CN109336997B - Method for extracting inulin from jerusalem artichoke at low temperature - Google Patents
Method for extracting inulin from jerusalem artichoke at low temperature Download PDFInfo
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- CN109336997B CN109336997B CN201811144283.1A CN201811144283A CN109336997B CN 109336997 B CN109336997 B CN 109336997B CN 201811144283 A CN201811144283 A CN 201811144283A CN 109336997 B CN109336997 B CN 109336997B
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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
- C08B37/0051—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Fructofuranans, e.g. beta-2,6-D-fructofuranan, i.e. levan; Derivatives thereof
- C08B37/0054—Inulin, i.e. beta-2,1-D-fructofuranan; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- 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
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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Abstract
The invention discloses a method for extracting inulin from jerusalem artichoke at low temperature, which belongs to the technical field of separation and extraction of natural plant components. The method has the advantages of high inulin extraction rate, simple operation, high production efficiency, low cost, low energy consumption and the like, and has higher comprehensive economic benefit.
Description
Technical Field
The invention relates to the technical field of separation and extraction of natural plant components, in particular to a method for extracting inulin from jerusalem artichoke.
Background
Jerusalem artichoke is commonly known as jerusalem artichoke and rhizoma Dysosmae Versipellis, and belongs to perennial Helianthus of Compositae. Inulin (also called inulin) in jerusalem artichoke accounts for 80% of the dry weight, and is a linear polysaccharide formed by connecting D-fructofuranose through beta- (2, 1) glycosidic bonds, the tail end of the linear polysaccharide is connected with a molecule of glucose through alpha- (2, 1) glycosidic bonds, the polymerization degree is generally 2-60 and is averagely 10. Inulin is a naturally occurring water-soluble dietary fiber in the nature, has physiological functions of reducing blood fat, improving the intestinal environment, promoting the proliferation of probiotics, preventing and treating constipation, preventing colon cancer, promoting the absorption of mineral substances, preventing obesity and the like, and is widely applied to dairy products, beverages and foods. Inulin as a purely natural functional ingredient has been approved as a nutritional supplement by more than 20 countries in the world, in 2009 the Ministry of health in China approved inulin as a new resource food, and in 2012 the Ministry of health promulgated and increased jerusalem artichoke as a raw material for producing inulin as a new resource food.
The method for extracting inulin from Jerusalem artichoke mainly comprises conventional hot water extraction method, countercurrent extraction method, etc. The hot water extraction method mainly adopts hot water with the temperature of more than 80 ℃ for repeated extraction, and has the problems of high solid-liquid ratio, large energy consumption, complex operation and the like; the countercurrent extraction technology is an improvement of the traditional hot water extraction method, and adopts hot water extraction at the temperature of more than 80 ℃ as well, but the solid-liquid ratio is lower, and although the countercurrent extraction technology reduces part of energy consumption, the extraction equipment is complex, the manufacturing cost is high, and the production efficiency is not high. In recent years, new extraction technologies such as ultrasonic extraction technology and microwave extraction technology which are widely applied to extracting plant polysaccharide have the characteristics of short time, high efficiency, high yield and the like, but also have the problems of complex extraction equipment, high manufacturing cost, high production cost and difficulty in realizing large-scale industrial production. In addition, in the existing inulin extraction method, the extract liquid is darker in color due to the frequent browning of the jerusalem artichoke, the burden of subsequent decoloring treatment is increased, and the sensory quality of the final product inulin is even affected.
Therefore, the development of a method for extracting inulin from jerusalem artichoke with high product quality, high extraction efficiency and low energy consumption is a technical problem which needs to be solved by technical personnel in the field urgently.
Disclosure of Invention
Through years of research and development practices, the applicant finds that the quality of inulin can be greatly improved by controlling the granularity of the pulverized jerusalem artichoke, adding low-temperature deionized water while pulverizing the jerusalem artichoke, adjusting the pH value of an extracting solution to be proper, passing through steps such as a ceramic membrane and the like, and the method has the advantages of high extraction efficiency, low energy consumption, large-scale continuous industrial production and the like.
Based on the above findings, the present invention has been completed by the applicant. Specifically, the invention provides a method for extracting inulin from jerusalem artichoke at low temperature, which comprises the following steps:
1) cleaning jerusalem artichoke to remove impurities, and pretreating the cleaned jerusalem artichoke by using a solvent;
2) pulverizing pretreated Jerusalem artichoke, adding low-temperature deionized water to obtain Jerusalem artichoke pulp, and separating to obtain Jerusalem artichoke extractive solution and Jerusalem artichoke residue; and adding the low-temperature deionized water while crushing.
