CN108912243B - Process for extracting pectin from kiwi fruit peel residues - Google Patents
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- C08B37/0045—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Galacturonans, e.g. methyl ester of (alpha-1,4)-linked D-galacturonic acid units, i.e. pectin, or hydrolysis product of methyl ester of alpha-1,4-linked D-galacturonic acid units, i.e. pectinic acid; Derivatives thereof
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Abstract
The invention discloses a process for extracting pectin from kiwi fruit peel residues, and relates to the technical field of plant extraction. The invention comprises the following steps: the method comprises the steps of pretreatment of the skin slag, acid extraction, purification, concentration and pulverization, epoxy resin and chitosan are used as raw materials, adsorption resin is formed through an ionic crosslinking agent, a chitosan adsorption film in the resin and the resin has a good adsorption effect on pigments and impurities in the pectin, the impurity removal efficiency of the pectin is high, the resin can be recycled, and the method is economical and environment-friendly.
Description
The technical field is as follows:
the invention relates to the technical field of plant extraction, and particularly relates to a process for extracting pectin from kiwi fruit peel residues.
Background art:
pectin is a polysaccharide polymer, a constituent of cell walls, and exists with cellulose, and has a molecular weight of 1-40 ten thousand. The pectin product is a powdery substance, and has light white or light yellow color, and can be used for preparing jam and jelly, and also can be used for preparing fruity cotton candy, crystal soft candy, sand-mixed soft candy, and sugar-free candy. Pectin and pectin aluminum salt can inhibit intestinal absorption of cholesterol and triglyceride, and can be used for adjuvant treatment of cardiovascular diseases such as arteriosclerosis.
The kiwi fruit peel residue is a byproduct of kiwi fruit after processing and extracting juice, and contains various substances such as soluble sugar, vitamins, mineral substances, cellulose and the like. At present, most of the skin slag is discarded as garbage, so that resources are greatly wasted and the environment is polluted.
The invention content is as follows:
the technical problem to be solved by the invention is to provide a pectin extraction process which is simple and easy to operate and can obviously improve the extraction rate and purity of pectin.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
a process for extracting pectin from Chinese gooseberry peel residues comprises the following steps:
(1) pretreatment of skin slag: soaking the kiwi fruit peel residues in 0.8-1.2% sodium carbonate solution for 1-3h, sterilizing and degreasing the peel residues, then sending the peel residues into a vacuum low-temperature cold air dryer, and drying the peel residues at the temperature of 32-35 ℃ until the moisture content of the peel residues is 25-32%;
(2) acid extraction: grinding and crushing the skin slag, adding deionized water, and mixing the materials according to a material-liquid ratio of 1: 5-10, adjusting the pH value to 1.5-2.0 by using an acidic solution, heating to 90-100 ℃, keeping the temperature, stirring for 1-2h, and filtering while hot to obtain a peel residue pectin extract; cooling the extractive solution to 50 deg.C, adding amylase 1-2% of the extractive solution, stirring and mixing for 20-30min, and heating to 80 deg.C to inactivate enzyme;
(3) and (3) purification: decoloring the extract liquid after enzyme deactivation in the step 2 by using adsorption resin, and removing impurities;
(4) concentration: heating the purified extractive solution to 50-55 deg.C, ultrafiltering with tubular polyacrylonitrile membrane ultrafilter with cut molecular weight of 50000u under pressure of 0.2Mpa, concentrating the purified extractive solution of pectin to content of 4.2-5.1% to obtain pectin concentrated solution;
(5) milling: and (3) carrying out spray drying on the pectin concentrated solution at the feeding temperature of 150-160 ℃ and the discharging temperature of 220-230 ℃ to obtain the pectin powder.
