CN111171178A - Method for extracting pectin from pericarp - Google Patents
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- CN111171178A CN111171178A CN201811334647.2A CN201811334647A CN111171178A CN 111171178 A CN111171178 A CN 111171178A CN 201811334647 A CN201811334647 A CN 201811334647A CN 111171178 A CN111171178 A CN 111171178A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- 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
- C08B37/0048—Processes of extraction from organic materials
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Abstract
The invention discloses a method for extracting pectin from pericarp, belonging to the technical field of pectin extraction, and the extraction method comprises the following steps: pretreating fruit peels; adding dry ice into the peel, stirring and mixing, placing the mixture in a liquid nitrogen system, placing the mixture of the dry ice and the peel at 20-40 ℃ for standing, and leaving the peel after the dry ice sublimes; adding an acidic solution into the peel, adjusting the pH to 1.5-2.0, heating to 90-100 ℃, preserving the heat for 1-2 h, and filtering while the pectin is hot to obtain a pectin extract; when the temperature is cooled to 50 ℃, adding amylase, stirring and mixing for 20-30 min, and then heating to 80 ℃ to inactivate enzyme; adding a decolorizing agent, preserving the heat for 20-30 min, and filtering to obtain decolorized filtrate; concentrating the decolorized filtrate; (5) spray drying to obtain pectin powder; the method adopts the modes of low-temperature freezing and dry ice sublimation to break the cell walls of the peels, so that the pectin is conveniently extracted, the extraction efficiency of the pectin is improved, and the content of impurities in the pectin extraction liquid is effectively reduced.
Description
Technical Field
The invention belongs to the technical field of pectin extraction, and particularly relates to a method for extracting pectin from pericarp.
Background
Natural pectins, which are widely present in the form of protopectin, pectin, and pectic acid in fruits, roots, stems, and leaves of plants, are a constituent of cell walls, and they are present along with cellulose to constitute an intermediate layer binder of adjacent cells, so that plant tissue cells are merely bound together. Protopectin is a water-insoluble substance, but can be hydrolyzed and converted into water-soluble pectin under the action of chemical reagents such as acid, alkali and salt and enzyme, and pectin is a linear polysaccharide polymer in nature.
Common fruits such as citrus, lemon, grapefruit, etc. contain about 30% pectin, which is the most abundant source of pectin, and vegetables and fruits with good water retention, such as apples, persimmons, pears, bananas, strawberries, dried beans, cauliflower, radishes, pumpkins, and potatoes, generally have relatively high pectin content.
The pectin extracting process in available technology includes material pre-treatment, extraction, decolorizing, concentration and drying to obtain the product. The pectin yield or the gel degree is reduced because the raw materials are easy to generate pectinase hydrolysis, fresh fruit peels are required to be timely treated, the activity of pectinase is generally passivated at high temperature, the enzyme-inactivated raw materials are squeezed to remove juice, and then are extracted by using an acidic solution, in the extraction process, pectin can be extracted through long-time leaching, the production efficiency is greatly influenced, calcium and magnesium ions in the fruit peels are high in content, the ions can have a sealing effect on the pectin and influence the conversion of the pectin into water-soluble substances, and the gel degree is influenced because the impurity content in the fruit peels is high, so that the extraction efficiency is poor, the extraction rate is low, and the extraction quality is poor due to the adoption of an acid method. In order to solve the problem, the food college of southwest agriculture university adopts cation exchange resin or sodium hexametaphosphate to improve the acid extraction, thereby improving the yield and the gelatinization degree of the pectin.