3) Mixing extractive solutions, adjusting pH, and passing through ceramic membrane to obtain Jerusalem artichoke extractive solution;
4) desalting the Jerusalem artichoke extract clear solution, decolorizing with resin, concentrating, and drying to obtain inulin.
The invention is further improved in that the solvent in the step 1) is one or more of peracetic acid, chlorine dioxide, ethanol and hydrogen peroxide.
The invention has the further improvement that the grain diameter of the crushed jerusalem artichoke in the step 2) is 10-300 meshes, the jerusalem artichoke residues can be further extracted repeatedly for 1-3 times by using a centrifugal screen, the temperature of deionized water is 5-35 ℃, and the adding amount of the deionized water is 1-3 times of the weight of the jerusalem artichoke.
The invention is further improved in that the pH value of the extracting solution is adjusted to be 1-7 in the step 3), and the aperture of the ceramic membrane is 5-200 nm.
The invention is further improved in that the type of the strongly acidic ion exchange resin used for desalting in the step 4) is any one of D001, AM007 and LD 206; the strong basic anion exchange resin used for decolorization is any one of D900, D941 and D296, a nanofiltration membrane is used for concentration, and spray drying is adopted for drying.
The invention adopts a low-temperature pulping extraction process, the particle size of the crushed jerusalem artichoke is controlled by pretreating the jerusalem artichoke, low-temperature deionized water is added while the jerusalem artichoke is crushed, the extracting solution is adjusted to a proper pH value, and the like, so that the following beneficial effects are achieved:
1) the extraction temperature is low;
2) the extraction time is short;
3) the color of the extracting solution is lighter, so that the pressure of subsequent decoloring treatment is reduced;
4) little microorganism breeding of the extracting solution in the process, and the loss of inulin is reduced;
5) the inulin in the jerusalem artichoke is dissolved out quickly, and the extraction rate is up to more than 98 percent;
6) compared with a hot water extraction method, the method saves the extraction process, shortens the production time, and reduces the energy consumption and the water consumption;
7) the final product has high purity, pure color and pure white color;
8) is suitable for large-scale continuous industrial production.
Detailed Description
The following specific examples and comparative examples are provided to enable those skilled in the art to better understand the technical solutions of the present invention.
The raw materials and auxiliary materials used in the specific embodiment of the invention are all purchased from the market.
Example 1
Cleaning 70kg of fresh jerusalem artichoke to remove surface silt, then pretreating the cleaned jerusalem artichoke by peroxyacetic acid solution, conveying the pretreated jerusalem artichoke to a crusher by a feeding device, adding 140kg of deionized water with the temperature of 25 ℃ while crushing, and crushing the jerusalem artichoke to obtain jerusalem artichoke pulp with the particle size of 50 meshes. Conveying the jerusalem artichoke slurry to a centrifugal sieve for separation to obtain jerusalem artichoke extracting solution and jerusalem artichoke residues, adding deionized water with the temperature of 25 ℃ into the jerusalem artichoke residues, repeatedly extracting the jerusalem artichoke residues for 1 time by using the centrifugal sieve, combining the obtained extracting solutions, adjusting the pH value of the extracting solution to be 4.0, passing the extracting solution with the adjusted pH value through a 50nm ceramic membrane to obtain jerusalem artichoke extracting clear solution, decoloring and desalting the obtained extracting clear solution by using strong acid ion exchange resin D001 and strong base anion exchange resin D296, concentrating by using a nanofiltration membrane, and performing spray drying to obtain inulin.
Examples 2 to 5/comparative examples 1 to 3
The extraction procedures of examples 2-5 and comparative examples 1-3 are substantially the same as example 1, except that the values of the specific process parameters are different, as detailed in the following table.
