CN108912242B - Method for extracting pectin with high gelatinization degree from pomelo peel in plateau mountain - Google Patents
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Abstract
The invention discloses a method for extracting pectin with high gelatinization degree from pomelo peel in plateau mountain, which comprises the steps of cutting the pomelo peel into small pieces, cleaning, sterilizing at high temperature, inactivating enzyme, drying, crushing and sieving to obtain pomelo peel powder for later use; mixing pericarpium Citri Grandis powder with hydrochloric acid water solution, adding EDTA, mixing, and performing microwave intermittent treatment to obtain extractive solution; filtering the hot extract to remove residue, and collecting the filtrate; concentrating the filtrate, adding anhydrous ethanol for precipitation, standing at normal temperature, filtering, collecting the filter residue, and washing the filter residue to obtain crude pectin precipitate; freeze drying the crude pectin precipitate, pre-freezing, and sublimating to obtain pectin product. The method for extracting the pectin with high gelatinization degree from the pomelo peel in the plateau mountain is simple and convenient, has high yield, is easy to operate, is suitable for industrial production, and has the advantages of good quality of the prepared pectin, high gelatinization degree and resource utilization of a large amount of waste pomelo peel.
Description
Technical Field
The invention belongs to biological extraction, and particularly relates to a method for extracting pectin with high gelatinization degree from pomelo peel in plateau mountain.
Background
The Ping mountain pomelo is a evergreen fruit tree in Rutaceae and is cultivated in Guangdong, Fujian and other places in China. In the actual production, a large amount of shaddock peel (accounting for about 30 percent of the mass of the shaddock) is not fully utilized, so that serious resource waste and environmental pollution are caused. Currently, the common pectin extraction raw materials in commerce are apple pomace, citrus peel, beet pulp and the like. The apple pomace and the citrus peel are mainly from the fruit juice processing industry, have short preservation period and are extremely easy to decay, generate a large amount of microorganisms, and then generate a large amount of pectinase to degrade pectin in the apple pomace and the citrus peel, so that the yield of subsequent pectin extraction is greatly reduced, and particularly the yield of high molecular weight pectin is increased. The beet pulp is mainly derived from the by-product of sugar production in beet sugar factory. The sugar beet used in sugar production in beet sugar factories is usually harvested before the biological mature period of the sugar beet, the sugar beet is not mature, and pectin in the immature sugar beet is mainly protopectin and is insoluble in water, thus increasing the extraction difficulty. And the molecular weights of the pectins extracted by the three are small, so that the requirement of high gelation degree is difficult to achieve. The pomelo is a common edible fruit, has long shelf life and is not easy to decay, and the pectin content in the pomelo peel is more than twice of that of apple and citrus pulp, so that the pomelo peel is a good raw material for extracting pectin. The shaddock peel adopted by the invention is derived from mature pomelo in Ping shan. The pomelo peel of the pomelo is thick, is storage and transportation resistant, has a shelf life of three months, is not easy to decay and rot, and most of pectin contained in the pomelo peel is soluble pectin. And the pomelos belong to high-yield and stable-yield early-maturing varieties, have sufficient sources and are not easy to cause the problem of source shortage.
Pectin is a polysaccharide polymer extracted from plant tissues and is generally considered to consist of protopectin, pectate acid, and pectate acid. The basic structure of the D-galactopyranose is a linear long chain linked by a- (1, 4) -glycosidic bond, and the relative molecular weight is 1-40 ten thousand. The pectin is white or light-colored powder, has no odor, strong heat property, is hardly dissolved in organic solvents such as ethanol, etc., the aqueous solution is viscous and weakly acidic, is stable under acidic condition than alkaline condition, and can form flocculent precipitate with various metal ions under certain condition. The conventional pectin extraction methods include conventional acid extraction, ion exchange, microwave, and ammonium oxalate methods.
Pectin is commonly used as a thickener, stabilizer, emulsifier, gelling agent and texturizing agent in the food processing industry and in the chemical industry. In the field of medicine, the medicine is an excellent medicine preparation matrix and has the functions of resisting bacteria, reducing swelling, stopping bleeding, detoxifying, relieving diarrhea, reducing blood pressure, resisting radiation and the like.