Disclosure of Invention
Aiming at the problems, the invention aims to overcome the defects in the prior art and provide a method for extracting pectin from peel, so that the extraction efficiency of the pectin is improved, and the impurity content in the pectin is reduced.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for extracting pectin from pericarp comprises the following steps:
(1) pretreating fruit peels; cleaning and crushing the peel until the length is not more than 1cm, adding water until the peel is immersed, soaking, and then drying the peel by drying;
(2) adding dry ice in an amount which is 0.5-1 time of the weight of the dried peel into the dried peel, stirring and mixing, then placing the mixture into a liquid nitrogen system, stirring the mixture of the dry ice and the peel for 30-40 min, then standing for 5-10 min, and stirring for 30-40 min; then placing the mixture of the dry ice and the peel in an environment with the temperature of 20-40 ℃ for standing for 30-60 min, and after the dry ice is sublimated, leaving the peel;
(3) adding an acidic solution into the peel, adjusting the pH to 1.5-2.0, heating to 90-100 ℃, preserving the temperature, stirring for 1-2 h, and filtering while the pectin is hot to obtain a pectin extract; cooling to 50 ℃, adding amylase accounting for 1-2% of the weight of the pectin extract, stirring and mixing for 20-30 min, and then heating to 80 ℃ to inactivate enzyme; then adding a decolorizing agent, keeping the temperature, stirring for 20-30 min, and filtering to obtain decolorized filtrate;
(4) concentrating the decolorized filtrate to obtain pectin concentrated solution;
(5) spray drying the pectin concentrated solution to obtain pectin powder.
According to the method, the fruit peel is cleaned, then the fruit peel is soaked in water until the space between cell tissues of the fruit peel is filled with liquid, then the fruit peel is mixed with dry ice, the temperature is reduced, the water among the fruit peel cells is frozen, the volume is increased, the cell walls are punctured, the cell walls of the fruit peel become brittle under the low-temperature condition, the dry ice sublimes along with the temperature rise of a system, the cell walls of the fruit peel are cracked, and the pectin existing among the cells is fully overflowed.
Preferably, in the step (1), a sodium carbonate solution with the weight of 0.3-0.8% of that of the peel is added when the peel is soaked in water, the temperature is raised to 40 ℃, and the stirring is carried out for 20-30 min, so that the sodium carbonate can activate endogenous pe enzyme of the peel to carry out degreasing.
After cell walls of the pericarp are damaged, adding an acidic solution for extracting the gel, wherein the type of the acidic solution is not specially required, and the pH can be adjusted and kept at 1.5-2.0, specifically, the acidic solution can be one selected from hydrochloric acid, sulfuric acid and nitric acid; after extracting to obtain pectin extract, reducing the system temperature, adding amylase, hydrolyzing starch contained in the pectin extract, then raising the temperature again to inactivate the amylase, and then carrying out decoloration treatment on the pectin extract, wherein the decoloration process is to remove the variegated colors in the pectin extract.
Preferably, the decolorizing agent is prepared from 4A molecular sieve raw powder, polyaspartic acid, N-hydroxymethyl acrylamide and magnesium dimethacrylate, and the preparation method comprises the following steps: preparing a polyaspartic acid saturated solution by using deionized water at the temperature of 20-25 ℃, adjusting the pH value to be 4.0-4.5 by using an acid solution, adding 4A molecular sieve raw powder, heating and refluxing for 15-30 min, then adding N-hydroxymethyl acrylamide and magnesium dimethacrylate, continuously refluxing and stirring for 0.5-3 h, standing the mixture, naturally cooling to room temperature, filtering, drying filter residues at the temperature of 60-70 ℃ to constant weight, preparing the obtained solid into micropowder by using a superfine pulverizer, and finally preparing into particles of 35-60 meshes by using a granulator to obtain the decolorizing agent.
The generated macromolecular compound is attached to the surface gaps of the 4A molecular sieve raw powder by the esterification reaction of polyaspartic acid and N-hydroxymethyl acrylamide and the polymerization reaction of N-hydroxymethyl acrylamide and magnesium dimethacrylate, so that the decoloration effect of the 4A molecular sieve raw powder is enhanced.
Preferably, the weight ratio of the polyaspartic acid, the 4A molecular sieve raw powder, the N-hydroxymethyl acrylamide and the magnesium dimethacrylate is (10-15): (25-40): (1-5): (5-10).
And (4) after the decolorization treatment, concentrating the decolorized filtrate of the pectin in order to improve the efficiency of subsequent treatment, wherein in the step (4), the temperature of the concentrated solution is increased to 40-50 ℃, and an ultrafilter is adopted for ultrafiltration concentration under the pressure of 0.2 Mpa. Specifically, for example, a tubular polyacrylonitrile membrane ultrafilter with a cut molecular weight of 50000u is used for ultrafiltration concentration at 45 deg.C and 0.2Mpa, and the decolorized filtrate of pectin is concentrated to 4.2%.
