CN112353832B - A method for separating active components from radix Adenophorae - Google Patents
A method for separating active components from radix Adenophorae Download PDFInfo
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Abstract
The invention relates to the technical field of separation and extraction of active components in medicinal materials, in particular to a method for separating active components from adenophora stricta. The invention provides a method for extracting and separating effective components such as polysaccharide, saponin and beta-sitosterol from adenophora stricta with low cost, high efficiency and no pollution as principles. The experimental result shows that the polysaccharide content in the crude product of the adenophora stricta polysaccharide obtained by the invention exceeds 80 wt%, and the yield is higher than 85%; the content of saponin in the finished product of adenophora stricta saponin exceeds 76 wt% and the yield is higher than 91% determined by high performance liquid chromatography; the content of beta-sitosterol in the adenophora stricta beta-sitosterol crystal exceeds 91 wt%, and the yield is higher than 89%.
Description
Technical Field
The invention relates to the technical field of separation and extraction of active components in medicinal materials, in particular to a method for separating active components from adenophora stricta.
Background
The Adenophora stricta Miq (Adenophora stricta Miq.) of Campanulaceae or Adenophora tetraphylla thumb (Fisch) is a perennial herb, and is prepared by mixing root with herbs, digging in spring and autumn, removing fibrous root and coarse skin, and sun drying. Other names are radix Adenophorae, radix Adenophorae Strictae, orchid, radix Platycodi, etc. Sha Shen is sweet and slightly bitter in taste. Modern researches show that the adenophora stricta has rich chemical components and medicinal values, contains various chemical components such as beta-sitosterol, beta-sitosterol-beta-D-glucopyranoside, taraxacil, docosanoic acid, adenophora stricta polysaccharide, saponin and the like, and has the pharmacological effects of nourishing yin, clearing heat, moistening lung, reducing phlegm, benefiting stomach, promoting the secretion of saliva or body fluid and the like. The traditional Chinese medicine is usually used for treating lung heat dry cough, yin deficiency over-strained cough, dry cough with sticky phlegm, stomach yin deficiency, anorexia and vomiting, qi yin deficiency, dysphoria with smothery sensation and dry mouth and the like. The polysaccharide and the beta-sitosterol chemical components have the functions of improving immunity, eliminating free radicals of a human body, resisting aging and radiation, and have good protection effect on the liver.
CN107029004A discloses a preparation method of adenophora tetraphylla saponin, which comprises the steps of chopping adenophora tetraphylla, extracting by ethanol through hot reflux, then concentrating under reduced pressure, adding water for dilution, then loading on treated macroporous adsorption resin, and then resolving by high ethanol to obtain the saponin compound.
CN110499214A discloses an extraction method of adenophora tetraphylla volatile oil, which comprises the following steps: ultrasonically extracting with ethanol, concentrating under reduced pressure, loading onto macroporous adsorbent resin, eluting with chloroform, and collecting eluate to obtain volatile oil components of radix Adenophorae.
The adenophora stricta chemical components obtained by using ethanol as an extraction solvent in the invention are saponin and volatile oil components, so that the extraction cost is high, chloroform is toxic, and the adenophora stricta chemical components are harmful to human bodies and environment.
Therefore, there is a need to develop a method for comprehensively and efficiently utilizing the active ingredients of the raw material of adenophora stricta, which can simultaneously extract and separate a plurality of active ingredients of adenophora stricta efficiently and at low cost. And the final product has high purity, stable quality and no pollution to the environment.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a method for separating active ingredients from adenophora stricta, wherein the yield and purity of the separated active ingredients are high.
The invention provides a method for separating active ingredients from adenophora stricta, which comprises the following steps:
mixing the adenophora stricta powder with water, carrying out first heating extraction, and centrifuging and carrying out first reduced pressure concentration on an aqueous extract obtained after the first heating extraction;
passing the concentrated solution after the first reduced pressure concentration through macroporous adsorbent resin, washing with water, collecting effluent liquid from column loading and effluent liquid from washing with water, mixing to obtain total effluent liquid, and precipitating the total effluent liquid with ethanol to obtain polysaccharide compound;
resolving the treated macroporous adsorption resin with an ethanol aqueous solution to obtain a resolving solution;
carrying out second reduced pressure concentration on the analysis solution, and adding water for dilution to obtain a diluted solution;
passing the diluent through an anion exchange resin and a cation exchange resin which are connected in series, and carrying out third reduced pressure concentration and drying on the effluent liquid of the cation exchange resin to obtain a saponin compound crude product;
mixing the extraction residue after the first heating extraction with ethanol, performing second heating extraction, and performing fourth reduced pressure concentration on the water extract after the second heating extraction;
and drying the concentrated solution after the fourth reduced pressure concentration to obtain a crude extract, heating and dissolving the crude extract and an organic solvent, cooling and crystallizing, and performing suction filtration to obtain the beta-sitosterol.
Preferably, the particle size of the adenophora stricta powder is not more than 40 meshes.
Preferably, the volume ratio of the adenophora stricta powder to water subjected to the first heating extraction is 1: 10-40;
the temperature of the first heating extraction is 70-90 ℃;
the heating extraction times of the first heating extraction are 3 times, and the extraction time is 1-3 h each time.
Preferably, the rotation speed of the water extract subjected to the first heating extraction is 4000r/min, and the centrifugation time is 4-6 min;
the pressure of the first reduced pressure concentration is 0.08-0.1 MPa, and the temperature of the first reduced pressure concentration is 70-80 ℃.
Preferably, the macroporous adsorption resin is selected from one of D101, AB-8 and LSA-10;
the dosage ratio of the macroporous adsorption resin to the radix adenophorae powder is 1-3L: 1 kg;
the height-diameter ratio of the macroporous adsorption resin is 5-7: 1;
the flow rate of the macroporous adsorption resin on the column is 1-1.5 bv/h;
the reagent adopted by alcohol precipitation is an aqueous solution of ethanol with the mass concentration of 80-90%.
