CN114209059A - Acanthopanax senticosus polysaccharide calcium and preparation method and application thereof - Google Patents

Acanthopanax senticosus polysaccharide calcium and preparation method and application thereof Download PDF

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CN114209059A
CN114209059A CN202111562285.4A CN202111562285A CN114209059A CN 114209059 A CN114209059 A CN 114209059A CN 202111562285 A CN202111562285 A CN 202111562285A CN 114209059 A CN114209059 A CN 114209059A
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calcium
polysaccharide
acanthopanax
acanthopanax senticosus
precipitate
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CN114209059B (en
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张洁
韩宝翠
刘静
王小宇
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Heilongjiang Wusuli River Pharmaceutical Co ltd
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Heilongjiang Wusuli River Pharmaceutical Co ltd
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Abstract

The invention provides a calcium acanthopanax polysaccharide and a preparation method and application thereof, wherein the preparation method comprises the following steps: (1) dissolving the waste precipitate obtained by separation in the acanthopanax injection process to obtain a waste precipitate solution, then mixing the waste precipitate solution with a protein precipitator, then removing the precipitate, carrying out alcohol precipitation on the obtained supernatant, and then drying the obtained precipitate to obtain acanthopanax polysaccharide; (2) and (2) mixing and dissolving the acanthopanax senticosus polysaccharide obtained in the step (1) with a calcium salt, adjusting pH for reaction, and purifying to obtain the acanthopanax senticosus polysaccharide calcium. The acanthopanax senticosus polysaccharide calcium provided by the invention has the effects of tonifying qi and spleen, tonifying kidney and soothing nerves, can effectively enhance the immunity of organisms and improve osteoporosis, and waste precipitates separated in the acanthopanax senticosus injection process are used as raw materials, so that the cost and resources are saved, and the waste and pollution are reduced.

Description

Acanthopanax senticosus polysaccharide calcium and preparation method and application thereof
Technical Field
The invention belongs to the field of medicine preparation, particularly relates to acanthopanax senticosus polysaccharide calcium and a preparation method and application thereof, and particularly relates to acanthopanax senticosus polysaccharide calcium with low cost and good effect and a preparation method and application thereof.
Background
Acanthopanax senticosus belongs to Araliaceae, is the same family as ginseng, is mainly produced in northeast mountain areas, and is a special and precious Chinese herbal medicine in the northeast. The active ingredients mainly comprise syringin, eleutheroside E and flavonoid active substances, and the composition has the effects of tonifying qi and spleen, tonifying kidney and soothing nerves, and has certain curative effects on preventing cardiovascular and cerebrovascular diseases, spleen-kidney yang deficiency, body weakness and hypodynamia, inappetence, soreness of waist and knees, insomnia and dreaminess.
The acanthopanax polysaccharide is an immune polysaccharide from natural sources, is green, safe and nontoxic, has immunostimulation activity, can induce and enhance cellular immunity and humoral immunity of organisms, and can improve the immune response of the organisms as an immunopotentiator. However, there are some problems and disadvantages in the use of acanthopanax senticosus polysaccharide at present. Like other plant polysaccharides, acanthopanax polysaccharide also has the problems of too fast metabolism and large dosage in the organism; in addition, part of the alkali-soluble polysaccharide is not easily absorbed; in addition, only acanthopanax flavone liposome and acanthopanax saponin liposome are developed aiming at the acanthopanax preparation, but no study of acanthopanax polysaccharide calcium is carried out; the existing acanthopanax health care function has the defects of insignificant effect, complex preparation method and process and the like. In addition, the direct waste of the precipitate after the preparation of the acanthopanax injection causes pollution and serious waste.
CN108323663A discloses an acanthopanax senticosus polysaccharide health drink and a method for extracting acanthopanax senticosus polysaccharide from acanthopanax senticosus, wherein acanthopanax senticosus polysaccharide in acanthopanax senticosus is extracted by adopting a high-pressure extraction process, and further purified by adopting a polyamide resin and macroporous adsorption resin separation and purification process; the acanthopanax polysaccharide health-care beverage only contains polysaccharide components with the function of improving immunity, has high content of effective active ingredients and less impurities, avoids potential sensitization risk of non-effective ingredients in the traditional Chinese patent medicine beverage and burden and damage of complex medicinal ingredients to liver and kidney of a user, prepares a health-care beverage with more pertinence, high efficiency and low toxicity, and comprehensively enhances the immunity of the user through compatibility of medicinal polysaccharides in the health-care beverage.
