CN111116766A - Method for extracting lycium barbarum polysaccharide by using ultrahigh pressure technology - Google Patents
Method for extracting lycium barbarum polysaccharide by using ultrahigh pressure technology Download PDFInfo
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- CN111116766A CN111116766A CN201811293820.9A CN201811293820A CN111116766A CN 111116766 A CN111116766 A CN 111116766A CN 201811293820 A CN201811293820 A CN 201811293820A CN 111116766 A CN111116766 A CN 111116766A
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- 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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- C—CHEMISTRY; METALLURGY
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- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
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Abstract
The invention relates to a method for extracting lycium barbarum polysaccharide. The invention applies the ultrahigh pressure technology, which is a processing method that the pressure is more than 100MPa to the raw material under the conditions of normal temperature and near normal temperature, the ultrahigh pressure can lead the solvent to enter the interior of plant cells, the solvent can overflow with effective components after pressure relief, high extraction efficiency of the effective components of the plant is realized, the macroporous resin is used for absorbing and purifying the lycium barbarum polysaccharide, the absorption selectivity to the lycium barbarum polysaccharide is good, the absorption speed is fast, the resolution is fast, the absorption capacity is large, and the defects of relatively low extraction rate, low extraction purity and the like of the conventional technology are overcome.
Description
Technical Field
The invention belongs to the field of natural organic chemistry, relates to a purification method of lycium barbarum polysaccharide, and particularly relates to a method for extracting lycium barbarum polysaccharide from lycium barbarum by an ultrahigh pressure technology.
Background
The medlar is not only a traditional rare Chinese medicinal material in China but also a common food ingredient in folk, and has various pharmacological effects and biological activity functions. Modern medical clinical research considers that the lycium barbarum polysaccharide extracted from the lycium barbarum is one of the main effective components of the lycium barbarum biological action, and the lycium barbarum polysaccharide becomes an important functional additive of health-care food. In recent years, the research on polysaccharides in China is rapidly advanced, and the extraction and separation, chemical analysis, pharmacological action and clinical application of the lycium barbarum polysaccharides have wide research foundation and show good application prospects.
The traditional Chinese wolfberry treatment method comprises the following steps: picking fructus Lycii, air drying, sun drying, soaking in wine, making tea, and cooking soup or taking as medicine. Scientific research shows that the traditional mode can not effectively retain the nutrient components of fresh wolfberry fruits, and the active components such as wolfberry polysaccharide and various amino acids such as taurine in dried, sunned and dehydrated wolfberry fruits can be lost or damaged. In addition, the waxy layer on the surface of the medlar makes the dried medlar soup or water-soaking difficult to completely absorb the nutrient components of the medlar.
Disclosure of Invention
Therefore, the invention provides an extraction process of lycium barbarum polysaccharide, which is used for solving the problems of long time consumption, high energy consumption, low yield, degradation of polysaccharide by high temperature and damaged biological activity of polysaccharide caused by traditional hot water extraction of lycium barbarum polysaccharide.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for extracting lycium barbarum polysaccharide from lycium barbarum by using an ultrahigh pressure technology comprises the following steps:
(1) screening the wolfberry fruits to remove impurities and diseased fruits in the wolfberry fruits;
(2) drying fructus Lycii at 50 deg.C under vacuum for 24 hr;
(3) crushing the dried wolfberry fruits by using a particle crusher at normal temperature;
(4) sieving crushed wolfberry fruits by a sieve of 60-80 meshes, putting into a pressure-resistant bag, adding ethanol with the volume of 10-12 times and the concentration of 70-90%, treating under the conditions of ultrahigh pressure of 200MPA and 300MPA for 10-15min and 18-20 ℃, recovering ethanol, and performing vacuum drying at 60 ℃ to obtain a crude product;
(5) dissolving the obtained crude lycium barbarum polysaccharide powder with a proper amount of 75% ethanol, adjusting the pH value to 3.0-7.5, heating to 40-60 ℃, adding 1.0-2.0% of pectinase (100 ten thousand u/ml), uniformly mixing, and keeping enzymolysis for 0.5-3 h. Cooling to room temperature, standing, filtering, removing residue, and concentrating the filtrate under reduced pressure to obtain fructus Lycii polysaccharide crude extract;
(6) adsorbing the obtained crude extract of the lycium barbarum polysaccharide by using macroporous adsorption resin; the macroporous adsorbent resin is one of X-5, NKA-9, S-8, D3520, D4006, H103, D4020, AB-8H and LX-100 type resins, and the adsorption is static adsorption or dynamic adsorption.