Preferably, the mass concentration of the ethanol aqueous solution adopted by the macroporous adsorption resin after the analysis treatment is 60-75%;
the volume of an ethanol aqueous solution adopted by the macroporous adsorption resin after the analysis treatment is 2-3 BV;
the flow rate of the ethanol water solution adopted by the macroporous adsorption resin after the analysis treatment is 1-1.5 bv/h.
Preferably, the pressure of the second reduced pressure concentration is 0.08-0.1 MPa, and the temperature of the second reduced pressure concentration is 60-65 ℃;
the anion exchange resin is selected from one of D941, D354 and D351; the height-diameter ratio of the anion exchange resin is 4-6: 1, the flow rate of the upper column is 1-2 bv/h;
the cation exchange resin is selected from one of D370, 732 and SDB-3; the height-diameter ratio of the cation exchange resin is 4-6: 1, the flow rate of the upper column is 1-2 bv/h.
Preferably, the pressure of the third reduced pressure concentration is 0.08-0.1 MPa, and the temperature of the third reduced pressure concentration is 50-80 ℃.
Preferably, the mass concentration of the ethanol mixed with the extraction residue after the first heating extraction is 70-95%;
the temperature of the second heating extraction is 70-85 ℃;
the heating extraction times of the second heating extraction are 3 times, and the extraction time of each time is 1.5-2.5 h;
the pressure of the fourth decompression concentration is 0.08-0.1 MPa, and the temperature of the fourth decompression concentration is 50-70 ℃.
Preferably, the drying temperature of the concentrated solution after the fourth reduced pressure concentration is 50-70 ℃;
the organic solvent is selected from methanol, absolute ethyl alcohol or ethyl acetate;
the mass volume ratio of the crude extract to the organic solvent is 1 kg: 10-20L;
the heating and dissolving temperature is 50-60 ℃;
the cooling crystallization temperature is 4-10 ℃, and the cooling crystallization time is 24-48 h.
The invention provides a method for separating active ingredients from adenophora stricta, which comprises the following steps: mixing the adenophora stricta powder with water, carrying out first heating extraction, and centrifuging and carrying out first reduced pressure concentration on an aqueous extract obtained after the first heating extraction; passing the concentrated solution after the first reduced pressure concentration through macroporous adsorbent resin, washing with water, collecting effluent liquid from column loading and effluent liquid from washing with water, mixing to obtain total effluent liquid, and precipitating the total effluent liquid with ethanol to obtain polysaccharide compound; resolving the treated macroporous adsorption resin with an ethanol aqueous solution to obtain a resolving solution; carrying out second reduced pressure concentration on the analysis solution, and adding water for dilution to obtain a diluted solution; passing the diluent through an anion exchange resin and a cation exchange resin which are connected in series, and carrying out third reduced pressure concentration and drying on the effluent liquid of the cation exchange resin to obtain a saponin compound crude product; mixing the extraction residue after the first heating extraction with ethanol, performing second heating extraction, and performing fourth reduced pressure concentration on the water extract after the second heating extraction; and drying the concentrated solution after the fourth reduced pressure concentration to obtain a crude extract, heating and dissolving the crude extract and an organic solvent, cooling and crystallizing, and performing suction filtration to obtain the beta-sitosterol. The invention provides the method for extracting and separating the effective components in the adenophora stricta, such as polysaccharide, saponin and beta-sitosterol, with low cost, high efficiency and no pollution as the principle, and the obtained effective components have high content and strong process operability, thereby being suitable for industrial production.
The experimental result shows that the polysaccharide content in the crude product of the adenophora stricta polysaccharide obtained by the invention exceeds 80 wt%, and the yield is higher than 85%; the content of saponin in the finished product of adenophora stricta saponin exceeds 76 wt% and the yield is higher than 91% determined by high performance liquid chromatography; the content of beta-sitosterol in the adenophora stricta beta-sitosterol crystal exceeds 91 wt%, and the yield is higher than 89%.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a method for separating active ingredients from adenophora stricta, which comprises the following steps:
mixing the adenophora stricta powder with water, carrying out first heating extraction, and centrifuging and carrying out first reduced pressure concentration on an aqueous extract obtained after the first heating extraction;
passing the concentrated solution after the first reduced pressure concentration through macroporous adsorbent resin, washing with water, collecting effluent liquid from column loading and effluent liquid from washing with water, mixing to obtain total effluent liquid, and precipitating the total effluent liquid with ethanol to obtain polysaccharide compound;
resolving the treated macroporous adsorption resin with an ethanol aqueous solution to obtain a resolving solution;
carrying out second reduced pressure concentration on the analysis solution, and adding water for dilution to obtain a diluted solution;
passing the diluent through an anion exchange resin and a cation exchange resin which are connected in series, and carrying out third reduced pressure concentration and drying on the effluent liquid of the cation exchange resin to obtain a saponin compound crude product;
mixing the extraction residue after the first heating extraction with ethanol, performing second heating extraction, and performing fourth reduced pressure concentration on the water extract after the second heating extraction;
and drying the concentrated solution after the fourth reduced pressure concentration to obtain a crude extract, heating and dissolving the crude extract and an organic solvent, cooling and crystallizing, and performing suction filtration to obtain the beta-sitosterol.
The method comprises the steps of mixing the adenophora stricta powder with water, carrying out first heating extraction, and carrying out centrifugation and first reduced pressure concentration on the water extract obtained after the first heating extraction.
In certain embodiments of the present invention, the particle size of the adenophora stricta powder is not greater than 40 mesh.
