pectin by using dielectric barrier discharge cold plasma is characterized by comprising: consecutive first control room, solution prepare room, cold plasma processing chamber, drying chamber and second control room, wherein:
the first control chamber is used for controlling the solution preparation chamber to prepare uniform pectin solution with specified concentration; the solution preparation chamber is provided with a first electric stirrer, and the uniformly stirred and dispersed pectin solution flows to the cold plasma treatment chamber through a control valve;
the cold plasma chamber comprises a cold plasma generating device, a filter screen and a second electric stirrer, wherein: the cold plasma generating device comprises a lifting platform, two electrode plates and a medium plate, wherein the lifting platform is used for adjusting the discharge distance between the two electrode plates according to the concentration of the pectin solution; the second electric stirrer enables the cold plasma treatment to be more uniform, after the treatment is finished, the filter screen is lifted, and the treated pectin solution flows to the drying chamber through the pipeline after being filtered;
the cold plasma processing chamber is connected with a second control chamber, and the second control chamber is used for controlling the working parameters of the cold plasma generating device in the cold plasma processing chamber and lifting the filter screen;
the first control chamber is provided with a first control disc and a second control disc, the first control disc controls the injection amount of the deionized water, and the second control disc controls the addition amount of the pectin;
the discharge distance between the two electrode plates is 0-5 cm;
the pectin is high methoxyl pectin with esterification degree higher than 50% and galacturonic acid content higher than or equal to 74%.
2. The device according to claim 1, wherein the treatment voltage of the cold plasma generating device is 30-70kV, and the treatment time is 1-4 min.
3. A method for modifying pectin by using dielectric barrier discharge cold plasma, which is realized based on the device for modifying pectin by using dielectric barrier discharge cold plasma as claimed in any one of claims 1-2, and comprises the following steps:
controlling the content of pectin and deionized water in a solution preparation chamber through a first control chamber to prepare uniform pectin solution with specified concentration, starting a first electric stirrer to uniformly mix the pectin solution, introducing the uniformly mixed pectin solution into a cold plasma treatment chamber through a valve, adjusting the discharge distance between two electrode plates and fixing the height;
and setting the treatment voltage and treatment time of the cold plasma treatment chamber through the second control chamber, starting the second electric stirrer, lifting the filter screen after treatment, closing the plasma treatment chamber equipment after filtration, lowering the filter screen, and introducing the pectin solution into the drying chamber through a pipeline for drying to obtain the modified pectin.
4. A method according to claim 3, wherein the pectin source is citrus, apple or grapefruit.
5. The method according to claim 3, wherein the pectin solution has a concentration of 0.1% to 0.5%.
6. The method of claim 4, wherein the processing voltage of the cold plasma generating device in the cold plasma processing chamber is 30-70kV and the processing time is 1-4 min.
7. The method of claim 3, wherein the pectin solution is dried in a drying chamber, the drying method comprising vacuum drying, freeze drying, and spray drying.
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US20080179286A1 (en) * 2007-01-29 2008-07-31 Igor Murokh Dielectric plasma chamber apparatus and method with exterior electrodes
US9192776B2 (en) * 2007-04-23 2015-11-24 Plasmology4, Inc. Harmonic cold plasma devices and associated methods
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CN106632724B (en) * 2016-12-23 2019-03-05 浙江大学 A method of efficiently preparing low molecular weight pectin
CN112087853A (en) * 2019-06-12 2020-12-15 中国石油化工股份有限公司 Plasma generating apparatus and control method for plasma generating apparatus
CN110229241B (en) * 2019-06-21 2021-07-20 华南理工大学 Method for preparing potato hydroxypropyl starch based on cold plasma
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