CN105418785B discloses a production method and application of acanthopanax senticosus polysaccharide, and the specific method is as follows: pretreating raw materials, extracting with water, removing impurities, purifying and adsorbing with polyamide resin, mixing the lower column solution and water washing solution, concentrating, precipitating with ethanol, and freeze drying to obtain Acanthopanax senticosus polysaccharide. The polysaccharide obtained by the method has high purity, simple operation and high yield, is suitable for industrial mass production, and has obvious treatment effect on tuberculous pleurisy.
The application of acanthopanax polysaccharide still has some limitations and problems at present. Therefore, how to provide a brand-new application method of acanthopanax polysaccharide becomes a problem to be solved urgently.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the calcium acanthopanax senticosus polysaccharide and the preparation method and the application thereof, and particularly provides the calcium acanthopanax senticosus polysaccharide with low cost and good effect and the preparation method and the application thereof. The acanthopanax senticosus polysaccharide calcium provided by the invention has the effects of tonifying qi and spleen, tonifying kidney and soothing nerves, can effectively enhance the immunity of organisms and improve osteoporosis, and waste precipitates separated in the acanthopanax senticosus injection process are used as raw materials, so that the cost and resources are saved, and the waste and pollution are reduced.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a preparation method of calcium acanthopanaxgenin polysaccharide, which comprises the following steps:
(1) dissolving the waste precipitate obtained by separation in the acanthopanax injection process to obtain a waste precipitate solution, then mixing the waste precipitate solution with a protein precipitator, then removing the precipitate, carrying out alcohol precipitation on the obtained supernatant, and then drying the obtained precipitate to obtain acanthopanax polysaccharide;
(2) and (2) mixing and dissolving the acanthopanax senticosus polysaccharide obtained in the step (1) with a calcium salt, adjusting pH for reaction, and purifying to obtain the acanthopanax senticosus polysaccharide calcium.
The method takes the waste precipitate separated in the acanthopanax injection process as the raw material, thereby saving the cost and resources and reducing the waste and pollution.
The waste precipitate may exemplarily be obtained by a method comprising the steps of:
pulverizing radix Acanthopanacis Senticosi, weighing, and adding the weighed radix Acanthopanacis Senticosi into a decocting tank. Adding purified water as solvent, adding 5-7 times of purified water, soaking for 30min, decocting for 1 hr, discharging the medicinal liquid to evaporation dish, adding purified water, and continuously extracting for 4 hr. Filtering the liquid medicine and transferring the liquid medicine into a sulfur stone tank. Cooling the medicinal liquid below 50 deg.C, adjusting pH to 10-12 with 20% lime milk, stirring, standing for 30min, measuring pH again to 10-12, slowly adding 20% sulfuric acid solution into the medicinal liquid, adjusting pH to 5-6, stirring, measuring pH again to 5-6, stopping stirring, transferring the medicinal liquid into a precipitation tank, standing for more than 4 hr, collecting supernatant, and concentrating under reduced pressure. Placing the concentrated medicinal liquid into an alcohol precipitation stirring tank, cooling to 35-40 deg.C, slowly adding 92-95% ethanol water solution while stirring to make the alcohol content of the medicinal liquid reach 83-85%, stirring thoroughly, sealing, and standing for more than 12 hr. Filtering by adopting a plate frame; and 5 layers of medium filter paper are filtered until the solution is clear. The clarified liquid is used for preparing the acanthopanax injection, and the filtered waste precipitate is used for subsequent preparation.
Preferably, the protein precipitant in step (1) comprises any one or a combination of at least two of trichloroacetic acid, sulfosalicylic acid, ethanol or n-butanol.
The protein precipitant can remove protein from waste precipitate, improve the purity of Acanthopanax senticosus polysaccharide in the product, and further improve the effects of the product of calcium acanthopanax senticosus polysaccharide in enhancing immunity and improving osteoporosis.
Preferably, the protein precipitant of step (1) is a combination of trichloroacetic acid, sulfosalicylic acid and ethanol.