The preparation method of the adsorption resin comprises the following steps:
(1) putting the chitosan solid into a reaction kettle, and adding an acetic acid solution with the mass fraction of 5% to prepare a chitosan acetic acid solution for later use;
(2) adding epoxy chloropropane into anhydrous ethanol, heating to reflux state, stirring for 10-20min under heat preservation, adding trimethylolethane and initiator, and continuing to reflux and stir for 1-2 h; adding the chitosan acetic acid solution and the ionic crosslinking agent in the step 1, and continuously refluxing and stirring for 1-2 hours;
(3) and (3) adding a modifier into the system in the step (2), cooling to 50-55 ℃, fully mixing, performing microwave treatment for 5-10min at microwave frequency of 2450MHz and power of 700W, standing for 15-30min, continuing the microwave treatment for 5-10min, filtering, washing impurities in the precipitate by deionized water and absolute ethyl alcohol, and drying in a drying box at the temperature of 100 ℃ and 110 ℃ to constant weight to obtain the adsorption resin.
The mass ratio of the chitosan solid to the 5% acetic acid solution is 20-30: 30-50.
The mass ratio of the epichlorohydrin to the trimethylolethane to the initiator to the ionic crosslinking agent to the modifier is 10-15: 15-20: 1-5: 1-5: 1-5.
The initiator is selected from benzoyl peroxide or lauroyl peroxide.
The ionic crosslinking agent is selected from one of sodium pyrophosphate, sodium tripolyphosphate and tetrapolyphosphate.
The modifier is a mixture of tea polyphenol, sodium alginate and polyethylene glycol 400, and the mass ratio is 5-10: 5-10: 10-15.
The working principle of the modifier is as follows:
the tea polyphenol is a common additive in food, and can improve the aging resistance of the resin and prolong the service life of the resin; chitosan is a polycation polysaccharide, sodium alginate is a polyanion polysaccharide, and electrostatic polymerization reaction occurs between the chitosan and the polyanion polysaccharide to form a layer of film on the surface of the resin, so that impurities and pigments which are not adsorbed by the resin can be effectively prevented from flowing out of the adsorption resin; polyethylene glycol is a film forming auxiliary agent, and the structural stability of the adsorption resin can be improved through the action of hydrogen bonds, and the adsorption efficiency of the resin on other impurities and pigments can be improved.
The invention has the beneficial effects that:
(1) according to the invention, epoxy resin and chitosan are used as raw materials, and are cross-linked and polymerized to prepare adsorption resin through an ion cross-linking agent, a layer of chitosan adsorption film is formed inside the resin, and impurities and pigments in pectin can be completely adsorbed in the resin through double-layer adsorption of the resin and the adsorption film, so that the pectin has strong adsorption to the pigment and the structure of the pectin is not damaged;
(2) the modifier taking the tea polyphenol, the sodium alginate and the polyethylene glycol 400 as raw materials can improve the structural strength and the service life of the adsorption resin, and simultaneously can form a layer of sodium alginate electrolyte membrane on the surface of the resin to prevent impurities from flowing out, thereby further improving the purification efficiency;
(3) the method takes the kiwi fruit peel residues as the raw material to extract the pectin, changes waste into valuable, reduces the waste of resources, avoids environmental pollution, can repeatedly use the adsorption resin for purification, and is economic and environment-friendly.
The specific implementation mode is as follows:
in order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Example 1
(1) Pretreatment of skin slag: soaking 10kg of Chinese gooseberry peel residues in 1.2% sodium carbonate solution for 1h, sterilizing and degreasing the peel residues, then sending the peel residues into a vacuum low-temperature cold air dryer, and drying the peel residues at the temperature of 32 ℃ until the moisture content of the peel residues is 25% -32%;
(2) acid extraction: grinding and crushing the skin residue, adding 60kg of deionized water, adjusting the pH value to 1.5-2.0 by using an acid solution, heating to 90 ℃, preserving the temperature, stirring for 1h, and filtering while the mixture is hot to obtain a skin residue pectin extract; when the extract liquid is cooled to 50 ℃, adding amylase accounting for 1 percent of the weight of the extract liquid, stirring and mixing for 20min, and then heating to 80 ℃ to inactivate the enzyme;
(3) and (3) purification: decoloring the extract liquid after enzyme deactivation in the step 2 by using adsorption resin, and removing impurities;
(4) concentration: heating the purified extractive solution to 55 deg.C, ultrafiltering and concentrating under 0.2Mpa by tubular polyacrylonitrile membrane ultrafilter with cut molecular weight of 50000u, and concentrating the purified extractive solution of pectin to content of 4.2-5.1% to obtain pectin concentrated solution;
(5) milling: spray drying the pectin concentrated solution at a feeding temperature of 150 deg.C and a discharging temperature of 220 deg.C to obtain pectin powder.