Comparative example 4
Extracting Jerusalem artichoke from Jerusalem artichoke by conventional hot water extraction method, cleaning 70kg fresh Jerusalem artichoke to remove silt on the surface, shredding cleaned Jerusalem artichoke, adding 350kg deionized water, extracting at 80 deg.C for 4 hr, separating to obtain Jerusalem artichoke residue and extractive solution, repeatedly extracting Jerusalem artichoke residue once, mixing extractive solutions, adding Ca (OH) into the extractive solution2Adjusting pH of the extractive solution to 10.0, flocculating at 80 deg.C for 1 hr, cooling to room temperature, adjusting pH to 8.0 with phosphoric acid solution, and introducing CO2Allowing the pH value of the extractive solution to be 7.0, standing for 30min, filtering with plate and frame, removing flocculation precipitate to obtain Jerusalem artichoke extractive clear solution, desalting and decolorizing with strong acid ion exchange resin D001 and strong base anion exchange resin D296, concentrating with nanofiltration membrane, and spray drying to obtain inulin.
Comparative example 5
Referring to the production process described in patent document CN104987434A, inulin is extracted from Jerusalem artichoke, 70kg of fresh Jerusalem artichoke is washed with mud and peeled, and then crushed in a crusher, and NaHSO with a concentration of 1 ‰ is added while crushing3And (3) feeding the solution and the crushed slurry into a stirring tank, adding 210kg of deionized water at the temperature of 30 ℃, and stirring for 30 min. Squeezing the stirred slurry with a belt press to obtain Jerusalem artichoke extract and Jerusalem artichoke residue, wherein the tension pressure of the filter belt of the belt press is 0.8Mpa, and the Jerusalem artichoke residue is repeatedly extracted once at 30 deg.C of deionized water with the amount of 2 times of the Jerusalem artichoke residue. Mixing the two extractive solutions, heating to 80 deg.C, adding food grade Ca (OH)2Adjusting pH of the extractive solution to 10.0, stirring for 30min, introducing CO2And (3) regulating the pH value of the extracting solution to 7.0 by using gas, cooling the temperature of the extracting solution to be below 40 ℃, filtering by using a plate frame, finely filtering by using a centrifugal machine, concentrating the filtrate by using a 300 dalton nanofiltration membrane until the inulin concentration is 20%, desalting the concentrated solution by using strong-base anion exchange resin D296, strong-acid ion exchange resin D001 and weak-base anion exchange resin D301, entering a double-effect concentrator, concentrating until the inulin concentration is about 50%, and spray-drying to obtain the inulin.
Taking the inulin prepared in the examples 1-5 and the comparative examples 1-5, calculating the extraction yield of the inulin, determining the purity of the product, wherein the inulin content in the product is the total sugar content minus the reducing sugar content, the total sugar content is determined by adopting a phenol sulfate colorimetric method, the reducing sugar content is determined by adopting a DNS colorimetric method, and the results are shown in the following table:
| inulin extraction yield | Inulin purity | |
| Example 1 | 98.6％ | 95％ |
| Example 2 | 98.2％ | 96％ |
| Example 3 | 98.0％ | 94％ |
| Example 4 | 98.1％ | 96％ |
| Example 5 | 98.8％ | 97％ |
| Comparative example 1 | 85.3％ | 87％ |
| Comparative example 2 | 90.4％ | 86％ |
| Comparative example 3 | 80.2％ | 90％ |
| Comparative example 4 | 78.2％ | 87％ |
| Comparative example 5 | 94.6％ | 90％ |
Therefore, the extraction yield and purity of the inulin prepared by the invention (examples 1-5) are obviously better than those of the technical scheme (comparative examples 1-3) outside the protection scope of the invention. In addition, compared with the traditional hot water extraction method (comparative example 4), the inulin prepared by the invention omits the extraction process, greatly shortens the extraction time, reduces the energy consumption, and finally the extraction yield and the purity of the inulin are also obviously superior to the products prepared by the traditional method. Compared with other prior art, such as patent CN104987434A (comparison example 5), the inulin production method disclosed by the invention integrates the crushing and extraction processes, further shortens the extraction time, simultaneously reduces the water temperature for extraction, removes impurities in the extracting solution by adopting a method of adjusting pH and passing through a ceramic membrane, avoids the process of heating and cooling firstly required by the method of removing impurities by filling carbon dioxide with lime in comparison example 5, simplifies the process steps, and finally has the yield and the purity of the inulin superior to those of comparison example 5.