(7) Eluting the macroporous adsorption resin by using ethanol with different concentrations (70-90%), tracking and detecting by using a thin-layer chromatography, and collecting eluent of each stage of the lycium barbarum polysaccharide; the elution is carried out by ethanol
(8) Concentrating eluate of fructus Lycii polysaccharide at each stage, and recovering ethanol to obtain fructus Lycii polysaccharide semi-finished product with content of above 40%;
(9) loading the obtained semi-finished product of fructus Lycii polysaccharide on silica gel chromatographic column, eluting with n-butanol and chloroform at different volume ratios, tracking and detecting by thin layer chromatography, and collecting eluate of fructus Lycii polysaccharide at each stage;
(10) dissolving the product with 6-8 times volume of 60-80% ethanol, concentrating to one tenth of the original volume, standing overnight to obtain crystal; separating crystal, dissolving the remainder with 50% -60% ethanol, concentrating again, recrystallizing, and repeating the above steps twice to obtain refined lycium barbarum polysaccharide with content of more than 90%.
The invention applies the ultrahigh pressure technology which is a processing method for applying pressure greater than 100 hydrostatic pressure to raw materials at normal temperature and near normal temperature, the ultrahigh pressure can enable a solvent to enter plant cells, the solvent can overflow with effective components after pressure relief, high extraction efficiency of the effective components of the plant is realized, the lycium barbarum polysaccharide is adsorbed and purified by using macroporous resin, the adsorption selectivity of the lycium barbarum polysaccharide is good, the adsorption speed and the resolution are fast, and the adsorption capacity is larger;
the invention selects the macroporous adsorption resin with stable physicochemical property, larger surface area, higher exchange speed, high mechanical strength, strong pollution resistance and good thermal stability, is not compatible with acid, alkali and organic medium, has better selectivity to organic matters, is not influenced by the existence of inorganic salts and strong ion low molecular compounds, can selectively adsorb the lycium barbarum polysaccharide from the solution through physical adsorption, and has fast adsorption, fast analysis and larger adsorption capacity.
The specific implementation mode is as follows:
example 1
A method for extracting lycium barbarum polysaccharide from lycium barbarum by using an ultrahigh pressure technology comprises the following steps:
(1) screening the wolfberry fruits to remove impurities and diseased fruits in the wolfberry fruits;
(2) drying fructus Lycii at 50 deg.C under vacuum for 24 hr;
(3) crushing the dried wolfberry fruits by using a particle crusher at normal temperature;
(4) sieving pulverized fructus Lycii with 60 mesh sieve, placing into pressure-resistant bag, adding 10 times volume of 70% ethanol, treating under ultrahigh pressure of 200MPA at 18 deg.C for 10min, recovering ethanol, and vacuum drying at 60 deg.C to obtain crude product;
(5) dissolving the obtained crude powder of fructus Lycii polysaccharide with appropriate amount of 75% ethanol, adjusting pH to 5.5, heating to 60 deg.C, adding pectase (100 ten thousand u/ml) 2.0%, mixing, and maintaining enzymolysis for 0.5 h. Cooling to room temperature, standing, filtering, removing residue, and concentrating the filtrate under reduced pressure to obtain fructus Lycii polysaccharide crude extract;
(6) adsorbing the crude extract with LX-100 type macroporous adsorbent resin;
(7) eluting macroporous adsorbent resin with 70%, 80%, 90% ethanol, detecting by thin layer chromatography, and collecting eluate of fructus Lycii polysaccharide at each stage;
(8) concentrating eluate of fructus Lycii polysaccharide at each stage, and recovering ethanol to obtain fructus Lycii polysaccharide semi-finished product with content of 46.3%;
(9) loading the obtained semi-finished product of Lycium barbarum polysaccharides onto silica gel chromatography column, eluting with n-butanol and chloroform at a ratio of 1: 3, 1: 4, 1: 5, 1: 6, and 1: 7, tracking and detecting by thin layer chromatography, and collecting eluate of Lycium barbarum polysaccharides at each stage;
(10) dissolving the product with 60% ethanol 6 times the volume of the product, concentrating to one tenth of the original volume, and standing overnight to obtain crystals; separating crystal, dissolving the residue with 50% ethanol, concentrating again, recrystallizing, and repeating the above steps twice to obtain refined fructus Lycii polysaccharide with content of more than 92.5%.