Preparation of the adsorption resin:
(1) putting 22g of chitosan solid into a reaction kettle, and adding 35g of acetic acid solution with the mass fraction of 5% to prepare chitosan acetic acid solution for later use;
(2) adding 10g of epichlorohydrin into absolute ethyl alcohol, heating to a reflux state, keeping the temperature and stirring for 10min, then adding 15g of trimethylolethane and 2g of benzoyl peroxide, and continuing to stir for 1h under reflux; adding the chitosan acetic acid solution obtained in the step 1 and 2g of sodium pyrophosphate, and continuously refluxing and stirring for 1 h;
(3) and (3) adding 3g of modifier into the system in the step (2), cooling to 50 ℃, fully mixing, performing microwave treatment for 5min under the microwave frequency of 2450MHz and the power of 700W, standing for 15min, continuing the microwave treatment for 10min, filtering, washing impurities of the precipitate by deionized water and absolute ethyl alcohol, and drying in a drying box at the temperature of 100 ℃ and 110 ℃ to constant weight to obtain the adsorption resin.
Modifying agent: 5g of tea polyphenol, 5g of sodium alginate and 10g of polyethylene glycol 400.
Example 2
(1) Pretreatment of skin slag: soaking 10kg of Chinese gooseberry peel residues in 1.2% sodium carbonate solution for 1h, sterilizing and degreasing the peel residues, then sending the peel residues into a vacuum low-temperature cold air dryer, and drying the peel residues at the temperature of 32 ℃ until the moisture content of the peel residues is 25% -32%;
(2) acid extraction: grinding and crushing the skin residue, adding 60kg of deionized water, adjusting the pH value to 1.5-2.0 by using an acid solution, heating to 90 ℃, preserving the temperature, stirring for 1h, and filtering while the mixture is hot to obtain a skin residue pectin extract; when the extract liquid is cooled to 50 ℃, adding amylase accounting for 1 percent of the weight of the extract liquid, stirring and mixing for 20min, and then heating to 80 ℃ to inactivate the enzyme;
(3) and (3) purification: decoloring the extract liquid after enzyme deactivation in the step 2 by using adsorption resin, and removing impurities;
(4) concentration: heating the purified extractive solution to 55 deg.C, ultrafiltering and concentrating under 0.2Mpa by tubular polyacrylonitrile membrane ultrafilter with cut molecular weight of 50000u, and concentrating the purified extractive solution of pectin to content of 4.2-5.1% to obtain pectin concentrated solution;
(5) milling: spray drying the pectin concentrated solution at a feeding temperature of 150 deg.C and a discharging temperature of 220 deg.C to obtain pectin powder.
Preparation of the adsorption resin:
(1) putting 22g of chitosan solid into a reaction kettle, and adding 35g of acetic acid solution with the mass fraction of 5% to prepare chitosan acetic acid solution for later use;
(2) adding 10g of epichlorohydrin into absolute ethyl alcohol, heating to a reflux state, keeping the temperature and stirring for 10min, then adding 15g of trimethylolethane and 2g of benzoyl peroxide, and continuing to stir for 1h under reflux; adding the chitosan acetic acid solution obtained in the step 1 and 2g of sodium pyrophosphate, and continuously refluxing and stirring for 1 h;
(3) and (3) adding 3g of modifier into the system in the step (2), cooling to 50 ℃, fully mixing, performing microwave treatment for 5min under the microwave frequency of 2450MHz and the power of 700W, standing for 15min, continuing the microwave treatment for 10min, filtering, washing impurities of the precipitate by deionized water and absolute ethyl alcohol, and drying in a drying box at the temperature of 100 ℃ and 110 ℃ to constant weight to obtain the adsorption resin.