The traditional extraction method of pectin is an acid extraction method, but the acid extraction method enables the pectin to be in a high-temperature and high-acidity environment for a long time, so that alpha-1, 4 glycosidic bonds in the pectin are broken, the molecular weight of the pectin is reduced, and the gelation degree is reduced.
The method has simple operation and environmental protection, but the cost of the enzyme is too high, thereby greatly improving the production cost and being not beneficial to the implementation of industrialization.
The basic principle of the metal chelating agent method is that a chelating agent is used to form calcium pectate precipitate with calcium and magnesium ions in protopectin, so that pectin molecules are released and extracted by dissolving in water. The chelating agent method has mild extraction conditions, and the extracted pectin has larger molecular weight, thereby having good gelling property. However, the single chelating agent method consumes too long time, and the addition of too much chelating agent increases ash content in the finished pectin product and is difficult to remove.
The common metal chelating agents in pectin extraction include sodium hexametaphosphate and ammonium oxalate. Sodium hexametaphosphate can form water-soluble precipitate with calcium and magnesium ions in plant tissues to relieve the sealing effect of pectin, but even food-grade sodium hexametaphosphate contains trace heavy metals such as lead and arsenic. Arsenic causes depigmentation, keratosis, canceration and the like of skin, and lead is hidden in human bodies and is easy to cause lead poisoning after long-term eating. The food-grade sodium hexametaphosphate also contains a certain content of fluoride, and low-concentration fluoride can cause chronic poisoning and fluorosis and cause harm to human health. Too low a concentration is difficult to completely remove the blocking effect of pectin, and too high a concentration may cause potential harm to human body. Therefore, the use amount of sodium hexametaphosphate needs to be strictly controlled, and the application of the sodium hexametaphosphate in pectin extraction is limited.
Ammonium oxalate is also a common pectin-extracting metal chelating agent in the literature at present, and ammonium oxalate can form water-insoluble precipitate with calcium and magnesium ions, so that the content of pectin in an extracting solution is reduced. The extraction of ammonium oxalate alone takes a long time and is not efficient. And the ammonium oxalate is toxic and can be easily decomposed into oxalic acid and ammonia gas under heat. The temperature is an important factor when pectin is extracted, pectin extraction is generally carried out at high temperature, and the characteristic that ammonium oxalate is easily decomposed by heat hinders the combination of the method and other methods, so that the practical operability is not strong.
EDTA can be chelated with various divalent metal ions, and is an excellent calcium-magnesium ion chelating agent. EDTA can effectively remove the sealing effect of calcium and magnesium ions on pectin to form water-soluble precipitate, and the precipitate mainly contains calcium and magnesium metal salt which is basically non-toxic to human bodies. The EDTA has stable structure, is easy to dissolve in hot water, can be effectively combined with other extraction methods to extract pectin, reduces the extraction time, improves the pectin yield, ensures that pectin with large molecular weight is not degraded, improves the molecular weight of the pectin through chelation, and further improves the viscosity and the gel strength of the pectin.
The ultrasonic method is a method widely applied to natural product extraction at present. The ultrasonic wave is mainly used for generating strong cavitation effect, mechanical effect and other multi-stage effects to accelerate the release of effective substances in cells. However, as the intensity and time of the ultrasonic wave increase, the side chain of the pectin degrades, and the molecular weight gradually decreases to affect the gelation degree of the pectin, which is not beneficial to the extraction of the pectin with high gelation degree.