The specific protein precipitator is selected by compounding trichloroacetic acid, sulfosalicylic acid and ethanol, so that the effect of removing protein is further improved, and the effects of enhancing the immunity of the organism and improving the osteoporosis of the product of the calcium acanthopanax senticosus polysaccharide are improved.
Preferably, the mass ratio of the protein precipitant in the step (1) to the waste precipitate solution is 2 (9-11);
preferably, the concentration of the waste precipitate solution is 0.1-0.15 g/mL. .
Preferably, the reagent added in the alcohol precipitation in the step (1) is ethanol water solution, and the volume fraction of the ethanol water solution is 90-95%;
preferably, the final concentration of ethanol in the supernatant of step (1) is 70-75%.
Preferably, the temperature of the alcohol precipitation in the step (1) is 0-6 ℃, and the time is 24-36 h.
Preferably, the number of alcohol precipitations in step (1) is at least 2.
Wherein, the mass ratio of the protein precipitator to the waste precipitate solution can be 2:9, 2:9.5, 2:10, 2:10.5 or 2:11, etc., the concentration of the waste precipitate solution can be 0.1g/mL, 0.11g/mL, 0.12g/mL, 0.13g/mL, 0.14g/mL or 0.15g/mL, etc., the volume fraction of the ethanol water solution can be 90%, 91%, 92%, 93%, 94% or 95%, etc., the final concentration of the ethanol in the supernatant can be 70%, 71%, 72%, 73%, 74% or 75%, etc., the temperature of the ethanol precipitation can be 0 ℃, 1 ℃, 2 ℃, 3 ℃, 4 ℃, 5 ℃ or 6 ℃, etc., the time can be 24h, 25h, 26h, 27h, 28h, 29h, 30h, 31h, 32h, 33h, 34h, 35h or 36h, etc., the times of the ethanol precipitation can be 2, 3 or 4, etc., but not limited to, the above-listed numerical values, and other numerical values not listed in the above numerical range are also applicable.
The alcohol precipitation reagent and the parameters thereof can effectively extract the acanthopanax senticosus polysaccharide in the waste precipitate, improve the yield of the acanthopanax senticosus polysaccharide, improve the content of the acanthopanax senticosus polysaccharide calcium in the product, and further improve the effects of the acanthopanax senticosus polysaccharide calcium in enhancing the immunity of the organism and improving the osteoporosis.
Preferably, the calcium salt of step (2) comprises calcium chloride and/or calcium hydroxide.
Preferably, the mass ratio of the acanthopanax senticosus polysaccharide to the calcium salt in the step (2) is 5 (0.8-1.2).
Preferably, the pH is adjusted to pH 7-11 in step (2).
Preferably, the reaction time of step (2) is 0.5-2 h.
Wherein, the mass ratio of the acanthopanax senticosus polysaccharide to the calcium salt can be 5:0.8, 5:0.9, 5:1, 5:1.1 or 5:1.2, the pH is adjusted to be 7, 8, 9, 10 or 11, the reaction time can be 0.5h, 0.6h, 0.7h, 0.8h, 0.9h, 1h, 1.1h, 1.2h, 1.3h, 1.4h, 1.5h, 1.6h, 1.7h, 1.8h, 1.9h or 2h, but not limited to the above-mentioned values, and other values not listed in the above-mentioned value range are also applicable.
In a second aspect, the invention provides calcium acanthopanaxgenin prepared by the preparation method of calcium acanthopanaxgenin as described above.
In a third aspect, the invention also provides the application of the acanthopanax polysaccharide calcium in preparing health care products or medicines.
Preferably, the health product and the medicine independently comprise any one of oral liquid, tablets, capsules or granules.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a acanthopanax senticosus polysaccharide calcium, which takes waste precipitate obtained by separation in an acanthopanax senticosus injection process as a raw material, thereby saving cost and resources and reducing waste and pollution; the protein precipitator can remove protein in the waste precipitate, improve the purity of acanthopanax polysaccharide in the product, and further improve the effects of the product of the acanthopanax polysaccharide calcium spike for enhancing the immunity of the organism and improving the osteoporosis; the acanthopanax senticosus polysaccharide in the waste precipitate can be effectively extracted by adopting a specific alcohol precipitation reagent and parameters thereof, so that the yield of the acanthopanax senticosus polysaccharide is increased, the content of the acanthopanax senticosus polysaccharide calcium in the product is increased, and the effects of the acanthopanax senticosus polysaccharide calcium in the product of enhancing the immunity of the organism and improving the osteoporosis are further improved.