In some embodiments of the present invention, the adenophora stricta powder can be prepared by cutting and pulverizing adenophora stricta, and then sieving with a 40-mesh sieve.
In certain embodiments of the present invention, the first heat extraction is performed with a ratio of the adenophora stricta powder to water of 1: 10 to 40. In certain embodiments, the first heat extraction is performed with a ratio of the adenophora stricta powder to water of 1: 40. 1: 25 or 1: 20.
in certain embodiments of the present invention, the temperature of the first heating extraction is 70 to 90 ℃. In certain embodiments of the invention, the temperature of the first heated extraction is 90 ℃, 80 ℃ or 85 ℃.
In some embodiments of the present invention, the number of times of the first heating extraction is 3, and the time of each extraction is 1-3 h.
In some embodiments of the present invention, mixing the adenophora stricta powder with water, and performing the first heating extraction specifically comprises:
mixing radix Adenophorae powder and water according to the ratio of 1: 15. 1: 13. 1: 12, adding water for extraction, and extracting for 3 times at 90 ℃ for 2h each time;
or mixing radix Adenophorae powder and water according to the ratio of 1: 10. 1: 8. 1: 7, adding water to extract for 3 times at 80 ℃, wherein the extraction time is 3 hours each time;
or mixing radix Adenophorae powder and water according to the ratio of 1: 10,1: 5,1: 5, adding water to extract, extracting for 3 times at 85 ℃, wherein the extraction time is 1.5h each time.
In certain embodiments of the present invention, after the first heating extraction, further comprising filtering. The method of filtration is not particularly limited in the present invention, and a filtration method known to those skilled in the art may be used. Filtering to obtain water extract after the first heating extraction and extraction residue after the first heating extraction.
In the present invention, the centrifugation of the aqueous extract after the first heat extraction is the first centrifugation.
In some embodiments of the invention, the rotation speed of the centrifugation of the water extract after the first heating extraction is 4000r/min, and the centrifugation time is 4-6 min. In certain embodiments of the invention, the centrifugation is performed in a horizontal decanter centrifuge with a separation factor of 3500.
In certain embodiments of the present invention, after the centrifuging, further comprising: and (5) suction filtration. The method of suction filtration is not particularly limited in the present invention, and a method of suction filtration known to those skilled in the art may be used. In the present invention, the suction filtration after centrifugation is the first suction filtration.
In some embodiments of the present invention, the pressure of the first vacuum concentration is 0.08 to 0.1MPa, and the temperature of the first vacuum concentration is 70 to 80 ℃. In certain embodiments, the pressure of the first reduced pressure concentration is 0.08MPa or 0.1 MPa. In certain embodiments, the temperature of the first reduced pressure concentration is 70 ℃.
In certain embodiments of the invention, the soluble solids content of the first reduced pressure concentrated solution is 4% brix.
And after the first reduced pressure concentration is finished, passing the concentrated solution after the first reduced pressure concentration through macroporous adsorption resin, washing with water, collecting effluent liquid of the upper column and effluent liquid of the washing with water, combining to obtain total effluent liquid, and carrying out alcohol precipitation on the total effluent liquid to obtain the polysaccharide compound.
In some embodiments of the invention, the dosage ratio of the macroporous adsorption resin to the adenophora stricta powder is 1-3L: 1 kg. In certain embodiments, the amount ratio of the macroporous adsorbent resin to the adenophora stricta powder is 1.4L: 1kg, 1.625L: 1kg or 1.67L: 1 kg.
In certain embodiments of the invention, the macroporous adsorbent resin is selected from one of D101, AB-8, and LSA-1. In certain embodiments of the present invention, the macroporous adsorbent resin has a height to diameter ratio of 5 to 7: 1. in certain embodiments, the macroporous adsorbent resin has a height to diameter ratio of 6: 1. in certain embodiments of the present invention, the flow rate of the macroporous adsorbent resin on the column is 1-1.5 bv/h. In certain embodiments, the macroporous adsorbent resin has an upper column flow rate of 1.5 bv/h.
In some embodiments of the present invention, the alcohol precipitation reagent is an aqueous solution of ethanol with a mass concentration of 80% to 90%. In certain embodiments, the aqueous solution of ethanol has a mass concentration of 90%, 85%, or 80%.
In some embodiments of the present invention, after the alcohol precipitation, the method further comprises: standing overnight, centrifuging and suction filtering. Standing overnight resulted in a large amount of precipitate.
In the present invention, the centrifugation after standing overnight is the second centrifugation. The method and parameters of the centrifugation are not particularly limited in the present invention, and the method and parameters of the centrifugation known to those skilled in the art can be used.
The method of suction filtration is not particularly limited in the present invention, and a method of suction filtration known to those skilled in the art may be used. In the present invention, the suction filtration performed after the second centrifugation is a second suction filtration.
In some embodiments of the present invention, after the second suction filtration, the method further comprises: proteins were removed by extraction using the Savag method.
In certain embodiments of the invention, after the second suction filtration, drying is included prior to the removal of the protein by extraction using the Savag method. The method of drying is not particularly limited in the present invention, and a drying method known to those skilled in the art may be used. In the present invention, the drying here is the first drying.
The method for removing proteins by extraction using the Savag method is not particularly limited in the present invention, and a method for removing proteins by extraction using the Savag method known to those skilled in the art may be used.
The invention adopts macroporous adsorption resin to separate and purify saponin compounds, the macroporous adsorption resin is lyophilic to saponin components and is hydrophobic to polysaccharide and protein compounds, and the polysaccharide and protein compounds are easier to wash off. Adding 80-90% ethanol water solution, and precipitating saccharide compounds with high concentration ethanol. The polysaccharides and proteins are separated by precipitation under high concentration of ethanol. The proteins were then removed by extraction using the Savag method.