The microwave method is a common auxiliary extraction method. Microwave refers to an electromagnetic wave having a wavelength of 1mm to 1m and a frequency of 300MHz to 30000 MHz. On one hand, in the microwave extraction process, high-frequency electromagnetic waves penetrate through an extraction medium to reach the interior of a material, so that the material is crushed and dissolved out. On the other hand, the electromagnetic field generated by the microwave accelerates the diffusion rate of the extracted part to the interface of the extraction solvent, and improves the extraction efficiency. The microwave extraction has the advantages of high speed, high efficiency, uniform heating and the like, and is widely used for extracting natural substances. However, the continuous microwave extraction method is difficult to control the temperature of an extraction system, and the temperature of the system rises at a high speed all the time, so that pectin molecules are always in a high-speed vibration heat-generating state, glycoside bonds are broken, and the pectin is degraded. The intermittent microwave method can well control the temperature of the extraction system within a certain range, timely reduce the temperature of the extraction system, prevent the breakage of glycosidic bonds or branched chains in the pectin and keep the structural integrity of the pectin.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the problems in the prior art, the invention provides a method for extracting pectin with high gelatinization degree from pomelo peel. The method for extracting the pectin with high gelatinization degree from the pomelo peel in the plateau mountain is simple and convenient, has high yield, is easy to operate, is suitable for industrial production, and has the advantages of good quality of the prepared pectin, high gelatinization degree and resource utilization of a large amount of waste pomelo peel.
The technical scheme is as follows: in order to achieve the above object, the method for extracting pectin with high gelatinization degree from pomelo peel as described in the present invention comprises the following steps:
(1) cutting pericarpium Citri Grandis into small pieces, cleaning, sterilizing at high temperature, inactivating enzyme, oven drying, pulverizing, and sieving to obtain pericarpium Citri Grandis powder;
(2) mixing the shaddock peel powder obtained in the step (1) with a hydrochloric acid aqueous solution with the pH value of 2, adding EDTA, fully mixing, and performing intermittent microwave treatment to obtain a pectin extracting solution;
(3) filtering the extracting solution in the step (2) while the extracting solution is hot to remove filter residues, and taking filtrate;
(4) concentrating the filtrate obtained in the step (3), adding absolute ethyl alcohol for precipitation, standing at normal temperature, filtering, taking filter residues, and washing the filter residues to obtain crude pectin precipitate;
(5) freeze drying the crude pectin precipitate, pre-freezing, and sublimating to obtain pectin product.
Preferably, the shaddock peel in the step (1) is a pomelo peel of a lawn mountain shaddock in a mature period, which is produced in Zhangzhou city in Fujian province. Pectin has a complex structure, and the characteristics of pectin are greatly related to sources, varieties and maturity. The pomelo peel has a high pectin content, is a mature pomelo peel of a Ping mountain pomelo, belongs to a high-yield and stable-yield early-maturing variety and is wide in source. The pomelo peel of the lawn mountain pomelo is thick, the storage and transportation are resistant, the quality guarantee period is as long as three months, and the pomelo is not easy to decay and rot. Once rotten and decayed, plants produce a large number of microorganisms, and pectinase produced by the microorganisms degrades pectin in the plants. And other sources such as apples and oranges have short shelf life, are easy to decay to generate a large number of microorganisms, accelerate the degradation of pectin and reduce the content of the pectin.
Wherein the high-temperature sterilization and enzyme deactivation in the step (1) is high-temperature steam sterilization and enzyme deactivation. Usually, the temperature is 121 ℃ for 20min, so as to ensure that the pectinase and the microorganisms which can generate the pectinase in the pomelo peel are killed.
Preferably, the pulverizing and sieving in step (1) is to pass through a 60-mesh sieve and not to pass through a 80-mesh sieve.
Wherein the shaddock peel powder in the step (2) is mixed with a hydrochloric acid aqueous solution according to the material-liquid ratio of 1:25g-1: 30/mL.
Further, the amount of EDTA in the step (2) accounts for 0.24-0.26% of the mass of the shaddock ped powder obtained in the step (1).
And further, the step (2) of intermittent treatment by microwaves is intermittent treatment in a microwave extraction instrument with power of 500- & ltSP & gt and 600- & ltSP & gt W, the microwave time is 15-25s, the intermittent time is the same as the microwave time, and the treatment is repeated for 5 times.