Detailed Description
To further illustrate the technical means and effects of the present invention, the following further describes the technical solution of the present invention with reference to the preferred embodiments of the present invention, but the present invention is not limited to the scope of the embodiments.
The preparation method of the waste precipitate separated in the acanthopanax injection process used in the following examples is as follows: pulverizing radix Acanthopanacis Senticosi, weighing, and adding the weighed radix Acanthopanacis Senticosi into a decocting tank. Adding purified water as solvent, adding purified water 6 times of the raw materials, soaking for 30min, decocting for 1 hr, discharging the medicinal liquid to evaporation dish, adding purified water, and continuously extracting for 4 hr. Filtering the liquid medicine and transferring the liquid medicine into a sulfur stone tank. When the temperature of the liquid medicine is reduced to below 50 ℃, adjusting the pH value to 11 by using lime milk with the mass fraction of 20%, fully stirring, standing for 30min, measuring the pH value again to be between 10 and 12, slowly adding sulfuric acid solution with the mass fraction of 20% into the liquid medicine, adjusting the pH value to 5, fully stirring, stopping stirring when measuring the pH value again to be between 5 and 6, transferring the liquid medicine into a settling tank, standing for 5h, extracting supernatant, and performing a pressure reduction concentration process. Putting the concentrated liquid medicine into an alcohol precipitation stirring tank, cooling to 35-40 deg.C, slowly adding 95% ethanol water solution, stirring while adding until the ethanol content of the liquid medicine reaches 85%, stirring thoroughly, sealing, and standing for 13 hr. Filtering by adopting a plate frame; and 5 layers of medium filter paper are filtered until the solution is clear. The clarified liquid is used for preparing the acanthopanax injection, and the filtered waste precipitate is used for subsequent preparation.
Example 1
The embodiment provides a acanthopanax senticosus polysaccharide calcium, and the preparation method comprises the following steps:
selecting waste precipitate separated in the acanthopanax injection process, adding water, stirring until the waste precipitate is dissolved to obtain a waste precipitate solution, then adding a trichloroacetic acid, sulfosalicylic acid and ethanol mixed solution (the mass ratio of the waste precipitate solution (0.125g/mL), trichloroacetic acid, sulfosalicylic acid and ethanol is 100:5:5:10) into the obtained solution while stirring, precipitating, removing protein in the solution by precipitation, centrifuging, and removing the precipitate to obtain a supernatant. Adding 92% ethanol solution into the supernatant until the alcoholic strength of the supernatant is 72%, refrigerating at 4 deg.C for 30h, repeating twice, vacuum filtering to obtain precipitate, and drying to obtain Acanthopanax senticosus polysaccharide;
dissolving acanthopanax senticosus polysaccharide with water, adding calcium chloride (the mass ratio of acanthopanax senticosus polysaccharide to calcium chloride is 5:1), mixing, adding sodium hydroxide to adjust the pH value to 9, reacting for 1.2h, purifying, filtering and drying to obtain the acanthopanax senticosus polysaccharide calcium.
Example 2
The embodiment provides a acanthopanax senticosus polysaccharide calcium, and the preparation method comprises the following steps:
selecting waste precipitate separated in the acanthopanax injection process, adding water, stirring until the waste precipitate is dissolved to obtain a waste precipitate solution, adding trichloroacetic acid (the mass ratio of the waste precipitate solution (0.1g/mL) to trichloroacetic acid is 20:3) into the obtained solution while stirring to generate precipitate, removing protein in the solution by precipitation, centrifuging, and removing the precipitate to obtain a supernatant. Adding 90% ethanol solution into the supernatant until the alcohol content of the supernatant is 70%, refrigerating at 0 deg.C for 24 hr, repeating twice, vacuum filtering to obtain precipitate, and drying to obtain Acanthopanax senticosus polysaccharide;
dissolving acanthopanax senticosus polysaccharide with water, adding calcium hydroxide (the mass ratio of acanthopanax senticosus polysaccharide to calcium hydroxide is 5:0.8), mixing, adding sodium hydroxide to adjust the pH value to 7, reacting for 2 hours, purifying, filtering and drying to obtain the acanthopanax senticosus polysaccharide calcium.
