CN113754792A - Preparation method of wolfberry extract containing wolfberry polysaccharide - Google Patents
Preparation method of wolfberry extract containing wolfberry polysaccharide Download PDFInfo
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- 244000241838 Lycium barbarum Species 0.000 title claims abstract description 58
- 235000015459 Lycium barbarum Nutrition 0.000 title claims abstract description 58
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 53
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 53
- 150000004676 glycans Chemical class 0.000 title claims abstract description 52
- 239000000284 extract Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 235000015468 Lycium chinense Nutrition 0.000 title claims abstract description 20
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 50
- 239000008518 lycium barbarum polysaccharide Substances 0.000 claims abstract description 37
- 239000000203 mixture Substances 0.000 claims abstract description 35
- 239000000843 powder Substances 0.000 claims abstract description 35
- 108090000790 Enzymes Proteins 0.000 claims abstract description 28
- 102000004190 Enzymes Human genes 0.000 claims abstract description 28
- 229940088598 enzyme Drugs 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 27
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 26
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229930003268 Vitamin C Natural products 0.000 claims abstract description 25
- 235000019154 vitamin C Nutrition 0.000 claims abstract description 25
- 239000011718 vitamin C Substances 0.000 claims abstract description 25
- 239000000047 product Substances 0.000 claims abstract description 20
- 238000002137 ultrasound extraction Methods 0.000 claims abstract description 20
- 239000006228 supernatant Substances 0.000 claims abstract description 15
- 108010059820 Polygalacturonase Proteins 0.000 claims abstract description 11
- 108010093305 exopolygalacturonase Proteins 0.000 claims abstract description 11
- 238000000926 separation method Methods 0.000 claims abstract description 11
- 108010059892 Cellulase Proteins 0.000 claims abstract description 10
- 108090000526 Papain Proteins 0.000 claims abstract description 10
- 239000004365 Protease Substances 0.000 claims abstract description 10
- 229940106157 cellulase Drugs 0.000 claims abstract description 10
- 229940055729 papain Drugs 0.000 claims abstract description 10
- 235000019834 papain Nutrition 0.000 claims abstract description 10
- 238000004108 freeze drying Methods 0.000 claims abstract description 8
- 239000012528 membrane Substances 0.000 claims abstract description 8
- 235000017784 Mespilus germanica Nutrition 0.000 claims description 23
- 244000182216 Mimusops elengi Species 0.000 claims description 23
- 235000000560 Mimusops elengi Nutrition 0.000 claims description 23
- 235000007837 Vangueria infausta Nutrition 0.000 claims description 23
- 239000002253 acid Substances 0.000 claims description 20
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- 238000010257 thawing Methods 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000007710 freezing Methods 0.000 claims description 8
- 230000008014 freezing Effects 0.000 claims description 8
- 238000010298 pulverizing process Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 2
- 238000000605 extraction Methods 0.000 abstract description 38
- 230000000694 effects Effects 0.000 abstract description 14
- 230000003078 antioxidant effect Effects 0.000 abstract description 10
- 230000015556 catabolic process Effects 0.000 abstract description 5
- 238000006731 degradation reaction Methods 0.000 abstract description 5
- 239000000654 additive Substances 0.000 abstract description 4
- 230000000996 additive effect Effects 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 235000013376 functional food Nutrition 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 16
- 210000004027 cell Anatomy 0.000 description 9
- 210000002421 cell wall Anatomy 0.000 description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 9
- 239000007853 buffer solution Substances 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 4
- 210000004185 liver Anatomy 0.000 description 4
- 238000000643 oven drying Methods 0.000 description 4
- 244000241872 Lycium chinense Species 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 108090000623 proteins and genes Proteins 0.000 description 3
- 102000004169 proteins and genes Human genes 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 206010067125 Liver injury Diseases 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 238000004440 column chromatography Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 231100000753 hepatic injury Toxicity 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 150000002772 monosaccharides Chemical class 0.000 description 2
- 229920001277 pectin Polymers 0.000 description 2
- 239000001814 pectin Substances 0.000 description 2
- 235000010987 pectin Nutrition 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 239000001509 sodium citrate Substances 0.000 description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 2
- 238000003809 water extraction Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 238000012424 Freeze-thaw process Methods 0.000 description 1
- 238000012425 Freezing-thawing process Methods 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 241000208292 Solanaceae Species 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- 238000012668 chain scission Methods 0.000 description 1