Has the advantages that: compared with the prior art, the invention has the following advantages:
1. the method for extracting pectin from the pomelo peel of the Ping shan pomelo takes the pomelo peel in the mature period as a raw material, has wide raw materials, changes waste into valuable, saves resources and protects the environment at the same time. According to the invention, the pomelo peel powder is crushed and sieved, and the part of particles which can pass through 60 meshes but not pass through 80 meshes is taken, so that the problems that the crushed particle size is too small, the pomelo peel powder is agglomerated and cannot react fully, the crushed particle size is too large and an extracting solution cannot enter pomelo peel tissues easily can be effectively prevented. The addition amount of the EDTA of the invention is 0.24-0.26 percent, which takes the mass of the pumelo peel dry powder as the base number. Too much EDTA will introduce too much impurities into the reaction system, and the pectin is not completely released from the plant tissue when the addition amount is reduced. The extraction of the invention emphasizes that the microwave intermittent extraction is necessary, otherwise, the phenomena of pectin degradation and gel strength reduction exist under the condition of continuous microwave treatment with the same power and the same time. Finally, the preparation method is simple, the yield is high, the operation equipment is simple, the quality of the obtained pectin is good, and the gelation degree is high.
2. The metal chelating agent used in the invention is EDTA, and the dosage of the metal chelating agent is 0.24-0.26%. The invention limits the pectin source to be pumelo peel of the pumelo of the plateau mountain, and the pectin with different sources, varieties and maturity has extremely different properties which are not the same. The dosage of ETDA in the method is repeatedly measured and corrected through a large number of preliminary experiments at the early stage, and the proper addition amount is selected, so that the impurities in the pectin finished product are reduced. The time required by the method is greatly reduced, and the time and energy are saved.
3. The invention uses intermittent microwave, and the time and power of microwave irradiation have great influence on the pectin yield, property, molecular weight and other aspects. The yield of the pomelo peel pectin extracted by the method can reach 38.34%, and the pectin obtained by the method has good gelling degree and thickening property.
Detailed description of the invention
The present invention is further illustrated by the following examples.
Example 1
(1) Cutting pericarpium Citri Grandis into small pieces, washing with flowing clear water, sterilizing and inactivating enzyme at 121 deg.C for 20min with high temperature steam, oven drying pericarpium Citri Grandis, pulverizing, sieving, and collecting 60 mesh and 80 mesh granules.
(2) Mixing the pomelo peel powder obtained in the step (1) with a hydrochloric acid aqueous solution with the pH value of 2 according to the material-liquid ratio of 1: mixing 25g/mL, adding EDTA 0.24% of pericarpium Citri Grandis powder, mixing, and intermittently processing in a microwave extraction instrument with power of 500W for 15s and 15s for 5 times.
(3) And (3) filtering the pectin extracting solution in the step (2) while the pectin extracting solution is hot to remove filter residues, and taking the filtrate.
(4) And (4) concentrating the filtrate obtained in the step (3) until the pectin concentration is about 24mg/mL, adding equal volume of absolute ethyl alcohol for precipitation, standing at normal temperature for 24 hours, filtering, taking filter residue, and washing the filter residue by using an ethanol water solution with the volume fraction of 95% v/v to obtain a crude pectin precipitate.
(5) Freeze drying the crude pectin precipitate, pre-freezing, and sublimating at-53 deg.C to obtain pectin product.
Example 2
(1) Cutting pericarpium Citri Grandis into small pieces, back washing with flowing clear water, and sterilizing and inactivating enzyme at 121 deg.C for 20min with high temperature steam. After sterilization, the shaddock peel is dried, crushed and sieved, and part of the shaddock peel which passes through 60 meshes but does not pass through 80 meshes is taken to obtain powder for later use.
(2) Mixing the pomelo peel powder obtained in the step (1) with a hydrochloric acid aqueous solution with the pH value of 2 according to the material-liquid ratio of 1: mixing at 27g/mL, adding EDTA 0.25% of pericarpium Citri Grandis powder, mixing, and intermittently processing in microwave extractor with power of 550W for 5 times (microwave time 20s and intermittent time 20 s).
(3) And (3) filtering the pectin extracting solution in the step (2) while the pectin extracting solution is hot to remove filter residues, and taking the filtrate.