And (5) resolving the treated macroporous adsorption resin by using an ethanol aqueous solution to obtain a resolving solution. The treated macroporous adsorption resin refers to macroporous adsorption resin for treating concentrated solution after first reduced pressure concentration.
In some embodiments of the present invention, the mass concentration of the ethanol aqueous solution used for the macroporous adsorption resin after the desorption treatment is 60-75%. In certain embodiments, the macroporous adsorbent resin after desorption treatment employs an aqueous solution of ethanol at a mass concentration of 70%, 65%, or 75%. In some embodiments of the invention, the volume of the ethanol aqueous solution adopted by the macroporous adsorption resin after the desorption treatment is 2-3 BV. In certain embodiments, the macroporous adsorbent resin after desorption treatment employs a volume of an aqueous solution of ethanol of 2.5BV, 3BV, or 2 BV. In some embodiments of the invention, the flow rate of the ethanol aqueous solution adopted by the macroporous adsorption resin after the desorption treatment is 1-1.5 bv/h. In certain embodiments, the flow rate of the aqueous ethanol solution used for the desorption-treated macroporous adsorbent resin is 1.5 bv/h.
And carrying out second reduced pressure concentration on the analysis solution, and adding water for dilution to obtain a diluted solution.
In some embodiments of the present invention, the pressure of the second vacuum concentration is 0.08 to 0.1MPa, and the temperature of the second vacuum concentration is 60 to 65 ℃. In certain embodiments, the pressure of the second reduced pressure concentration is 0.08MPa or 0.1 MPa. In certain embodiments, the temperature of the second reduced pressure concentration is 60 ℃. The second concentration under reduced pressure is used to remove alcohol from the filtrate.
In certain embodiments of the present invention, the volume ratio of the concentrated solution after the second vacuum concentration to the concentrated solution before the second vacuum concentration is 1: 3 to 5. In certain embodiments, the ratio of the volume of the concentrate after the second vacuum concentration to the volume of the concentrate before the second vacuum concentration is 1: 4.
in certain embodiments of the invention, the soluble solids content of the dilution is 4% brix.
And after obtaining the diluent, sequentially passing the diluent through an anion exchange resin and a cation exchange resin which are connected in series, and carrying out third reduced pressure concentration and drying on the effluent of the cation exchange resin to obtain the saponin compound.
In certain embodiments of the present invention, the volume ratio of the anion exchange resin to the diluent is 0.8 to 1.2: 28 to 32. In certain embodiments, the volume ratio of the anion exchange resin to the diluent is 1: 30. in some embodiments of the present invention, the ratio of the cation exchange resin to the diluent is 0.8 to 1.2: 28 to 32. In certain embodiments of the invention, the volume ratio of the cation exchange resin to the diluent is 1: 30.
in certain embodiments of the present invention, the anion exchange resin is selected from one of D941, D354 and D351. In certain embodiments of the present invention, the anion exchange resin has an aspect ratio of 4 to 6: 1. in certain embodiments, the anion exchange resin has an aspect ratio of 6: 1. in certain embodiments of the present invention, the anion exchange resin has an upper column flow rate of 1 to 2 bv/h. In certain embodiments, the anion exchange resin has an upper column flow rate of 1.5 bv/h.
In certain embodiments of the invention, the cation exchange resin is selected from one of D370, 732 and SDB-3. In certain embodiments of the present invention, the cation exchange resin has an aspect ratio of 4 to 6: 1. in certain embodiments, the cation exchange resin has an aspect ratio of 6: 1. in some embodiments of the present invention, the upper column flow rate of the ion exchange resin is 1 to 2 bv/h. In certain embodiments of the invention, the upper column flow rate of the ion exchange resin is 1 bv/h.
The invention adopts anion exchange resin and cation exchange resin to adsorb pigment components in the diluent without adsorbing saponin components, thereby achieving the purpose of removing impurities and improving the purity of the separated components. The cation exchange resin can adsorb impurities with cations such as amino acid in the effluent of the anion exchange resin on one hand, thereby achieving the purpose of purification; on the other hand, the salt is desalted, and is extracted along with the extraction solvent, so that the cation exchange resin can effectively remove the salt in the solution.
In some embodiments of the present invention, the pressure of the third vacuum concentration is 0.08 to 0.1MPa, and the temperature of the third vacuum concentration is 50 to 80 ℃. In certain embodiments, the pressure of the third reduced pressure concentration is 0.08MPa or 0.1 MPa. In certain embodiments, the temperature of the third reduced pressure concentration is 70 ℃, 80 ℃, or 75 ℃.
In certain embodiments of the present invention, the volume ratio of the concentrated solution after the third reduced pressure concentration to the concentrated solution before the third reduced pressure concentration is 1: 3 to 5. In certain embodiments, the volume ratio of the concentrated solution after the third reduced pressure concentration to the concentrated solution before the third reduced pressure concentration is 1: 4.
in the present invention, the concentrated solution after the third vacuum concentration is dried for the second time. The method of the first drying is not particularly limited in the present invention, and a drying method known to those skilled in the art may be used.
In the invention, the extraction residue after the first heating extraction is mixed with ethanol for the second heating extraction, and the water extract after the second heating extraction is subjected to the fourth reduced pressure concentration.
In some embodiments of the invention, the ethanol mixed with the extraction residue after the first heat extraction has a mass concentration of 70% to 95%. In certain embodiments, the mass concentration of ethanol mixed with the extraction residue after the first heat extraction is 80%, 85%, or 70%.
In some embodiments of the invention, the temperature of the second heating extraction is 70-85 ℃. In certain embodiments, the temperature of the second heated extraction is 80 ℃, 75 ℃, or 70 ℃.
In some embodiments of the present invention, the second heating extraction is performed 3 times, and each extraction time is 1.5-2.5 h.