- 238000002144 chemical decomposition reaction Methods 0.000 description 1
- -1 compound polysaccharide Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- HHEAADYXPMHMCT-UHFFFAOYSA-N dpph Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1[N]N(C=1C=CC=CC=1)C1=CC=CC=C1 HHEAADYXPMHMCT-UHFFFAOYSA-N 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000004438 eyesight Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000005802 health problem Effects 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000004853 microextraction Methods 0.000 description 1
- 238000000874 microwave-assisted extraction Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920001184 polypeptide Polymers 0.000 description 1
- 102000004196 processed proteins & peptides Human genes 0.000 description 1
- 108090000765 processed proteins & peptides Proteins 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 235000019605 sweet taste sensations Nutrition 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000009777 vacuum freeze-drying Methods 0.000 description 1
Classifications
-
- 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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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- Sustainable Development (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention relates to the technical field of functional food preparation, in particular to a preparation method of a lycium barbarum extract containing lycium barbarum polysaccharide, which comprises the following process steps: (1) micronizing fructus Lycii to obtain fructus Lycii fine powder; (2) adding vitamin C into the fine wolfberry powder to obtain a mixture; (3) adding enzyme into the mixture for ultrasonic extraction, wherein the enzyme is mixed enzyme consisting of cellulase, pectinase and papain; (4) centrifuging the enzymolysis extracting solution, and collecting supernatant; (5) and (3) carrying out ultrafiltration separation on the supernatant by using an ultrafiltration membrane system to obtain a product with a molecular weight section of 10-50kDa, and then carrying out freeze drying on the product to obtain the wolfberry extract containing wolfberry polysaccharide. The invention has the beneficial effects that: the invention combines physical degradation and biological degradation without adding any additive with side effect. The extraction process of the lycium barbarum polysaccharide is green, environment-friendly and safe, and the prepared lycium barbarum polysaccharide is high in extraction rate and purity and strong in antioxidant activity.
Description
Technical Field
The invention relates to the technical field of functional food preparation, in particular to a preparation method of a lycium barbarum extract containing lycium barbarum polysaccharide.
Background
Lycium chinense (Lycium chinense Milll) belongs to Solanaceae, is a traditional Chinese medicinal material used as both medicine and food, has sweet taste and mild nature, and has the functions of nourishing liver and kidney, benefiting essence and blood and improving eyesight. The lycium barbarum polysaccharide is a main effective component of lycium barbarum, is a compound polysaccharide consisting of acidic heteropolysaccharide and polypeptide or protein, has a large molecular weight and a very complex structure composition, has the effects of resisting bacteria, tumors and aging and protecting liver, and is also an active substance of the lycium barbarum for reducing blood sugar, blood pressure, fat and inflammation and the like.
Chinese patent CN101029088 discloses a preparation method of lycium barbarum polysaccharide, wherein lycium barbarum polysaccharide is separated and purified by using column chromatography by using fresh lycium barbarum fruits as raw materials. The whole process comprises the working procedures of soaking, crushing, extracting, enzymolysis, column chromatography, alcohol precipitation, dealcoholization, drying and the like, the extraction solution is treated by pectinase, the purity of the polysaccharide is improved, but the selected enzyme is single, the crushing is conventional crushing, the yield and the antioxidant activity of the polysaccharide cannot be further improved, the raw materials are not fully utilized, and additives such as ethanol and the like which are not beneficial to health are used.
At present, conventional extraction methods of plant polysaccharides comprise a water extraction and alcohol precipitation method, a microwave extraction method, an acid-base decomposition extraction method and the like, most of the conventional methods need high-temperature treatment and the like to be unfavorable for protecting the activity of the polysaccharides, and chemical degradation methods such as water extraction and alcohol precipitation and the like are not environment-friendly enough and can bring health problems. The conventional method for preparing the lycium barbarum polysaccharide also easily causes the defects of easy chain scission of molecular weight, deepened browning of product color, loss of biological activity and the like.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: provides a preparation method of the lycium barbarum extract containing lycium barbarum polysaccharide, which is green and environment-friendly and has high extraction rate and purity.