Modifying agent: 5g of tea polyphenol, 5g of sodium alginate and 10g of polyethylene glycol 400.
Comparative example 1
(1) Pretreatment of skin slag: soaking 10kg of Chinese gooseberry peel residues in 1.2% sodium carbonate solution for 1h, sterilizing and degreasing the peel residues, then sending the peel residues into a vacuum low-temperature cold air dryer, and drying the peel residues at the temperature of 32 ℃ until the moisture content of the peel residues is 25% -32%;
(2) acid extraction: grinding and crushing the skin residue, adding 60kg of deionized water, adjusting the pH value to 1.5-2.0 by using an acid solution, heating to 90 ℃, preserving the temperature, stirring for 1h, and filtering while the mixture is hot to obtain a skin residue pectin extract; when the extract liquid is cooled to 50 ℃, adding amylase accounting for 1 percent of the weight of the extract liquid, stirring and mixing for 20min, and then heating to 80 ℃ to inactivate the enzyme;
(3) and (3) purification: decoloring the extract liquid after enzyme deactivation in the step 2 by using adsorption resin, and removing impurities;
(4) concentration: heating the purified extractive solution to 55 deg.C, ultrafiltering and concentrating under 0.2Mpa by tubular polyacrylonitrile membrane ultrafilter with cut molecular weight of 50000u, and concentrating the purified extractive solution of pectin to content of 4.2-5.1% to obtain pectin concentrated solution;
(5) milling: spray drying the pectin concentrated solution at a feeding temperature of 150 deg.C and a discharging temperature of 220 deg.C to obtain pectin powder.
Preparation of the adsorption resin:
(1) adding 10g of epichlorohydrin into absolute ethyl alcohol, heating to a reflux state, keeping the temperature and stirring for 10min, then adding 15g of trimethylolethane and 2g of benzoyl peroxide, and continuing to stir for 1h under reflux; then 2g of sodium pyrophosphate is added, and the mixture is refluxed and stirred for 1 hour;
(2) and (3) adding 3g of modifier into the solution obtained in the step (2), cooling to 50 ℃, fully mixing, performing microwave treatment for 5min under the microwave frequency of 2450MHz and the power of 700W, standing for 15min, continuing the microwave treatment for 10min, filtering, washing out impurities from the precipitate by using deionized water and absolute ethyl alcohol, and drying in a drying box at the temperature of 100 ℃ and 110 ℃ to constant weight to obtain the adsorption resin.
Modifying agent: 5g of tea polyphenol, 5g of sodium alginate and 10g of polyethylene glycol 400.
Comparative example 2
(1) Pretreatment of skin slag: soaking 10kg of Chinese gooseberry peel residues in 1.2% sodium carbonate solution for 1h, sterilizing and degreasing the peel residues, then sending the peel residues into a vacuum low-temperature cold air dryer, and drying the peel residues at the temperature of 32 ℃ until the moisture content of the peel residues is 25% -32%;
(2) acid extraction: grinding and crushing the skin residue, adding 60kg of deionized water, adjusting the pH value to 1.5-2.0 by using an acid solution, heating to 90 ℃, preserving the temperature, stirring for 1h, and filtering while the mixture is hot to obtain a skin residue pectin extract; when the extract liquid is cooled to 50 ℃, adding amylase accounting for 1 percent of the weight of the extract liquid, stirring and mixing for 20min, and then heating to 80 ℃ to inactivate the enzyme;
(3) and (3) purification: decoloring the extract liquid after enzyme deactivation in the step 2 by using adsorption resin, and removing impurities;
(4) concentration: heating the purified extractive solution to 55 deg.C, ultrafiltering and concentrating under 0.2Mpa by tubular polyacrylonitrile membrane ultrafilter with cut molecular weight of 50000u, and concentrating the purified extractive solution of pectin to content of 4.2-5.1% to obtain pectin concentrated solution;
(5) milling: spray drying the pectin concentrated solution at a feeding temperature of 150 deg.C and a discharging temperature of 220 deg.C to obtain pectin powder.