Claims (5)
1. A method for extracting inulin from Jerusalem artichoke at low temperature comprises the following steps:
1) cleaning jerusalem artichoke to remove impurities, and pretreating the cleaned jerusalem artichoke by using a solvent;
2) pulverizing pretreated Jerusalem artichoke, adding low-temperature deionized water to obtain Jerusalem artichoke pulp, and separating to obtain Jerusalem artichoke extractive solution and Jerusalem artichoke residue;
3) mixing extractive solutions, adjusting pH, and passing through ceramic membrane to obtain Jerusalem artichoke extractive solution;
4) desalting the Jerusalem artichoke extract clear solution, treating with decolorizing resin, concentrating, and drying to obtain inulin;
wherein, the solvent in the step 1) is one or more of peracetic acid solution, chlorine dioxide solution, ethanol and hydrogen peroxide solution;
wherein the temperature of the deionized water in the step 2) is 5-35 ℃;
wherein the pH value of the extracting solution is adjusted to be 1-7 in the step 3), and the aperture of the ceramic membrane is 5-200 nm;
wherein the type of the resin used for desalting in the step 4) is any one of D001, AM007 and LD 206; the resin type used for decoloring is any one of D900, D941 and D296.
2. The method for low-temperature extraction of inulin from Jerusalem artichoke according to claim 1, wherein the particle size of the pulverized Jerusalem artichoke in the step 2) is 10-300 meshes.
3. The method for low-temperature extraction of inulin from Jerusalem artichoke according to claim 1, wherein the Jerusalem artichoke dregs obtained in step 2) are further extracted repeatedly for 1-3 times by using a centrifugal sieve.
4. The method for extracting inulin from Jerusalem artichoke at low temperature according to claim 1, wherein the amount of deionized water added in step 2) is 1-3 times of the weight of Jerusalem artichoke.
5. The method for low-temperature extraction of inulin from Jerusalem artichoke according to claim 1, wherein nanofiltration membrane is used for concentration in the step 4), and spray drying is adopted for drying.
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| CN110423293A (en) * | 2019-03-13 | 2019-11-08 | 陕西森弗天然制品有限公司 | It is a kind of using jerusalem artichoke as the inulin preparation method of raw material |
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| CN101570580A (en) * | 2009-05-14 | 2009-11-04 | 同济大学 | Clean production process for extracting synanthrin from Jerusalem artichoke |
| WO2012141617A1 (en) * | 2011-04-13 | 2012-10-18 | Artemyev Vladimir Dmitrievich | Method for producing inulin and other fructan-containing products from jerusalem artichoke |
| CN104672352A (en) * | 2014-11-26 | 2015-06-03 | 张利 | Clean production technology for extracting inulin from jerusalem artichoke |
| CN104987434A (en) * | 2015-07-15 | 2015-10-21 | 中国科学院烟台海岸带研究所 | Method for extracting inulin by medium-low-temperature water |
| CN105646734A (en) * | 2016-01-19 | 2016-06-08 | 新疆正生农业资源开发研究院（有限公司） | Production method for inulin |
| CN106632738A (en) * | 2016-12-30 | 2017-05-10 | 晨光生物科技集团股份有限公司 | Industrial production method for extracting inulin from jerusalem artichoke |
| CN107602731A (en) * | 2017-10-09 | 2018-01-19 | 晨光生物科技集团股份有限公司 | A kind of industrialized preparing process for extracting inulin in jerusalem artichoke |
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- 2018-09-28 CN CN201811144283.1A patent/CN109336997B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101570580A (en) * | 2009-05-14 | 2009-11-04 | 同济大学 | Clean production process for extracting synanthrin from Jerusalem artichoke |
| WO2012141617A1 (en) * | 2011-04-13 | 2012-10-18 | Artemyev Vladimir Dmitrievich | Method for producing inulin and other fructan-containing products from jerusalem artichoke |
| CN104672352A (en) * | 2014-11-26 | 2015-06-03 | 张利 | Clean production technology for extracting inulin from jerusalem artichoke |
| CN104987434A (en) * | 2015-07-15 | 2015-10-21 | 中国科学院烟台海岸带研究所 | Method for extracting inulin by medium-low-temperature water |
| CN105646734A (en) * | 2016-01-19 | 2016-06-08 | 新疆正生农业资源开发研究院（有限公司） | Production method for inulin |
| CN106632738A (en) * | 2016-12-30 | 2017-05-10 | 晨光生物科技集团股份有限公司 | Industrial production method for extracting inulin from jerusalem artichoke |
| CN107602731A (en) * | 2017-10-09 | 2018-01-19 | 晨光生物科技集团股份有限公司 | A kind of industrialized preparing process for extracting inulin in jerusalem artichoke |
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