The technical scheme provided by the invention is as follows: provides a preparation method of a medlar extract containing medlar polysaccharide, which comprises the following process steps:
(1) micronizing fructus Lycii to obtain fructus Lycii fine powder;
(2) adding 8-12 times of water by weight into the medlar fine powder, and adding vitamin C to obtain a mixture;
(3) adding enzyme into the mixture for ultrasonic extraction to obtain an enzymolysis extracting solution; the enzyme is a mixed enzyme consisting of cellulase, pectinase and papain;
(4) centrifuging the enzymolysis extracting solution, and collecting supernatant;
(5) and (3) carrying out ultrafiltration separation on the supernatant by using an ultrafiltration membrane system to obtain a product with a molecular weight of 10-50kDa, and freeze-drying the product to obtain freeze-dried powder, namely the lycium barbarum extract containing lycium barbarum polysaccharide.
The invention has the beneficial effects that: the preparation method of the lycium barbarum extract containing lycium barbarum polysaccharide combines physical degradation and biodegradation, no additive with side effect is added, the extraction process is green, environment-friendly and safe, and the prepared lycium barbarum polysaccharide is high in extraction rate and purity and strong in antioxidant activity. The extraction rate of the existing ultrafiltration polysaccharide extraction method is low, in the preparation method, the medlar is firstly subjected to superfine grinding technology to destroy the cell structure, then is soaked by vitamin C, and finally is subjected to ultrasonic enzyme combined extraction, so that the extraction rate of the medlar polysaccharide is improved to the greatest extent, and the vitamin C is used for protecting the extract, so that the obtained extract has the advantage of white color.
Detailed Description
In order to explain the technical content, the objects and the effects of the present invention in detail, the following description will be given with reference to the embodiments.
The invention provides a preparation method of a wolfberry extract containing wolfberry polysaccharide, which comprises the following process steps:
(1) micronizing fructus Lycii to obtain fructus Lycii fine powder;
(2) adding 8-12 times of water by weight into the medlar fine powder, and adding vitamin C to obtain a mixture;
(3) adding enzyme into the mixture for ultrasonic extraction to obtain an enzymolysis extracting solution; the enzyme is a mixed enzyme consisting of cellulase, pectinase and papain;
(4) centrifuging the enzymolysis extracting solution, and collecting supernatant;
(5) and (3) carrying out ultrafiltration separation on the supernatant by using an ultrafiltration membrane system to obtain a product with a molecular weight of 10-50kDa, and freeze-drying the product to obtain freeze-dried powder, namely the lycium barbarum extract containing lycium barbarum polysaccharide.
The invention combines physical degradation and biological degradation without adding any additive with side effect, the polysaccharide extraction process is green, environment-friendly and safe, and the prepared lycium barbarum polysaccharide has high extraction rate and purity and strong antioxidant activity.
The invention adopts the superfine grinding technology to pretreat the material, and the superfine grinding technology can greatly destroy the cell structure and even break the cell wall, so that the polysaccharide component existing in the cell is exposed, and the polysaccharide extraction rate can be improved. Meanwhile, the granularity of the extract is greatly reduced, the contact area of the extract and an extraction solvent is increased, and the dissolution speed of the polysaccharide is improved; the invention also protects the polysaccharide active polysaccharide molecules from being easily broken by vitamin C, so that the finally prepared wolfberry polysaccharide product has good color and luster, and can further protect the antioxidant activity of the wolfberry polysaccharide from being damaged; the invention also assists ultrasonic enzyme extraction treatment, and a plurality of enzymes are combined for use to more fully hydrolyze pectin, cellulose, polysaccharide and the like in the medlar, decompose cell wall components, destroy cell wall structures, generate local collapse, dissolution and loosening, reduce resistance from cell walls and intercellular substances during extraction, accelerate the speed of dissolving out cells of effective components and improve extraction efficiency. And enzymolysis is carried out on protein and other impurities, so that the polysaccharide is extracted more thoroughly and has higher purity. The lycium barbarum polysaccharides with the molecular weight of 10-50kDa extracted by ultrafiltration comprise polysaccharides of the effective part of lycium barbarum, and the balance of monosaccharides with small molecular weight or impurities in larger molecules.
Preferably, in the preparation method of the lycium barbarum extract containing lycium barbarum polysaccharide, the step (1) is specifically as follows: pulverizing fructus Lycii, drying at 40-50 deg.C, and micronizing the coarse powder in micronizer to obtain 300-400 mesh fructus Lycii fine powder.