Preparation of the adsorption resin:
(1) putting 22g of chitosan solid into a reaction kettle, and adding 35g of acetic acid solution with the mass fraction of 5% to prepare chitosan acetic acid solution for later use;
(2) adding 10g of epichlorohydrin into absolute ethyl alcohol, heating to a reflux state, keeping the temperature and stirring for 10min, then adding 15g of trimethylolethane and 2g of benzoyl peroxide, and continuing to stir for 1h under reflux; adding the chitosan acetic acid solution obtained in the step 1 and 2g of sodium pyrophosphate, and continuously refluxing and stirring for 1 h;
(3) and (3) cooling the system in the step (2) to 50 ℃, fully mixing, performing microwave treatment for 5min under the microwave frequency of 2450MHz and the power of 700W, standing for 15min, continuing the microwave treatment for 10min, filtering, washing out impurities from the precipitate by deionized water and absolute ethyl alcohol, and drying in a drying box at the temperature of 100 ℃ and 110 ℃ to constant weight to obtain the adsorption resin.
Comparative example 3
(1) Pretreatment of skin slag: soaking 10kg of Chinese gooseberry peel residues in 1.2% sodium carbonate solution for 1h, sterilizing and degreasing the peel residues, then sending the peel residues into a vacuum low-temperature cold air dryer, and drying the peel residues at the temperature of 32 ℃ until the moisture content of the peel residues is 25% -32%;
(2) acid extraction: grinding and crushing the skin residue, adding 60kg of deionized water, adjusting the pH value to 1.5-2.0 by using an acid solution, heating to 90 ℃, preserving the temperature, stirring for 1h, and filtering while the mixture is hot to obtain a skin residue pectin extract; when the extract liquid is cooled to 50 ℃, adding amylase accounting for 1 percent of the weight of the extract liquid, stirring and mixing for 20min, and then heating to 80 ℃ to inactivate the enzyme;
(3) and (3) purification: decoloring the extract liquid after enzyme deactivation in the step 2 by using commercially available D201 resin, and removing impurities;
(4) concentration: heating the purified extractive solution to 55 deg.C, ultrafiltering and concentrating under 0.2Mpa by tubular polyacrylonitrile membrane ultrafilter with cut molecular weight of 50000u, and concentrating the purified extractive solution of pectin to content of 4.2-5.1% to obtain pectin concentrated solution;
(5) milling: spray drying the pectin concentrated solution at a feeding temperature of 150 deg.C and a discharging temperature of 220 deg.C to obtain pectin powder.
Example 3
Based on example 1, comparative example 1 in which no chitosan-acetic acid solution was added, comparative example 2 in which no modifier was added, and comparative example 3 in which decolorization and impurity removal were performed by a commercially available D201 resin were provided.
The pectin extraction was performed on the same batch of kiwi fruit peel and pomace according to examples 1-2 and comparative examples 1-3, and the content of galacturonic acid, the extraction rate of pectin, and the decolorization rate of pigment in the finished pectin were determined, and the results are shown in table 1.