Example 2
A method for extracting lycium barbarum polysaccharide from lycium barbarum by using an ultrahigh pressure technology comprises the following steps:
(1) screening the wolfberry fruits to remove impurities and diseased fruits in the wolfberry fruits;
(2) drying fructus Lycii at 50 deg.C under vacuum for 24 hr;
(3) crushing the dried wolfberry fruits by using a particle crusher at normal temperature;
(4) sieving crushed fructus Lycii with 80 mesh sieve, placing into pressure-resistant bag, adding 12 times volume of 90% ethanol, treating under ultrahigh pressure 300MPA at 20 deg.C for 15min, recovering ethanol, and vacuum drying at 60 deg.C to obtain crude product;
(5) dissolving the obtained crude powder of fructus Lycii polysaccharide with appropriate amount of 75% ethanol, adjusting pH to 7.5, heating to 60 deg.C, adding pectase (100 ten thousand u/ml) 2.0%, mixing, and maintaining enzymolysis for 1.5 h. Cooling to room temperature, standing, filtering, removing residue, and concentrating the filtrate under reduced pressure to obtain fructus Lycii polysaccharide crude extract;
(6) adsorbing the obtained crude extract with AB-8H macroporous adsorbent resin;
(7) eluting macroporous adsorbent resin with 70%, 80%, 90% ethanol, tracking and detecting with thin layer chromatography, and collecting eluate of fructus Lycii polysaccharide at each stage;
(8) concentrating eluate of fructus Lycii polysaccharide at each stage, and recovering ethanol to obtain fructus Lycii polysaccharide semi-finished product with content of above 41.4%;
(9) loading the obtained semi-finished product of Lycium barbarum polysaccharides onto silica gel chromatography column, eluting with n-butanol and chloroform at a ratio of 1: 3, 1: 4, 1: 5, 1: 6, and 1: 7, tracking and detecting by thin layer chromatography, and collecting eluate of Lycium barbarum polysaccharides at each stage;
(10) dissolving the product with 80% ethanol 8 times the volume of the product, concentrating to one tenth of the original volume, and standing overnight to obtain crystals; separating crystal, dissolving the residue with 60% ethanol, concentrating again, recrystallizing, and repeating the above steps twice to obtain refined fructus Lycii polysaccharide with content of 91.7%.
Embodiment 3
A method for extracting lycium barbarum polysaccharide from lycium barbarum by using an ultrahigh pressure technology comprises the following steps:
(1) screening the wolfberry fruits to remove impurities and diseased fruits in the wolfberry fruits;
(2) drying fructus Lycii at 50 deg.C under vacuum for 24 hr;
(3) crushing the dried wolfberry fruits by using a particle crusher at normal temperature;
(4) sieving crushed fructus Lycii with 80 mesh sieve, placing into pressure-resistant bag, adding 12 times volume of 80% ethanol, treating under ultrahigh pressure of 200MPA at 18 deg.C for 12min, recovering ethanol, and vacuum drying at 60 deg.C to obtain crude product;
(5) dissolving the obtained crude powder of fructus Lycii polysaccharide with appropriate amount of 75% ethanol, adjusting pH to 4.5, heating to 50 deg.C, adding 1.5% pectase (100 ten thousand u/ml), mixing, and maintaining enzymolysis for 2 hr. Cooling to room temperature, standing, filtering, removing residue, and concentrating the filtrate under reduced pressure to obtain fructus Lycii polysaccharide crude extract;
(6) adsorbing the obtained crude extract of fructus Lycii polysaccharide with H103 macroporous adsorbent resin;
(7) eluting macroporous adsorbent resin with 70%, 80%, 90% ethanol, and thin layer chromatography
Tracking and detecting, and collecting eluent of each stage of the lycium barbarum polysaccharide;
(8) concentrating eluate of fructus Lycii polysaccharide at each stage, and recovering ethanol to obtain fructus Lycii polysaccharide semi-finished product with content of 42.6%;
(9) loading the obtained semi-finished product of Lycium barbarum polysaccharides onto silica gel chromatography column, eluting with n-butanol and chloroform at a ratio of 1: 3, 1: 4, 1: 5, 1: 6, and 1: 7, tracking and detecting by thin layer chromatography, and collecting eluate of Lycium barbarum polysaccharides at each stage;
(10) dissolving the product with 70% ethanol 8 times the volume of the product, concentrating to one tenth of the original volume, and standing overnight to obtain crystals; separating crystal, dissolving the residue with 60% ethanol, concentrating again, recrystallizing, and repeating the above steps twice to obtain refined fructus Lycii polysaccharide with content of 93.6%.