Example 3
The embodiment provides a acanthopanax senticosus polysaccharide calcium, and the preparation method comprises the following steps:
selecting waste precipitate separated in the acanthopanax injection process, adding water, stirring until the waste precipitate is dissolved to obtain a waste precipitate solution, adding ethanol (the mass ratio of the waste precipitate solution (0.15g/mL) to the ethanol is 4:1) into the obtained solution while stirring to generate precipitate, removing protein in the solution by precipitation, centrifuging, and removing the precipitate to obtain a supernatant. Adding 95 vol% ethanol solution into the supernatant until the alcohol content of the supernatant is 75%, cold preserving at 6 deg.C for 36h, repeating for three times, vacuum filtering to obtain precipitate, and drying to obtain Acanthopanax senticosus polysaccharide;
dissolving Acanthopanax senticosus polysaccharide with water, adding calcium chloride (the mass ratio of the Acanthopanax senticosus polysaccharide to the calcium chloride is 5:1.2), mixing, adding sodium hydroxide to adjust the pH value to 11, reacting for 0.5h, purifying, filtering and drying to obtain the calcium acanthopanax senticosus polysaccharide.
Example 4
This example provides a calcium acanthopanaxgenin polysaccharide, prepared according to example 1 except that it does not contain trichloroacetic acid, and the reduced fraction is apportioned to ethanol and sulfosalicylic acid.
Example 5
This example provides a calcium acanthopanaxgenin polysaccharide, prepared according to example 1 except that it does not contain ethanol, and the reduced fraction is apportioned to trichloroacetic acid and sulfosalicylic acid.
Example 6
This example provides a calcium acanthopanaxgenin polysaccharide, prepared according to example 1 except that it does not contain sulfosalicylic acid, and a reduced portion is apportioned to ethanol and trichloroacetic acid.
Example 7
This example provides a calcium acanthopanaxgenin polysaccharide, which is the same as example 1 except that it does not contain trichloroacetic acid and sulfosalicylic acid, and a reduced portion of it is distributed to ethanol.
Example 8
This example provides a calcium acanthopanaxgenin polysaccharide, which is the same as example 1 except that it does not contain ethanol and sulfosalicylic acid, and a reduced portion of it is distributed to trichloroacetic acid.
Example 9
This example provides a calcium acanthopanaxgenin polysaccharide, which is identical to example 1 except that it does not contain ethanol and trichloroacetic acid, and a reduced proportion is apportioned to sulfosalicylic acid.
Example 10
This example provides a calcium acanthopanaxgenin polysaccharide prepared according to the method of example 1 except that the ethanol is replaced by an equal amount of n-butanol.
Example 11
This example provides a calcium acanthopanax senticosus polysaccharide, which is prepared in a manner consistent with example 1, except that the alcoholic strength of the supernatant is 70%.
Example 12
This example provides a calcium acanthopanax senticosus polysaccharide, which is prepared in a manner consistent with example 1, except that the alcoholic strength of the supernatant is 75%.
Example 13
This example provides a calcium acanthopanax senticosus polysaccharide, which is prepared in a manner consistent with example 1, except that the alcoholic strength of the supernatant is 65%.
Example 14
This example provides a calcium acanthopanax senticosus polysaccharide, which is prepared in a manner similar to that of example 1, except that the alcoholic strength of the supernatant is 80%.
Effect verification:
the yields and calcium contents of the calcium acanthopanaxgenin provided in examples 1-14 were measured and calculated as follows:
group of Yield (%) Calcium content (%) Group of Yield (%) Calcium content (%)
Example 1 55.3 14.48 Example 8 43.2 10.35
Example 2 43.3 9.2 Example 9 38.9 7.26
Example 3 36.3 6.64 Example 10 34.8 6.2
Example 4 46.5 11.63 Example 11 49.8 13.56
Example 5 44.8 11.24 Example 12 49.4 12.73
Example 6 37.8 7.05 Examples13 40.7 8.24
Example 7 35.7 6.92 Example 14 41.9 8.91
The results show that the acanthopanax senticosus polysaccharide calcium obtained by the method is high in yield and high in calcium content, and further reflect that the obtained product acanthopanax senticosus polysaccharide calcium is high in purity; comparing example 1 with examples 4-10, it can be found that the invention further improves the effect of removing protein from waste sediment and improves the yield and calcium content of the product compared with other protein precipitants by selecting the compounding of ethanol, trichloroacetic acid and sulfosalicylic acid; comparing example 1 with examples 11-14, the invention can find that acanthopanax polysaccharide in the waste sediment after protein removal can be further extracted by controlling the concentration of alcohol during alcohol precipitation, thereby improving the yield and calcium content of the product.