In some embodiments of the present invention, after the second heating and extracting, the method further comprises: and (5) suction filtration. The method of suction filtration is not particularly limited in the present invention, and a suction filtration method known to those skilled in the art may be used. In the invention, the suction filtration after the second heating extraction is the third suction filtration.
In some embodiments of the present invention, the pressure of the fourth vacuum concentration is 0.08 to 0.1MPa, and the temperature of the fourth vacuum concentration is 50 to 70 ℃. In certain embodiments, the pressure of the fourth reduced pressure concentration is 0.08MPa or 0.1 MPa. In certain embodiments, the temperature of the fourth reduced pressure concentration is 60 ℃ or 55 ℃. In the present invention, too high a temperature of the fourth reduced-pressure concentration may result in a low concentration of the recovered ethanol and cause loss of ethanol, resulting in an increase in production cost.
In certain embodiments of the present invention, the volume ratio of the fourth vacuum-concentrated concentrate to the concentrate before the fourth vacuum-concentration is 1: 2 to 4. In certain embodiments, the volume ratio of the fourth vacuum-concentrated concentrate to the concentrate before the fourth vacuum-concentration is 1: 2 or 1: 3.
and after the fourth reduced pressure concentration is finished, drying the concentrated solution after the fourth reduced pressure concentration to obtain a crude extract, heating and dissolving the crude extract and an organic solvent, cooling and crystallizing, and performing suction filtration to obtain the beta-sitosterol.
In the present invention, the fourth concentrated solution after concentration under reduced pressure is dried to a third drying. In some embodiments of the present invention, the drying temperature of the fourth concentrated solution after decompression concentration is 50 to 70 ℃. In certain embodiments, the temperature at which the fourth concentrated solution after concentration under reduced pressure is dried is 70 ℃. In some embodiments of the present invention, the fourth concentrated solution after concentration under reduced pressure is dried under vacuum.
In certain embodiments of the present invention, the organic solvent is selected from methanol, absolute ethanol, or ethyl acetate.
In certain embodiments of the invention, the mass to volume ratio of the crude extract to organic solvent is 1 kg: 10-20L. In certain embodiments, the mass to volume ratio of the crude extract to organic solvent is 1 kg: 15L, 1 kg: 10L or 1 kg: 20L.
In some embodiments of the present invention, the temperature for heating and dissolving is 50-60 ℃. In certain embodiments, the temperature of the heated dissolution is 50 ℃, 55 ℃, or 60 ℃.
In some embodiments of the invention, the cooling crystallization temperature is 4-10 ℃, and the cooling crystallization time is 24-48 h. In certain embodiments, the temperature of the cooling crystallization is 4 ℃, 8 ℃, or 6 ℃. In certain embodiments, the cooling crystallization time is 24h, 48h, or 36 h.
The method of suction filtration is not particularly limited in the present invention, and a suction filtration method known to those skilled in the art may be used. In the invention, the suction filtration after cooling and crystallization is the fourth suction filtration.
And carrying out suction filtration for the fourth time to obtain crystals, namely the beta-sitosterol.
In certain embodiments of the present invention, the filtrate obtained after the fourth suction filtration is subjected to a subsequent treatment step of the aqueous extract after the second heating extraction to obtain beta-sitosterol again. In some embodiments of the present invention, the number of repetitions is 3-5. In certain embodiments, the number of repetitions is 3, 4, or 5.
In certain embodiments of the invention, the resulting beta-sitosterol is stored dry.
The source of the above-mentioned raw materials is not particularly limited in the present invention, and may be generally commercially available.
In the present invention, 1BV is 1 column volume.
The invention provides the method for extracting and separating the effective components in the adenophora stricta, such as polysaccharide, saponin and beta-sitosterol, with low cost, high efficiency and no pollution as the principle, and the obtained effective components have high content and strong process operability, thereby being suitable for industrial production.
The invention provides a low-cost and high-efficiency method for obtaining the adenophora stricta extract with high content, and provides data for the comprehensive utilization and development of the active ingredients of the adenophora stricta plant.
The invention takes the products with low cost, low pollution and high content as the starting points to develop the comprehensive utilization method of the effective components of polysaccharide, saponin, beta-sitosterol and the like in the adenophora stricta, the whole process flow has strong operability and is suitable for large-scale industrial continuous production.
The experimental result shows that the polysaccharide content in the crude product of the adenophora stricta polysaccharide obtained by the invention exceeds 80 wt%, and the yield is higher than 85%; the content of saponin in the finished product of adenophora stricta saponin exceeds 76 wt% and the yield is higher than 91% determined by high performance liquid chromatography; the content of beta-sitosterol in the adenophora stricta beta-sitosterol crystal exceeds 91 wt%, and the yield is higher than 89%.
In order to further illustrate the present invention, the following examples are provided to describe the isolation method of the active ingredients from adenophora stricta, but they should not be construed as limiting the scope of the present invention.
The adenophora stricta used in the invention is obtained by conventional market purchase, and the ion exchange resin and the macroporous adsorption resin used in the embodiment of the invention are purchased from Xian blue Xiao science and technology New materials, Inc.; the starting materials or chemicals used in the examples of the present invention are, unless otherwise specified, commercially available in a conventional manner.
In the embodiment of the invention, the content of total polysaccharide is measured by adopting a (UV) ultraviolet-visible spectrophotometry; the contents of saponin and beta-sitosterol were measured by High Performance Liquid Chromatography (HPLC).
Example 1
(1) Water extraction: weighing 50kg of radix adenophorae sample, cutting, pulverizing, sieving with a 40-mesh sieve, and respectively weighing 1: 15,1: 13,1: 12 volume percent, extracting for 3 times at 90 ℃ for 2h each time, performing coarse filtration, and reserving centrifugal slag for use.