Preferably, in the above method for preparing an extract of lycium barbarum containing lycium barbarum polysaccharides, the step (2) further comprises: the mixture is rapidly cooled to-20 to-16 ℃, frozen for 2 to 4 hours and then rapidly thawed by microwave, and the microwave power is 3500 and 5000W. Repeating the steps of rapidly cooling to-20 to-16 ℃, freezing for 2-4 hours and then rapidly thawing by microwave for 3 times. The rapid cooling to-20 to-16 ℃ means that the temperature is reduced to-20 to-16 ℃ within 1-3 min.
As can be seen from the above description, in the low-temperature freeze-thaw process of the present invention, a huge temperature difference is generated due to uneven temperature changes inside and outside the cell, and the thermal shock effect caused by the temperature difference can effectively destroy the cell structure, so that the polysaccharide components inside the cell can be sufficiently dissolved out, the polysaccharide leaching rate can be effectively improved, and the low-temperature freeze-thaw extraction process is always performed at a lower temperature, thereby effectively reducing the loss of the active components of the polysaccharide.
Preferably, in the above method for preparing an extract of lycium barbarum containing lycium barbarum polysaccharides, the step (2) is specifically: adding 8-12 times of water into the fructus Lycii fine powder, adding vitamin C and edible acid, and treating for 30-60min to obtain mixture.
From the above description, the present invention further decomposes cell walls by adding edible acid, thereby improving extraction yield.
Preferably, in the preparation method of the lycium barbarum extract containing lycium barbarum polysaccharide, the addition amount of the vitamin C is 1.5-3g/L, the mass concentration of the edible acid in the mixture after the edible acid is added is 3-5%, and the edible acid is acetic acid.
Preferably, in the preparation method of the lycium barbarum extract containing lycium barbarum polysaccharide, the addition amount of the enzyme is 1-3% of the mixture by mass, and the addition mass ratio of the cellulase, the pectinase and the papain is 1:2: 3.
Preferably, in the preparation method of the lycium barbarum extract containing lycium barbarum polysaccharide, the ultrasonic extraction conditions are as follows: the temperature is 20-40 ℃; the ultrasonic power is 500-1700W; the circulating stirring speed is 500-2000 rpm; duty ratio 1: 1-1: 3; ultrasonic extraction time is 0.5-2 h.
Preferably, in the above method for preparing an extract of lycium barbarum containing lycium barbarum polysaccharides, the step (4) is specifically: centrifuging the enzymolysis extracting solution at 4000-.
The preparation method of the lycium barbarum extract containing lycium barbarum polysaccharide has the following advantages:
1. the invention adopts the superfine powder technology, improves the extraction efficiency, reduces the molecular weight of the extracted polysaccharide and ensures that the prepared polysaccharide has higher antioxidant activity.
2. According to the invention, the active polysaccharide molecules of the polysaccharide are protected by the vitamin C, so that the chains are not easily broken, the finally prepared wolfberry polysaccharide product has good color and luster, and the antioxidant activity of the wolfberry polysaccharide is further improved. The invention can be added with edible acid to further decompose cell walls and synergistically improve the vitamin C protection function.
3. The invention also assists ultrasonic enzyme extraction treatment, and a plurality of enzymes are combined for use to more fully hydrolyze pectin, cellulose, polysaccharide and the like in the medlar, decompose cell wall components, destroy cell wall structures, generate local collapse, dissolution and loosening, reduce resistance from cell walls and intercellular substances during extraction, accelerate the speed of dissolving out cells of effective components and improve extraction efficiency. And enzymolysis is carried out on protein and other impurities, so that the polysaccharide is extracted more thoroughly and has higher purity.
4. The lycium barbarum polysaccharide with the molecular weight of 10-50kDa extracted by ultrafiltration comprises the polysaccharide of the effective part of lycium barbarum, and the impurities in the rest monosaccharide with small molecular weight or larger molecules are discarded, so that the purity of the polysaccharide is improved.
5. The invention also adopts a low-temperature freeze thawing technology, and utilizes the thermal shock effect generated in the freezing-thawing process to destroy the cell structure, thereby achieving the purpose of increasing the extraction rate and activity of the polysaccharide.
Example 1
A preparation method of a medlar extract containing medlar polysaccharide comprises the following process steps:
(1) pulverizing fructus Lycii, oven drying at 30 deg.C, and micronizing the coarse powder in micronizer to obtain 400-mesh fructus Lycii fine powder.