After the concentration treatment, carrying out spray drying on the pectin concentrated solution to obtain pectin powder, wherein in the step (5), the spray drying method specifically comprises the following steps: and drying the pectin concentrated solution at the feeding temperature of 150-160 ℃ and the discharging temperature of 220-230 ℃ to obtain pectin powder.
In the invention, the pericarp is preferably pericarp of citrus, lemon and grapefruit, and the pericarp has high pectin content and good extraction effect.
Compared with the prior art, the invention has the following technical effects:
the traditional crushing and squeezing extraction mode is abandoned, the cell walls of the peel are broken by adopting the modes of low-temperature freezing and dry ice sublimation, and the pectin is convenient to extract, so that the extraction efficiency of the pectin is improved, and the content of impurities in the pectin extraction liquid is effectively reduced;
the improved decoloring agent is adopted to remove the color in the pectin extraction liquid, and the generated high molecular compound is attached to the surface gaps of the raw powder of the 4A molecular sieve through the esterification reaction of polyaspartic acid and N-hydroxymethyl acrylamide and the polymerization reaction of N-hydroxymethyl acrylamide and magnesium dimethacrylate, so that the pectin extraction liquid can be effectively decolored, and small molecular impurities in the pectin extraction liquid can be adsorbed, the impurity content in the pectin extraction liquid is reduced, and the purity of the pectin is improved.
Detailed Description
The present invention is further explained below with reference to specific examples.
Example 1 extraction of pectin from grapefruit peel
(1) Pretreating shaddock peel; cleaning and crushing the shaddock peel to a length of not more than 1cm, adding water until the shaddock peel is immersed, adding a sodium carbonate solution with the weight of 0.5% of that of the shaddock peel, heating to 40 ℃, stirring for 20min, and then spin-drying the shaddock peel;
(2) adding dry ice 0.8 times the weight of the dried shaddock peel into the dried shaddock peel, stirring and mixing, then placing the mixture into a liquid nitrogen system, stirring the mixture of the dry ice and the shaddock peel for 30min, then standing for 8min, and stirring for 30 min; then placing the mixture of the dry ice and the shaddock peel in an environment with the temperature of 30 ℃ for standing for 40min, and leaving the shaddock peel after the dry ice is sublimated;
(3) adding a hydrochloric acid solution into the shaddock peel, adjusting the pH to 2.0, heating to 90 ℃, keeping the temperature, stirring for 2 hours, and filtering while the pectin is hot to obtain a pectin extract; cooling to 50 deg.C, adding amylase 2% of pectin extract, stirring and mixing for 20min, and heating to 80 deg.C to inactivate enzyme; then adding a decolorizing agent, preserving heat, stirring for 20min, and filtering to obtain decolorized filtrate;
(4) ultrafiltering with tubular polyacrylonitrile membrane ultrafilter with cut molecular weight of 50000u at 45 deg.C and pressure of 0.2Mpa, and concentrating to obtain pectin concentrate;
(5) 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.
The decolorizing agent is prepared from 4A molecular sieve raw powder (purchased from Gallery, Peng color, Fine chemical Co., Ltd.), polyaspartic acid, N-hydroxymethyl acrylamide and magnesium dimethacrylate, wherein the weight ratio of the polyaspartic acid to the 4A molecular sieve raw powder to the N-hydroxymethyl acrylamide to the magnesium dimethacrylate is 12: 30: 2: 7.
the preparation method comprises the following steps: preparing a polyaspartic acid saturated solution by using deionized water at 20 ℃, adjusting the pH value to be 4.0 by using a hydrochloric acid solution, adding 4A molecular sieve raw powder, heating and refluxing for 20min, then adding N-hydroxymethyl acrylamide and magnesium dimethacrylate, continuously refluxing and stirring for 2h, standing the mixture, naturally cooling to room temperature, filtering, drying filter residues at 65 ℃ to constant weight, preparing the obtained solid into micropowder by using a micronizer, and finally preparing the micropowder into 50-mesh particles by using a granulator to obtain the decolorizing agent.
The pectin extraction rate refers to the ratio of the actual yield of pectin to the amount of pectin contained in the peel (shaddock peel), and in this example, the pectin extraction rate is 93.8%.