(2) Centrifuging and concentrating: centrifuging the water extractive solution with horizontal screw centrifuge at rotation speed of 4000r/min and separation factor of 3500 for 5min, vacuum filtering, concentrating the filtrate under reduced pressure at 70 deg.C under 0.08MPa, and concentrating to 4 brix.
(3) And (3) polysaccharide separation and purification: and (3) passing the concentrated solution through D101 macroporous adsorption resin, wherein the column volume is 70L, and the height-diameter ratio is 6: 1, feeding the raw materials into a column at a flow rate of 1.5bv/h, collecting effluent, adding an ethanol aqueous solution with the mass concentration of 90% into the effluent, standing overnight to separate out a precipitate, centrifuging to obtain centrifugal slag, performing suction filtration and drying on the centrifugal slag, and extracting by using a Savag method to remove protein to obtain 3.5kg of a crude product of the adenophora stricta polysaccharide.
(4) And (3) separation of saponin: resolving the macroporous adsorbent resin in the step (3) with 2.5BV of 70 wt% ethanol at a flow rate of 1.5BV/h, draining the resolving solution, collecting the resolving solution, concentrating under reduced pressure at 0.08MPa and 60 ℃ until no alcohol smell exists, wherein the volume ratio of the volume after the concentration under reduced pressure to the volume before the concentration under reduced pressure is 1: 4.
(5) and (3) decoloring: adding water into the concentrated solution obtained after the vacuum concentration in the step (4) to dilute the concentrated solution to 4% brix, and enabling the concentrated solution to pass through an anion exchange resin D941 resin and be connected with a cation exchange resin 732 in series, wherein the using amounts of the two resins are respectively 50L (the volume ratio of the anion exchange resin to the diluted solution is 1: 30, and the volume ratio of the cation exchange resin to the diluted solution is 1: 30), and the height-diameter ratio of the two resins is 6: 1, the column flow rate of the two resins is 1bv/h, the effluent of the cation exchange resin is collected and is dried under the reduced pressure of 0.08MPa and at the temperature of 70 ℃ (the volume ratio of the concentrated solution after the reduced pressure concentration to the concentrated solution before the reduced pressure concentration is 1: 4), and about 5.1kg of the finished product of the adenophoral saponin is obtained.
(6) Extracting beta-sitosterol: adding 80 wt% ethanol into the extraction residue obtained in the step (1), heating and extracting at 80 ℃ for 3 times, wherein the extraction time is 2h each time, combining the three extraction solutions, carrying out suction filtration, and carrying out reduced pressure concentration at 0.08MPa and 60 ℃ (the volume ratio of the concentrated solution after the reduced pressure concentration to the concentrated solution before the reduced pressure concentration is 1: 2), thus obtaining the beta-sitosterol extraction solution.
(7) Separating and purifying beta-sitosterol: drying the beta-sitosterol extracting solution in the step (6) at 70 ℃ in vacuum to obtain beta-sitosterol crude extract dry powder, adding absolute ethyl alcohol (the mass-volume ratio of the crude extract dry powder to the organic solvent is 1 kg: 15L) to heat and dissolve at 50 ℃, then placing in a refrigerator at 4 ℃ for 24h for crystallization, and performing suction filtration; and (4) repeating the treatment steps of the filtrate after suction filtration in the step (6) on the filtrate after suction filtration for 3 times, combining the crystals after suction filtration, and drying the crystals to obtain 3.14 kg.
The content of polysaccharide in the crude product of adenophora stricta polysaccharide obtained in this example was 81.2 wt% and the yield was 85.7% as determined by ultraviolet spectrophotometry; the content of saponin in the finished product of adenophora stricta saponin is 78.3 wt% and the yield is 95% determined by high performance liquid chromatography; the beta-sitosterol content in the adenophora stricta beta-sitosterol crystal is 92.4 wt%, and the yield is 89.5%.
Example 2
(1) Water extraction: weighing 40kg of adenophora sample, cutting, powdering, sieving with a 40-mesh sieve, and respectively weighing 1: 10,1: 8,1: 7, adding water to extract for 3 times at 80 ℃, wherein the extraction time is 3h each time, carrying out coarse filtration, and reserving centrifugal slag for use.
(2) Centrifuging and concentrating: centrifuging the water extractive solution with horizontal screw centrifuge at rotation speed of 4000r/min and separation factor of 3500 for 5min, vacuum filtering, concentrating the filtrate under reduced pressure at 75 deg.C under 0.1MPa, and concentrating to 4 brix.
(3) And (3) polysaccharide separation and purification: passing the concentrated solution through AB-8 macroporous adsorbent resin, wherein the column volume is 65L, and the height-diameter ratio is 6: 1, feeding the raw materials into a column at a flow rate of 1.5bv/h, collecting effluent, adding an aqueous solution of ethanol with the mass concentration of 85% into the effluent, standing overnight to separate out a precipitate, centrifuging to obtain centrifugal slag, performing suction filtration and drying on the centrifugal slag, and removing protein by a Savag method to obtain 3.25kg of crude adenophora stricta polysaccharide.
(4) And (3) separation of saponin: resolving the macroporous adsorbent resin in the step (3) with 3BV and 75 wt% ethanol at a flow rate of 1.5BV/h, draining the resolved solution, collecting the resolved solution, concentrating under reduced pressure at 0.1MPa and 60 ℃ until no alcohol smell exists, wherein the volume ratio of the volume after the concentration under reduced pressure to the volume before the concentration under reduced pressure is 1: 4.