Claims (3)
1. A method for extracting lycium barbarum polysaccharide from lycium barbarum by using an ultrahigh pressure technology comprises the following steps:
(1) pulverizing dried fructus Lycii, sieving with 60-80 mesh sieve, placing into pressure-resistant bag, adding 10-12 times volume of 70% -90% ethanol, treating under ultrahigh pressure of 200MPA at 10-15min and 18-20 deg.C, recovering ethanol, and vacuum drying at 60 deg.C to obtain crude product;
(2) dissolving the obtained crude lycium barbarum polysaccharide powder with a proper amount of 75% ethanol, adjusting the pH value to 3.0-7.5, heating to 40-60 ℃, adding 1.0-2.0% of pectinase (100 ten thousand u/ml), uniformly mixing, and keeping enzymolysis for 0.5-3 h. Cooling to room temperature, standing, filtering, removing residue, and concentrating the filtrate under reduced pressure to obtain fructus Lycii polysaccharide crude extract;
(3) adsorbing the obtained crude extract of the lycium barbarum polysaccharide by using macroporous adsorption resin;
(4) eluting macroporous adsorbent resin with ethanol of different concentrations, detecting by thin layer chromatography, and collecting Lycium barbarum extract
Eluent in each stage of sugar;
(5) concentrating eluate of fructus Lycii polysaccharide at each stage, and recovering ethanol to obtain fructus Lycii polysaccharide semi-finished product with content of above 40%;
(6) loading the obtained semi-finished product of fructus Lycii polysaccharide on silica gel chromatographic column, eluting with n-butanol and chloroform at different volume ratios, tracking and detecting by thin layer chromatography, and collecting eluate of fructus Lycii polysaccharide at each stage;
(7) dissolving the product with 6-8 times volume of 60-80% ethanol, concentrating to one tenth of the original volume, standing overnight to obtain crystal; separating crystal, dissolving the remainder with 50% -60% ethanol, concentrating again, recrystallizing, and repeating the above steps twice to obtain refined lycium barbarum polysaccharide with content of more than 90%.
The macroporous adsorption resin used in the step (3) is one of resins of X-5, NKA-9, S-8, D3520, D4006, H103, D4020, AB-8H and LX-100, and the adsorption is static adsorption or dynamic adsorption.
And (4) eluting by using 70-90% ethanol.
2. The method for extracting the lycium barbarum polysaccharide from the lycium barbarum by using the ultrahigh pressure technology according to claim 1, which is characterized in that: in the step (1), the medlar powder is sieved by a sieve of 60-80 meshes and then is subjected to ultrahigh pressure extraction.
3. The method for extracting lycium barbarum polysaccharide from lycium barbarum by using the ultrahigh pressure technology as claimed in claim l, wherein the method comprises the following steps: in the step (2), after the ultrahigh pressure extraction is finished, the enzymolysis technology is utilized for re-extraction.
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| CN115040894A (en) * | 2022-06-09 | 2022-09-13 | 广州泽力医药科技有限公司 | Low-temperature efficient nutrient component extraction technology |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115040894A (en) * | 2022-06-09 | 2022-09-13 | 广州泽力医药科技有限公司 | Low-temperature efficient nutrient component extraction technology |
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Application publication date: 20200508 |