(2) Adding 10 times of water by weight of the medlar fine powder, and adding vitamin C to obtain a mixture; the addition amount of the vitamin C is 2 g/L.
(3) Adding enzyme into the mixture obtained in the step (2) for ultrasonic extraction to obtain an enzymolysis extracting solution; the ultrasonic extraction conditions are as follows: the temperature is 20 ℃; the ultrasonic power is 500W; the circulating stirring speed is 500 rpm; duty ratio 1: 3; ultrasonic extraction time is 0.5 h; the adding mass percentage of the enzyme in the mixture is 1%, and the adding mass ratio of the cellulase, the pectinase and the papain is 1:2: 3.
(4) Centrifuging the enzymolysis extracting solution at the rotating speed of 4000r/min for 10min, and collecting the supernatant.
(5) And (3) carrying out ultrafiltration separation on the supernatant by using an ultrafiltration membrane system to obtain a product with a molecular weight of 10-50kDa, and freeze-drying the product to obtain freeze-dried powder, namely the lycium barbarum extract containing lycium barbarum polysaccharide.
Example 2
A preparation method of a medlar extract containing medlar polysaccharide comprises the following process steps:
(1) pulverizing fructus Lycii, oven drying at 30 deg.C, and micronizing the coarse powder in micronizer to obtain 400-mesh fructus Lycii fine powder.
(2) Adding 10 times of water by weight into the medlar fine powder, and then adding vitamin C and acetic acid for treatment for 50min to obtain a mixture; the addition amount of the vitamin C is 2g/L, and the mass concentration of the acetic acid in the mixture after the acetic acid is added is 2%.
And (3) reducing the temperature of the mixture to-20 ℃ within 2min, freezing for 2 hours, and then rapidly thawing by microwave, wherein the microwave power is 3500W. Repeating the steps of rapidly cooling to-20 ℃, freezing for 2 hours and then rapidly thawing by microwave for 3 times.
(3) Adding enzyme into the mixture obtained in the step (2) for ultrasonic extraction to obtain an enzymolysis extracting solution; the ultrasonic extraction conditions are as follows: the temperature is 20 ℃; the ultrasonic power is 500W; the circulating stirring speed is 500 rpm; duty ratio 1: 3; ultrasonic extraction time is 0.5 h;
the adding mass percentage of the enzyme in the mixture is 1%, and the adding mass ratio of the cellulase, the pectinase and the papain is 1:2: 3.
(4) Centrifuging the enzymolysis extracting solution at the rotating speed of 4000r/min for 10min, and collecting the supernatant.
(5) And (3) carrying out ultrafiltration separation on the supernatant by using an ultrafiltration membrane system to obtain a product with a molecular weight of 10-50kDa, and freeze-drying the product to obtain freeze-dried powder, namely the lycium barbarum extract containing lycium barbarum polysaccharide.
Example 3
The procedure of example 1 was repeated except that the ultrafine pulverization in step (1) was not conducted to obtain a fine powder of Lycium chinense having a mesh size of 50 mesh, as compared with example 2.
Example 4
Same as example 1 except that no vitamin C was added in step (1) compared to example 2.
Example 5
The procedure was as in example 1 except that the rapid cooling and microwave thawing in step (2) were not conducted, as compared with example 2.
Example 6
Compared with the example 2, the method is the same as the example 1 except that the ultrafiltration separation in the step (5) obtains the product with the molecular weight section of 1-100 kDa.
The purity, extraction rate and DPPH clearance of the Lycium barbarum polysaccharides of the Lycium barbarum extracts prepared in examples 1-6 are shown in Table 1.
TABLE 1
Compared with the example 1, the purity, the extraction rate and the antioxidant activity of the lycium barbarum polysaccharide are greatly improved by performing microwave thawing treatment after edible acid and rapid cooling;
as can be seen from the comparison between the example 3 and the example 2, the ultra-micro extraction has a great effect on the extraction rate and the antioxidant activity of the lycium barbarum polysaccharide;
as can be seen from the comparison between example 4 and example 2, vitamin C has a greater effect on protecting the activity of polysaccharides and improving the antioxidant activity of lycium barbarum polysaccharides;
as can be seen from the comparison between example 5 and example 2, the microwave thawing after the rapid cooling also has a great effect on the extraction rate of the lycium barbarum polysaccharide.