And (3) immune function verification:
170 Kunming mice are selected, the weight of the Kunming mice is 20-22g, the Kunming mice are randomly divided into 17 groups, 10 mice are selected in each group, the male and female mice are half-and-half injected with the aqueous solution of the calcium acanthopanax pentosaceus provided by the example 1-14 (100mg/kg), the cyclophosphamide (100mg/kg), the mixed aqueous solution of the calcium acanthopanax pentosaceus provided by the example 1 and the cyclophosphamide (100mg/kg of the injection amount respectively, the test group) and the physiological saline with the same amount (blank control), and the injection is performed with intraperitoneal injection for 1 time every day and the administration is continuously performed for 5 days. 24 hours after the last administration, the mice were sacrificed by cervical dislocation and weighed. Taking partial tissues of the spleen and the lymph tissue respectively, precisely weighing the partial tissues to prepare cell suspensions, counting under a microscope and converting into the total number of cells of each organ, and calculating an average value, wherein the result is as follows:
Figure BDA0003420679180000101
the data show that the acanthopanax senticosus polysaccharide calcium provided by the invention can effectively promote the increase of spleen and lymphoid tissue cells and improve the immunity of an organism; comparing the embodiment 1 with the embodiments 4-10, the invention can find that the effect of removing protein from waste sediment is further improved by selecting the compounding of the ethanol, the trichloroacetic acid and the sulfosalicylic acid compared with other protein precipitants, the purity and the yield of the product are improved, and the capability of improving the immunity of the organism is further improved; comparing the example 1 with the examples 11 to 14, the invention can find that the acanthopanax polysaccharide in the waste sediment after protein removal can be further extracted by controlling the concentration of alcohol during alcohol precipitation, so that the yield and purity of the product are improved, and the capability of improving the immunity of the organism is further improved; comparing example 1, the cyclophosphamide group, the blank control group and the test group, it can be found that cyclophosphamide can effectively inhibit the immunocompetence of a mouse, and when cyclophosphamide is mixed with the acanthopanax senticosus polysaccharide calcium provided by the invention, the immunocompetence of the mouse can be improved to a level equivalent to a normal condition, so that the effect that the acanthopanax senticosus polysaccharide calcium provided by the preparation method can effectively improve the immunity of an organism is fully demonstrated.
Functional verification for improving bone mineral density:
160 rats with the weight equivalent to that of Wister are selected, the rats are fed with retinoic acid 70mg/kg intragastrically once a day for 4 weeks, a rat osteoporosis model is established, the rats are randomly divided into 16 groups, 10 rats are fed into each group, the rats are half-and-half in sex, the rats in each group are subjected to intragastrically gavage (150 mg each time) by respectively adopting physiological saline and a commercially available calcium tablet, the rats are weighed once a day and once a week and fed for 12 weeks continuously, 24 hours after the last administration, the rats are anesthetized by intraperitoneal injection of 4% sodium pentobarbital (40mg/kg), the rats are killed by X-ray, the thighs of the rats are dissected, the bone density is measured on a bone densitometer, and the results are as follows:
Figure BDA0003420679180000111
the results show that the acanthopanax senticosus polysaccharide calcium provided by the invention can effectively improve the symptoms of osteoporosis; comparing the embodiment 1 with the embodiments 4 to 10, the invention can find that the effect of removing protein from waste sediment is further improved by selecting the compounding of the ethanol, the trichloroacetic acid and the sulfosalicylic acid compared with other protein precipitants, the purity and the yield of the product are improved, the calcium content of a unit product is further improved, and the treatment effect on osteoporosis is improved; comparing example 1 with examples 11-14, the invention can find that acanthopanax polysaccharide in the waste sediment after protein removal can be further extracted by controlling the concentration of alcohol in alcohol precipitation, so that the yield and purity of the product are improved, the calcium content of a unit product is further improved, and the treatment effect on osteoporosis is improved.