TABLE 1 extraction of pectin from the rind of Kiwi berry according to the invention
| Item of implementation | Content of galacturonic acid/%) | Pectin extraction yield/%) | Decolorization ratio/% |
| Example 1 | 94.2 | 96.8 | 97.6 |
| Example 2 | 94.5 | 97.1 | 97.5 |
| Comparative example 1 | 72.3 | 74.2 | 80.9 |
| Comparative example 2 | 81.4 | 82.5 | 86.4 |
| Comparative example 3 | 79.1 | 80.2 | 83.6 |
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. A process for extracting pectin from kiwi fruit peel residues is characterized by comprising the following steps:
(1) pretreatment of skin slag: soaking the kiwi fruit peel residues in 0.8-1.2% sodium carbonate solution for 1-3h, sterilizing and degreasing the peel residues, then sending the peel residues into a vacuum low-temperature cold air dryer, and drying the peel residues at the temperature of 32-35 ℃ until the moisture content of the peel residues is 25-32%;
(2) acid extraction: grinding and crushing the skin slag, adding deionized water, and mixing the materials according to a material-liquid ratio of 1: 5-10, adjusting the pH value to 1.5-2.0 by using an acidic solution, heating to 90-100 ℃, keeping the temperature, stirring for 1-2h, and filtering while hot to obtain a peel residue pectin extract; cooling the extractive solution to 50 deg.C, adding amylase 1-2% of the extractive solution, stirring and mixing for 20-30min, and heating to 80 deg.C to inactivate enzyme;
(3) and (3) purification: decoloring the extract liquid after enzyme deactivation in the step 2 by using adsorption resin, and removing impurities;
(4) concentration: heating the purified extractive solution to 50-55 deg.C, ultrafiltering with tubular polyacrylonitrile membrane ultrafilter with cut molecular weight of 50000u under pressure of 0.2Mpa, concentrating the purified extractive solution of pectin to content of 4.2-5.1% to obtain pectin concentrated solution;
(5) milling: spray drying the pectin concentrated solution at the feeding temperature of 150-160 ℃ and the discharging temperature of 220-230 ℃ to obtain pectin powder;
the preparation method of the adsorption resin comprises the following steps:
(1) putting the chitosan solid into a reaction kettle, and adding an acetic acid solution with the mass fraction of 5% to prepare a chitosan acetic acid solution for later use;
(2) adding epoxy chloropropane into anhydrous ethanol, heating to reflux state, stirring for 10-20min under heat preservation, adding trimethylolethane and initiator, and continuing to reflux and stir for 1-2 h; adding the chitosan acetic acid solution and the ionic crosslinking agent in the step 1, and continuously refluxing and stirring for 1-2 hours;
(3) adding a modifier into the system obtained in the step 2, cooling to 50-55 ℃, fully mixing, performing microwave treatment for 5-10min at microwave frequency of 2450MHz and power of 700W, standing for 15-30min, continuing the microwave treatment for 5-10min, filtering, washing impurities of the precipitate by deionized water and absolute ethyl alcohol, and drying in a drying box at the temperature of 100 ℃ and 110 ℃ to constant weight to obtain the adsorption resin;
the modifier is a mixture of tea polyphenol, sodium alginate and polyethylene glycol 400, and the mass ratio is 5-10: 5-10: 10-15.
2. The process of extracting pectin from kiwi berry peel residue as claimed in claim 1, wherein: the mass ratio of the chitosan solid to the 5% acetic acid solution is 20-30: 30-50.
3. The process of extracting pectin from kiwi berry peel residue as claimed in claim 1, wherein: the mass ratio of the epichlorohydrin to the trimethylolethane to the initiator to the ionic crosslinking agent to the modifier is 10-15: 15-20: 1-5: 1-5: 1-5.
4. The process of extracting pectin from kiwi berry peel residue as claimed in claim 1, wherein: the initiator is selected from benzoyl peroxide or lauroyl peroxide.
5. The process of extracting pectin from kiwi berry peel residue as claimed in claim 1, wherein: the ionic crosslinking agent is selected from one of sodium pyrophosphate, sodium tripolyphosphate and tetrapolyphosphate.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102551074A (en) * | 2012-01-18 | 2012-07-11 | 南京师范大学 | Method for preparing pectin from Chinese gooseberry pomace |
| CN103641933A (en) * | 2013-11-27 | 2014-03-19 | 威海市桢昊生物技术有限公司 | Method for extraction of pectin from kiwifruit peel pomace |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102551074A (en) * | 2012-01-18 | 2012-07-11 | 南京师范大学 | Method for preparing pectin from Chinese gooseberry pomace |
| CN103641933A (en) * | 2013-11-27 | 2014-03-19 | 威海市桢昊生物技术有限公司 | Method for extraction of pectin from kiwifruit peel pomace |
Non-Patent Citations (1)
| Title |
|---|
| 荆迎军等."三聚磷酸钠和环氧氯丙烷二次交联壳聚糖对Pb(II)的吸附特性".《化工新型材料》.2014,第42卷(第8期), * |
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