From the above results, it can be seen that: according to the invention, by adopting a combined extraction mode of ultramicro extraction, vitamin C and edible acid addition, cooling and microwave thawing, compared with the mode lacking one of the extraction modes, the prepared wolfberry extract containing wolfberry polysaccharide has higher purity, extraction rate and oxidation resistance. Thus, the synergistic effect is achieved between the combination of vitamin C and edible acid, cooling, microwave thawing and ultrafiltration separation extraction.
Example 7
A preparation method of a medlar extract containing medlar polysaccharide comprises the following process steps:
(1) pulverizing fructus Lycii, oven drying at 50 deg.C, and micronizing the coarse powder in micronizer to obtain 400 mesh fructus Lycii fine powder.
(2) Adding 12 times of water into the medlar fine powder, and then adding vitamin C and edible acid for treatment for 60min to obtain a mixture; the addition amount of the vitamin C is 3g/L, the mass concentration of the added edible acid in the mixture is 5%, and the edible acid is citric acid.
And (3) reducing the temperature of the mixture to-20 ℃ within 3min, freezing for 4 hours, and then quickly thawing by microwave, wherein the microwave power is 5000W.
Repeating the steps of rapidly cooling to-20 ℃, freezing for 4 hours and then rapidly thawing by microwave for 3 times.
(3) Adding enzyme into the mixture obtained in the step (2), adding a buffer solution to prepare a pH value of 5, wherein the buffer solution is a mixed buffer solution of citric acid and sodium citrate, and then carrying out ultrasonic extraction to obtain an enzymolysis extracting solution;
the ultrasonic extraction conditions are as follows: the temperature is 40 ℃; the ultrasonic power is 1700W; the circulating stirring speed is 2000 rpm; duty ratio 1: 1; ultrasonic extraction time is 2 h;
the adding mass percentage of the enzyme in the mixture is 3%, and the adding mass ratio of the cellulase to the pectinase to the papain is 1:2: 3.
(4) Centrifuging the enzymolysis extractive solution at 5000r/min for 15min, and collecting supernatant.
(5) And (3) carrying out ultrafiltration separation on the supernatant by using an ultrafiltration membrane system to obtain a product with a molecular weight of 10-50kDa, and freeze-drying the product to obtain freeze-dried powder, namely the lycium barbarum extract containing lycium barbarum polysaccharide. The pressure of the vacuum freeze drying treatment is 0.5-0.6 mbar, and the temperature is-5-30 ℃.
The extract obtained in this example had a purity of 75.2% for lycium barbarum polysaccharides and an extraction rate of 95.7%.
Example 8
A preparation method of a medlar extract containing medlar polysaccharide comprises the following process steps:
(1) pulverizing fructus Lycii, oven drying at 40 deg.C, and micronizing the coarse powder in micronizer to obtain 300-mesh fructus Lycii fine powder.
(2) Adding 10 times of water by weight into the medlar fine powder, and then adding vitamin C and edible acid for treatment for 45min to obtain a mixture; the addition amount of the vitamin C is 2g/L, the mass concentration of the edible acid in the mixture after the edible acid is added is 4%, and the edible acid is acetic acid.
And (3) cooling the mixture to-18 ℃ within 2min, freezing for 3 hours, and then quickly thawing by using microwaves, wherein the microwave power is 4000W. Repeating the steps of rapidly cooling to-18 ℃, freezing for 3 hours and then rapidly thawing by microwave for 3 times.
(3) Adding enzyme into the mixture obtained in the step (2), adding a buffer solution to prepare a pH value of 4, wherein the buffer solution is a mixed buffer solution of citric acid and sodium citrate, and then carrying out ultrasonic extraction to obtain an enzymolysis extracting solution;
the ultrasonic extraction conditions are as follows: the temperature is 30 ℃; the ultrasonic power is 1000W; the circulating stirring speed is 1000 rpm; duty ratio 1: 1-1: 3; ultrasonic extraction time is 0.5-2 h;
the adding mass percentage of the enzyme in the mixture is 2%, and the adding mass ratio of the cellulase to the pectinase to the papain is 1:2: 3.
(4) Centrifuging the enzymolysis extracting solution at the rotating speed of 4000-.