The applicant states that the invention is illustrated by the above examples to the calcium acanthopanaxgenin and the preparation method and application thereof, but the invention is not limited to the above examples, i.e. it is not meant that the invention must be implemented by the above examples. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.

Claims (10)

1. The preparation method of the acanthopanax senticosus polysaccharide calcium is characterized by comprising the following steps:
(1) dissolving the waste precipitate obtained by separation in the acanthopanax injection process to obtain a waste precipitate solution, then mixing the waste precipitate solution with a protein precipitator, then removing the precipitate, carrying out alcohol precipitation on the obtained supernatant, and then drying the obtained precipitate to obtain acanthopanax polysaccharide;
(2) and (2) mixing and dissolving the acanthopanax senticosus polysaccharide obtained in the step (1) with a calcium salt, adjusting pH for reaction, and purifying to obtain the acanthopanax senticosus polysaccharide calcium.
2. The method for preparing calcium spindt-plus polysaccharide according to claim 1, wherein the protein precipitant in step (1) comprises one or a combination of at least two of trichloroacetic acid, sulfosalicylic acid, ethanol or n-butanol.
3. The method for preparing calcium spindt-plus-polysaccharide according to claim 2, wherein the protein precipitant in step (1) is a combination of trichloroacetic acid, sulfosalicylic acid and ethanol.
4. The method for preparing calcium acanthopanax senticosus polysaccharide according to any one of claims 1-3, wherein the mass ratio of the protein precipitating agent to the waste precipitate solution in the step (1) is 2 (9-11);
preferably, the concentration of the waste precipitate solution is 0.1-0.15 g/mL.
5. The preparation method of calcium acanthopanax senticosus polysaccharide according to any one of claims 1-4, wherein a reagent added in the alcohol precipitation in the step (1) is an aqueous ethanol solution, and the volume fraction of the aqueous ethanol solution is 90-95%;
preferably, the final concentration of ethanol in the supernatant of step (1) is 70-75%.
6. The preparation method of calcium acanthopanax senticosus according to any one of claims 1-5, wherein the temperature of the alcohol precipitation in the step (1) is 0-6 ℃, and the time is 24-36 h.
7. The method for preparing calcium acanthopanax senticosus according to any one of claims 1-6, wherein the number of alcohol precipitations in step (1) is at least 2.
8. The method for preparing calcium acanthopanaxgenin according to any one of claims 1-6, wherein the calcium salt of step (2) comprises calcium chloride and/or calcium hydroxide;
preferably, the mass ratio of the acanthopanax senticosus polysaccharide to the calcium salt in the step (2) is 5 (0.8-1.2);
preferably, the pH is adjusted to pH 7-11 in step (2);
preferably, the reaction time of step (2) is 0.5-2 h.
9. A calcium acanthopanax elatus prepared according to the method for preparing calcium acanthopanax elatus according to any one of claims 1-8.
10. The use of the calcium acanthopanax senticosus polysaccharide according to claim 9 in the preparation of health products or medicines;
preferably, the health product and the medicine independently comprise any one of oral liquid, tablets, capsules or granules.
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CN105418785A (en) * 2015-12-25 2016-03-23 长春市传染病医院 Production method and application of eleutherococcus senticosus polysaccharide
CN106977596A (en) * 2017-05-22 2017-07-25 南宁学院 A kind of method for extracting bovine serum albumin
CN110183550A (en) * 2019-06-25 2019-08-30 广元市海天实业有限责任公司 A kind of preparation process of refined heparin sodium

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101084953A (en) * 2007-06-20 2007-12-12 黑龙江省珍宝岛制药有限公司 Method for preparing acanthopanax senticousus extracting liquid/extraction
CN104774277A (en) * 2015-03-26 2015-07-15 广东省农业科学院蚕业与农产品加工研究所 Flammulina velutipes polysaccharide chelated trace element calcium preparation method
CN105418785A (en) * 2015-12-25 2016-03-23 长春市传染病医院 Production method and application of eleutherococcus senticosus polysaccharide
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