(5) and (3) decoloring: diluting the concentrated solution obtained in the step (4) to 4brix by adding water, passing through anion exchange resin D354 resin and connecting cation exchange resin 732 in series, wherein the use amount of the two resins is respectively 50L (the volume ratio of the anion exchange resin to the diluent is 1: 30, the volume ratio of the cation exchange resin to the diluent is 1: 30), and the height-diameter ratio of the two resins is 6: 1, the column flow rate of the two resins is 1bv/h, the effluent of the cation exchange resin is collected and is dried under the reduced pressure of 0.1MPa and at the temperature of 80 ℃ (the volume ratio of the concentrated solution after the reduced pressure concentration to the concentrated solution before the reduced pressure concentration is 1: 4), and about 4.92kg of finished product of the adenophoral saponin is obtained.
(6) Extracting beta-sitosterol: adding 85 wt% ethanol into the extraction residue obtained in the step (1), heating and extracting at 70 ℃ for 3 times, wherein the extraction time is 2h each time, combining the three extraction solutions, carrying out suction filtration, and carrying out reduced pressure concentration at 0.1MPa and 55 ℃ (the volume ratio of the concentrated solution after the reduced pressure concentration to the concentrated solution before the reduced pressure concentration is 1: 3), thus obtaining the beta-sitosterol extraction solution.
(7) Separating and purifying beta-sitosterol: drying the beta-sitosterol extracting solution in the step (6) at 70 ℃ in vacuum to obtain beta-sitosterol crude extract dry powder, adding absolute ethyl alcohol (the mass-volume ratio of the crude extract dry powder to the organic solvent is 1 kg: 20L), heating and dissolving at 55 ℃, then placing in a 6 ℃ refrigeration house for 36h for crystallization, and carrying out suction filtration; and (4) repeating the treatment steps of the filtrate after suction filtration in the step (6) on the filtrate after suction filtration, repeating the operation for 4 times, combining the crystals after suction filtration, and drying the crystals to obtain 3.23 kg.
The content of polysaccharide in the crude product of adenophora stricta polysaccharide obtained in this example was 80.3 wt% and the yield was 82.1% as determined by ultraviolet spectrophotometry; the content of saponin in the finished product of adenophora stricta saponin is 76.2 wt% and the yield is 93.1% by measuring through a high performance liquid chromatography; the beta-sitosterol content in the adenophora stricta beta-sitosterol crystal is 91.5 wt%, and the yield is 90.1%.
Example 3
(1) Water extraction: weighing 45kg of adenophora stricta sample, cutting, powdering, sieving with a 40-mesh sieve, and respectively weighing 1: 10,1: 5,1: 5, extracting for 3 times at 85 ℃ for 1.5h, performing coarse filtration, and reserving centrifugation residues for use.
(2) Centrifuging and concentrating: centrifuging the water extractive solution with horizontal screw centrifuge at rotation speed of 4000r/min and separation factor of 3500 for 5min, vacuum filtering, concentrating the filtrate under reduced pressure at 80 deg.C under 0.08MPa, and concentrating to 4 brix.
(3) And (3) polysaccharide separation and purification: passing the concentrated solution through LSA-1 macroporous adsorbent resin, wherein the column volume is 75L, and the height-diameter ratio is 6: 1, feeding the raw materials into a column at a flow rate of 1.5bv/h, collecting effluent, adding an aqueous solution of ethanol with the mass concentration of 80% into the effluent, standing overnight to separate out a precipitate, centrifuging to obtain centrifugal slag, performing suction filtration and drying on the centrifugal slag, and removing protein by a Savag method to obtain 3.3kg of crude adenophora stricta polysaccharide.
(4) And (3) separation of saponin: resolving the macroporous adsorbent resin in the step (3) with 2BV and 65 wt% ethanol at a flow rate of 1.5BV/h, draining the resolving solution, collecting the resolving solution, concentrating under reduced pressure at 0.08MPa and 65 ℃ until no alcohol smell exists, wherein the volume ratio of the volume after the concentration under reduced pressure to the volume before the concentration under reduced pressure is 1: 4.
(5) and (3) decoloring: adding water into the concentrated solution obtained in the step (4) to dilute the concentrated solution to 4brix, and connecting anion exchange resin D351 resin with cation exchange resin SDB-3 in series, wherein the use amounts of the two resins are respectively 50L (the volume ratio of the anion exchange resin to the diluent is 1: 30, the volume ratio of the cation exchange resin to the diluent is 1: 30), and the height-diameter ratio of the two resins is 6: 1, the column flow rate of the two resins is 1bv/h, the effluent of the cation exchange resin is collected and is dried under the reduced pressure of 0.08MPa and at the temperature of 75 ℃ (the volume ratio of the concentrated solution after the reduced pressure concentration to the concentrated solution before the reduced pressure concentration is 1: 4), and about 4.85kg of finished product of the adenophoral saponin is obtained.
(6) Extracting beta-sitosterol: adding 70 wt% of ethanol into the extraction residue obtained in the step (1), heating and extracting for 3 times at 75 ℃ with each extraction time being 2h, combining the three extraction solutions, carrying out suction filtration, and carrying out reduced pressure concentration at 0.08MPa and 60 ℃ (the volume ratio of the concentrated solution after the reduced pressure concentration to the concentrated solution before the reduced pressure concentration is 1: 3) to obtain the beta-sitosterol extraction solution.
(7) Separating and purifying beta-sitosterol: drying the beta-sitosterol extracting solution in the step (6) at 70 ℃ in vacuum to obtain beta-sitosterol crude extract dry powder, adding absolute ethyl alcohol (the mass-volume ratio of the crude extract dry powder to the organic solvent is 1 kg: 10L) to heat and dissolve at 60 ℃, then placing in a refrigeration house at 8 ℃ for 48h for crystallization, and performing suction filtration; and (4) repeating the treatment steps of the filtrate after suction filtration in the step (6) for 5 times, combining the crystals after suction filtration, and drying the crystals to obtain 3.3 kg.