Example 2 extraction of pectin from grapefruit peel
(1) Pretreating shaddock peel; cleaning and crushing the shaddock peel to a length of not more than 1cm, adding water until the shaddock peel is immersed, adding a sodium carbonate solution with the weight of 0.3% of that of the shaddock peel, heating to 40 ℃, stirring for 30min, and then spin-drying the shaddock peel;
(2) adding dry ice 0.5 times the weight of the dried shaddock peel into the dried shaddock peel, stirring and mixing, then placing the mixture into a liquid nitrogen system, stirring the mixture of the dry ice and the shaddock peel for 40min, then standing for 5min, and stirring for 30 min; then placing the mixture of the dry ice and the shaddock peel in an environment with the temperature of 20 ℃ for standing for 60min, and leaving the shaddock peel after the dry ice is sublimated;
(3) adding a hydrochloric acid solution into the shaddock peel, adjusting the pH to 1.5, heating to 90 ℃, keeping the temperature, stirring for 1h, and filtering while the pectin is hot to obtain a pectin extract; cooling to 50 deg.C, adding amylase 1 wt% of pectin extract, stirring and mixing for 20min, and heating to 80 deg.C to inactivate enzyme; then adding a decolorizing agent, preserving heat, stirring for 20min, and filtering to obtain decolorized filtrate;
(4) ultrafiltering with tubular polyacrylonitrile membrane ultrafilter with cut molecular weight of 50000u at 45 deg.C and pressure of 0.2Mpa, and concentrating to obtain pectin concentrate;
(5) 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.
The decolorizing agent is prepared from 4A molecular sieve raw powder (purchased from Gallery, Peng color, Fine chemical Co., Ltd.), polyaspartic acid, N-hydroxymethyl acrylamide and magnesium dimethacrylate, wherein the weight ratio of the polyaspartic acid to the 4A molecular sieve raw powder to the N-hydroxymethyl acrylamide to the magnesium dimethacrylate is 10: 25: 1: 5.
the preparation method comprises the following steps: preparing a polyaspartic acid saturated solution by using deionized water at 20 ℃, adjusting the pH value to be 4.0 by using a hydrochloric acid solution, adding 4A molecular sieve raw powder, heating and refluxing for 15min, then adding N-hydroxymethyl acrylamide and magnesium dimethacrylate, continuously refluxing and stirring for 0.5h, standing the mixture, naturally cooling to room temperature, filtering, drying filter residues at 60 ℃ to constant weight, preparing the obtained solid into micro powder by using a superfine pulverizer, and finally preparing the micro powder into 35-mesh particles by using a granulator to obtain the decolorizing agent.
The pectin extraction rate of this example was 93.3%.
Example 3 extraction of pectin from grapefruit peel
(1) Pretreating shaddock peel; cleaning and crushing the shaddock peel to a length of not more than 1cm, adding water until the shaddock peel is immersed, adding a sodium carbonate solution with the weight of 0.8% of that of the shaddock peel, heating to 40 ℃, stirring for 30min, and then spin-drying the shaddock peel;
(2) adding dry ice in an amount which is 1 time of the weight of the shaddock peel into the dried shaddock peel, stirring and mixing, then placing the mixture into a liquid nitrogen system, stirring the mixture of the dry ice and the shaddock peel for 40min, then standing for 10min, and stirring for 40 min; then placing the mixture of the dry ice and the shaddock peel in an environment with the temperature of 40 ℃ for standing for 60min, and leaving the shaddock peel after the dry ice is sublimated;
(3) adding hydrochloric acid solution into pericarpium Citri Grandis, adjusting pH to 2.0, heating to 100 deg.C, maintaining temperature and stirring for 2 hr, and filtering to obtain pectin extractive solution; cooling to 50 deg.C, adding amylase 2% of pectin extract, stirring and mixing for 30min, and heating to 80 deg.C to inactivate enzyme; then adding a decolorizing agent, preserving heat, stirring for 30min, and filtering to obtain decolorized filtrate;
(4) ultrafiltering with tubular polyacrylonitrile membrane ultrafilter with cut molecular weight of 50000u at 45 deg.C and pressure of 0.2Mpa, and concentrating to obtain pectin concentrate;
(5) spray drying the pectin concentrated solution at 160 deg.C and 230 deg.C to obtain pectin powder.