(4) And (4) concentrating the filtrate obtained in the step (3) until the pectin concentration is about 24mg/mL, adding equal volume of absolute ethyl alcohol for precipitation, standing at normal temperature for 24 hours, filtering, taking filter residue, and washing the filter residue by using an ethanol water solution with the volume fraction of 95% v/v to obtain a crude pectin precipitate.
(5) Freeze drying the crude pectin precipitate, pre-freezing, and sublimating at-53 deg.C to obtain pectin product.
Example 3
(1) Cutting pericarpium Citri Grandis into small pieces, back washing with flowing clear water, and sterilizing and inactivating enzyme at 121 deg.C for 20min with high temperature steam. After sterilization, the shaddock peel is dried, crushed and sieved, and part of the shaddock peel which passes through 60 meshes but does not pass through 80 meshes is taken to obtain powder for later use.
(2) Mixing the pomelo peel powder obtained in the step (1) with a hydrochloric acid aqueous solution with the pH value of 2 according to the material-liquid ratio of 1: mixing at 30g/mL, adding EDTA 0.26% of pericarpium Citri Grandis powder, mixing, and intermittently processing in a microwave extraction instrument with power of 600W for 5 times (microwave time 25s and intermittent time 25 s).
(3) And (3) filtering the pectin extracting solution in the step (2) while the pectin extracting solution is hot to remove filter residues, and taking the filtrate.
(4) And (4) concentrating the filtrate obtained in the step (3) until the pectin concentration is about 24mg/mL, adding equal volume of absolute ethyl alcohol for precipitation, standing at normal temperature for 24 hours, filtering, taking filter residue, and washing the filter residue by using an ethanol water solution with the volume fraction of 95% v/v to obtain a crude pectin precipitate.
(5) Freeze drying the crude pectin precipitate, pre-freezing, and sublimating at-53 deg.C to obtain pectin product.
Test example 1
The influence of the batch microwave combined with the EDTA method on the extraction of the pectin with high gelation degree from the pomelo peel is examined and is shown in Table 1.
Comparative example 1 extraction of pectin from Mi xi GUAN shaddock peel with continuous microwave alone, using the storage Jun "research on extraction Process of pectin from Mi xi GUAN shaddock peel". (continuous microwave method only, without EDTA addition)
Comparative example 2 is the same as the method of example 2 of the present invention except that EDTA is added in step (2) in an amount of 0.2% by mass based on the grapefruit peel powder.
Comparative example 3 is the same as the method of example 2 of the present invention except that EDTA is added in step (2) in an amount of 0.3% by mass based on the grapefruit peel powder.
Comparative example 4 is the same as the method of example 2 of the present invention except that step (2) was continued for a microwave treatment time of 100s in a microwave extractor having a power of 550W.
Comparative example 5 is the same as the method of inventive example 2 except that the microwave treatment in step (2) was not performed but the high temperature extraction was performed at 85 ℃ for 90 min.
Comparative example 6 is the same as the method of inventive example 2 except that EDTA was not added in step (2).
TABLE 1
The pectin yield is (mass of pectin/mass of sample) × 100%.
As can be seen from Table 1, in comparative example 1, "the extraction of pectin from Mian xi GUAN PI" in continuous microwave extraction, the pectin obtained was inferior in quality to that obtained by the extraction methods of examples 1 to.
Comparative examples 2 and 3 compared to the inventive examples, EDTA content between 0.24% and 0.26% is the best choice. The proper EDTA content can increase the extraction amount of pectin and does not increase the ash content in the pectin. The national standard requires that the acid insoluble ash content in the pectin is not more than 1%, excessive EDTA is added to introduce excessive impurities into the reaction system, the reaction system is beyond the national standard, and the pectin yield is not obviously increased or even slightly reduced. If the addition amount is reduced, pectin cannot be completely released from the plant tissue, and the extraction amount of pectin is reduced.