The content of polysaccharide in the crude product of adenophora stricta polysaccharide obtained in this example was 81.4 wt% and the yield was 87.3% as determined by ultraviolet spectrophotometry; the content of saponin in the finished product of adenophora stricta saponin is 77.2 wt% and the yield is 91.6% determined by high performance liquid chromatography; the beta-sitosterol content in the adenophora stricta beta-sitosterol crystal is 92.2 wt%, and the yield is 91.1%.
The experimental result shows that the polysaccharide content in the crude product of the adenophora stricta polysaccharide obtained by the invention exceeds 80 wt%, and the yield is higher than 85%; the content of saponin in the finished product of adenophora stricta saponin exceeds 76 wt% and the yield is higher than 91% determined by high performance liquid chromatography; the content of beta-sitosterol in the adenophora stricta beta-sitosterol crystal exceeds 91 wt%, and the yield is higher than 89%.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A method for separating active ingredients from Adenophora stricta comprises the following steps:
mixing the adenophora stricta powder with water, carrying out first heating extraction, and centrifuging and carrying out first reduced pressure concentration on an aqueous extract obtained after the first heating extraction; the temperature of the first heating extraction is 70-90 ℃;
passing the concentrated solution after the first reduced pressure concentration through macroporous adsorbent resin, washing with water, collecting effluent liquid from column loading and effluent liquid from washing with water, mixing to obtain total effluent liquid, and precipitating the total effluent liquid with ethanol to obtain polysaccharide compound; the macroporous adsorption resin is selected from one of D101, AB-8 and LSA-10; the dosage ratio of the macroporous adsorption resin to the radix adenophorae powder is 1-3L: 1 kg; the height-diameter ratio of the macroporous adsorption resin is 5-7: 1; the flow rate of the macroporous adsorption resin on the column is 1-1.5 bv/h;
resolving the treated macroporous adsorption resin with an ethanol aqueous solution to obtain a resolving solution; the mass concentration of an ethanol aqueous solution adopted by the macroporous adsorption resin after the desorption treatment is 60-75%; the flow rate of an ethanol aqueous solution adopted by the macroporous adsorption resin after the analysis treatment is 1-1.5 bv/h;
carrying out second reduced pressure concentration on the analysis solution, and adding water for dilution to obtain a diluted solution;
passing the diluent through an anion exchange resin and a cation exchange resin which are connected in series, and carrying out third reduced pressure concentration and drying on the effluent liquid of the cation exchange resin to obtain a saponin compound crude product;
mixing the extraction residue obtained after the first heating extraction with ethanol with the mass concentration of 70-95%, performing second heating extraction, and performing fourth reduced pressure concentration on the ethanol extract obtained after the second heating extraction;
drying the concentrated solution after the fourth reduced pressure concentration to obtain a crude extract, heating and dissolving the crude extract and an organic solvent, cooling and crystallizing, and performing suction filtration to obtain beta-sitosterol; the organic solvent is selected from methanol, absolute ethyl alcohol or ethyl acetate; the cooling crystallization temperature is 4-10 ℃.
2. The separation method according to claim 1, wherein the particle size of the adenophora stricta powder is not more than 40 mesh.
3. The separation method according to claim 1, wherein the first heat extraction is carried out with a ratio of the adenophora stricta powder to water of 1: 10-40;
the heating extraction times of the first heating extraction are 3 times, and the extraction time is 1-3 h each time.
4. The separation method according to claim 1, wherein the rotation speed of the centrifugation of the aqueous extract after the first heating extraction is 4000r/min, and the centrifugation time is 4-6 min;
the pressure of the first decompression concentration is 0.08-0.1 MPa, and the temperature of the first decompression concentration is 70-80 ℃.
5. The separation method according to claim 1, wherein the ethanol precipitation is carried out by using an ethanol aqueous solution with a mass concentration of 80-90%.
6. The separation method according to claim 1, wherein the volume of the ethanol aqueous solution adopted by the macroporous adsorption resin after the desorption treatment is 2-3 BV.
7. The separation method according to claim 1, wherein the pressure of the second reduced pressure concentration is 0.08 to 0.1MPa, and the temperature of the second reduced pressure concentration is 60 to 65 ℃;
the anion exchange resin is selected from one of D941, D354 and D351; the height-diameter ratio of the anion exchange resin is 4-6: 1, the flow rate of the upper column is 1-2 bv/h;
the cation exchange resin is selected from one of D370, 732 and SDB-3; the height-diameter ratio of the cation exchange resin is 4-6: 1, the flow rate of the upper column is 1-2 bv/h.
8. The separation method according to claim 1, wherein the pressure of the third vacuum concentration is 0.08 to 0.1MPa, and the temperature of the third vacuum concentration is 50 to 80 ℃.
9. The separation method according to claim 1, wherein the temperature of the second heating extraction is 70 to 85 ℃;
the heating extraction times of the second heating extraction are 3 times, and the extraction time of each time is 1.5-2.5 h;
the pressure of the fourth decompression concentration is 0.08-0.1 MPa, and the temperature of the fourth decompression concentration is 50-70 ℃.
10. The separation method according to claim 1, wherein a temperature for drying the concentrated solution after the fourth vacuum concentration is 50 to 70 ℃;
the mass volume ratio of the crude extract to the organic solvent is 1 kg: 10-20L;
the heating and dissolving temperature is 50-60 ℃;
the cooling and crystallization time is 24-48 h.
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| CN111793099A (en) * | 2020-07-27 | 2020-10-20 | 湖南华诚生物资源股份有限公司 | Method for separating hesperidin, neohesperidin, naringin and synephrine from immature bitter orange |
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| CN111793099A (en) * | 2020-07-27 | 2020-10-20 | 湖南华诚生物资源股份有限公司 | Method for separating hesperidin, neohesperidin, naringin and synephrine from immature bitter orange |
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