The decolorizing agent is prepared from 4A molecular sieve raw powder (purchased from Gallery, Peng color, Fine chemical Co., Ltd.), polyaspartic acid, N-hydroxymethyl acrylamide and magnesium dimethacrylate, wherein the weight ratio of the polyaspartic acid to the 4A molecular sieve raw powder to the N-hydroxymethyl acrylamide to the magnesium dimethacrylate is 3: 8: 1: 2.
the preparation method comprises the following steps: preparing a polyaspartic acid saturated solution by using deionized water at 25 ℃, adjusting the pH value to be 4.5 by using a hydrochloric acid solution, adding 4A molecular sieve raw powder, heating and refluxing for 30min, then adding N-hydroxymethyl acrylamide and magnesium dimethacrylate, continuously refluxing and stirring for 3h, standing the mixture, naturally cooling to room temperature, filtering, drying filter residues at 70 ℃ to constant weight, preparing the obtained solid into micropowder by using a micronizer, and finally preparing the micropowder into 60-mesh particles by using a granulator to obtain the decolorizing agent.
The pectin extraction rate in this example was 94.1%.
The above embodiments are only for the purpose of promoting an understanding of the core concepts of the invention, and any obvious modifications, equivalents or other improvements made without departing from the spirit of the invention are intended to be included within the scope of the invention.
Claims (4)
1. A method for extracting pectin from pericarp is characterized in that: the method comprises the following steps:
(1) pretreating fruit peels; cleaning pericarp, crushing to length no more than 1cm, adding water until the pericarp is immersed, soaking, and spin-drying;
(2) adding dry ice in an amount which is 0.5-1 time of the weight of the dried peel into the dried peel, stirring and mixing, then placing the mixture into a liquid nitrogen system, stirring the mixture of the dry ice and the peel for 30-40 min, then standing for 5-10 min, and stirring for 30-40 min; then placing the mixture of the dry ice and the peel in an environment with the temperature of 20-40 ℃ for standing for 30-60 min, and after the dry ice is sublimated, leaving the peel;
(3) adding an acidic solution into the peel, adjusting the pH to 1.5-2.0, heating to 90-100 ℃, preserving the temperature, stirring for 1-2 h, and filtering while the pectin is hot to obtain a pectin extract; cooling to 50 ℃, adding amylase accounting for 1-2% of the weight of the pectin extract, stirring and mixing for 20-30 min, and then heating to 80 ℃ to inactivate enzyme; then adding a decolorizing agent, keeping the temperature, stirring for 20-30 min, and filtering to obtain decolorized filtrate;
(4) concentrating the decolorized filtrate to obtain pectin concentrated solution;
(5) spray drying the pectin concentrated solution to obtain pectin powder.
2. The method of extracting pectin from pericarp as claimed in claim 1, wherein: in the step (1), a sodium carbonate solution with the weight of 0.3-0.8% of that of the peel is added when the peel is soaked in water, the temperature is raised to 40 ℃, and the stirring is carried out for 20-30 min.
3. The method of extracting pectin from pericarp as claimed in claim 1, wherein: in the step (4), the concentration method of the decolorized filtrate specifically comprises the following steps: heating the concentrated solution to 40-50 ℃, and carrying out ultrafiltration concentration by using an ultrafilter under the pressure of 0.2 Mpa.
4. The method of extracting pectin from pericarp as claimed in claim 1, wherein: in the step (5), the specific method of spray drying is as follows: and drying the pectin concentrated solution at the feeding temperature of 150-160 ℃ and the discharging temperature of 220-230 ℃ to obtain pectin powder.
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| CN201811334647.2A CN111171178A (en) | 2018-11-10 | 2018-11-10 | Method for extracting pectin from pericarp |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113307895A (en) * | 2021-04-20 | 2021-08-27 | 廖晶 | Adopt pectin semi-manufactured goods making devices of dry ice method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113307895A (en) * | 2021-04-20 | 2021-08-27 | 廖晶 | Adopt pectin semi-manufactured goods making devices of dry ice method |
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Application publication date: 20200519 |