Comparative example 4 compared with the inventive example, even though the same amount of EDTA was added, the time of microwave irradiation had a great influence on the yield, properties, molecular weight, etc. of pectin. The yield of the comparative example 4 is 22.29%, the yield of the pomelo peel pectin extracted by the method can reach 38.34%, the yield is 1.7 times of the pomelo peel pectin, and the gel strength is 1.41 times of the pomelo peel pectin. The extraction of the invention emphasizes that the extraction must be microwave intermittent extraction, and the phenomena of pectin degradation and gel strength reduction can exist under the condition of continuous microwave treatment with the same power and the same time.
Comparative example 5 and comparative example 6 compared with the examples of the present invention, the extraction rate of pectin was greatly reduced and the molecular weight was also small, and the degree of gelation was much lower than that of the pectin of the present invention.
In conclusion, the pectin obtained by the method has better gelling degree and thickening property than the pectin obtained by the comparative example, and the method can more effectively obtain the pectin with high yield and high gelling degree.
Claims (5)
1. A method for extracting pectin with high gelatinization degree from pomelo peel in plateau mountain is characterized by comprising the following steps:
(1) cutting pericarpium Citri Grandis into small pieces, cleaning, sterilizing at high temperature, inactivating enzyme, oven drying, pulverizing, and sieving to obtain pericarpium Citri Grandis powder;
(2) mixing the shaddock peel powder obtained in the step (1) with a hydrochloric acid aqueous solution with the pH =2, adding EDTA, fully mixing, and performing microwave intermittent treatment on pectin to obtain an extracting solution;
(3) filtering the pectin extracting solution in the step (2) while the pectin extracting solution is hot to remove filter residues, and taking a filtrate;
(4) concentrating the filtrate obtained in the step (3), adding absolute ethyl alcohol for precipitation, standing at normal temperature, filtering, taking filter residues, and washing the filter residues to obtain crude pectin precipitate;
(5) freeze drying the crude pectin precipitate, pre-freezing, and sublimating to obtain pectin product;
the EDTA in the step (2) accounts for 0.24-0.26% of the mass of the shaddock peel powder obtained in the step (1); and (3) the intermittent treatment of the microwave in the step (2) is intermittent treatment in a microwave extraction instrument with power of 500-600W, the microwave time is 15-25s, the intermittent time is the same as the microwave time, and the treatment is repeated.
2. The method for extracting pectin with high gelation degree from the pomelo peel as claimed in claim 1, wherein the pomelo peel of the step (1) is mature pomelo peel.
3. The method for extracting pectin with high gelatinization degree from pomelo peel as claimed in claim 1, wherein said high temperature sterilization and enzyme deactivation of step (1) is high temperature steam sterilization and enzyme deactivation.
4. The method for extracting pectin with high gelation degree from pomelo peel as claimed in claim 1, wherein said pulverizing and sieving of step (1) is to pass 60 mesh sieve and not to pass 80 mesh sieve.
5. The method for extracting pectin with high gelatinization degree from pomelo peel in claim 1, wherein in step (2), the pomelo peel powder is mixed with hydrochloric acid aqueous solution according to the feed-to-solution ratio of 1:25-1:30 g/mL.
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| CN110140854A (en) * | 2019-06-14 | 2019-08-20 | 仲恺农业工程学院 | A kind of compound nectar and preparation method thereof |
| CN113621090B (en) * | 2021-07-08 | 2023-05-23 | 浙江工业大学 | Multi-stage pectin decoloring method |
| CN113679032A (en) * | 2021-08-27 | 2021-11-23 | 烟台帝斯曼安德利果胶股份有限公司 | Pretreatment method of apple wet slag for extracting pectin and pectin extraction method |
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| CN102702379A (en) * | 2012-04-26 | 2012-10-03 | 赛珂睿德生物医药科技(上海)有限公司 | Extraction and preparation process of citrus pectin |
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Application publication date: 20181130 Assignee: Jiangsu Mingjia Construction Engineering Co.,Ltd. Assignor: HUAIYIN INSTITUTE OF TECHNOLOGY Contract record no.: X2021980010817 Denomination of invention: A method for extracting high gelation pectin from Pingshan pomelo peel Granted publication date: 20210727 License type: Common License Record date: 20211018 |