(5) And (3) carrying out ultrafiltration separation on the supernatant by using an ultrafiltration membrane system to obtain a product with a molecular weight range of 10-50kDa, and then carrying out freeze drying on the product. The obtained freeze-dried powder is the medlar extract containing medlar polysaccharide.
The ultrafiltration separation specifically comprises the following steps: performing ultrafiltration with ultrafiltration device with molecular weight cut-off of 10kDa to retain solution with molecular weight greater than 10kDa, and performing ultrafiltration with ultrafiltration device with molecular weight cut-off of 50kDa to retain solution with molecular weight less than 50 kDa.
The purity of the lycium barbarum polysaccharide of the lycium barbarum extract containing lycium barbarum polysaccharide obtained in the example is 77.6%, and the extraction rate is 96.3%.
The lycium barbarum polysaccharide of the lycium barbarum extract containing lycium barbarum polysaccharide provided by the invention has high purity, white color, excellent quality and high extraction rate which can reach more than 75%, has good effect of protecting liver, and can be used for developing medicines, health-care foods or special medical formula foods for protecting liver, alcoholic liver injury and chemical liver injury.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent modifications made by the present invention in the specification or directly or indirectly applied to the related technical field are included in the scope of the present invention.
Claims (10)
1. A preparation method of a wolfberry extract containing wolfberry polysaccharide is characterized by comprising the following steps:
(1) micronizing fructus Lycii to obtain fructus Lycii fine powder;
(2) adding 8-12 times of water by weight into the medlar fine powder, and adding vitamin C to obtain a mixture;
(3) adding enzyme into the mixture for ultrasonic extraction to obtain an enzymolysis extracting solution; the enzyme is a mixed enzyme consisting of cellulase, pectinase and papain;
(4) centrifuging the enzymolysis extracting solution, and collecting supernatant;
(5) and (3) carrying out ultrafiltration separation on the supernatant by using an ultrafiltration membrane system to obtain a product with a molecular weight of 10-50kDa, and freeze-drying the product to obtain freeze-dried powder, namely the lycium barbarum extract containing lycium barbarum polysaccharide.
2. The method for preparing the lycium barbarum extract containing lycium barbarum polysaccharide according to claim 1, wherein the step (1) is specifically as follows: pulverizing fructus Lycii, drying at 40-50 deg.C, and micronizing the coarse powder in micronizer to obtain 300-400 mesh fructus Lycii fine powder.
3. The method for preparing the lycium barbarum extract containing lycium barbarum polysaccharides according to claim 1, wherein the step (2) further comprises: the mixture is rapidly cooled to-20 to-16 ℃, frozen for 2 to 4 hours and then rapidly thawed by microwave, and the microwave power is 3500 and 5000W.
4. The process of claim 3, wherein the step of rapidly cooling to-20 to-16 ℃ and freezing for 2-4 hours followed by rapid microwave thawing is repeated for 3 times.
5. The method of claim 4, wherein the "rapid cooling to-20 to-16 ℃ C" means that the temperature is reduced to-20 to-16 ℃ C within 1-3 min.
6. The method for preparing the lycium barbarum extract containing lycium barbarum polysaccharide according to claim 1, wherein the step (2) is specifically as follows: adding 8-12 times of water into the fructus Lycii fine powder, adding vitamin C and edible acid, and treating for 30-60min to obtain mixture.
7. The method for preparing the lycium barbarum extract containing lycium barbarum polysaccharide according to claim 1, wherein the vitamin C is added in an amount of 1.5-3g/L, the mass concentration of the edible acid in the mixture after the edible acid is added is 3-5%, and the edible acid is acetic acid.
8. The method for preparing the lycium barbarum extract containing lycium barbarum polysaccharide according to claim 1, wherein the addition amount of the enzyme is 1-3% of the mixture by mass, and the addition mass ratio of the cellulase, the pectinase and the papain is 1:2: 3.
9. The method for preparing the lycium barbarum extract containing lycium barbarum polysaccharide according to claim 1, wherein the ultrasonic extraction conditions are as follows: the temperature is 20-40 ℃; the ultrasonic power is 500-1700W; the circulating stirring speed is 500-2000 rpm; duty ratio 1: 1-1: 3; ultrasonic extraction time is 0.5-2 h.
10. The method for preparing the lycium barbarum extract containing lycium barbarum polysaccharide according to claim 1, wherein the step (4) is specifically as follows: centrifuging the enzymolysis extracting solution at 4000-.
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