CN111096990A - Method for extracting panax notoginseng saponins from fresh panax notoginseng - Google Patents
Method for extracting panax notoginseng saponins from fresh panax notoginseng Download PDFInfo
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Abstract
The invention relates to a method for extracting panax notoginseng saponins from fresh panax notoginseng, belonging to the technical field of medicine preparation. The method has simple operation steps, greatly reduces the production cost and the energy consumption, has the extraction efficiency of the panax notoginseng saponins up to more than 99 percent, can realize the resource utilization of the starch contained in the panax notoginseng, has the content of the starch extracted from the fresh panax notoginseng up to more than 80 percent, and has the extraction rate of more than 65 percent.
Description
Technical Field
The invention belongs to the technical field of medicine preparation, and particularly relates to a method for extracting panax notoginseng saponins from fresh panax notoginseng.
Background
The Notoginseng radix total saponin is the main effective component of Notoginseng radix, and can be used for preventing and treating cardiovascular disease and cerebrovascular disease such as hyperlipidemia, hypertension, atherosclerosis, myocardial ischemia, and ischemic stroke. The panax notoginseng saponins are mainly extracted from panax notoginseng medicinal materials, and the extraction method mainly comprises the processing steps of drying panax notoginseng, crushing, extracting by ethanol, recovering the ethanol under reduced pressure, adsorbing by macroporous resin, eluting by the ethanol, recovering the ethanol under reduced pressure, decoloring, concentrating, drying and the like.
The extraction of the panax notoginseng saponins also can be researched by a water extraction process, however, as a traditional Chinese medicine, the panax notoginseng ingredients are complex and contain panax notoginseng saponins R1, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb and the like and a plurality of enzymes, and due to the existence of the enzymes in panax notoginseng, the direct water extraction can cause part of the panax notoginseng saponins to be subjected to enzymolysis. In addition, because the aqueous extract of panax notoginseng has more impurities, has the characteristics of difficult filtration, difficult decoloration and the like, the protein, tannin and pectin which are easy to block resin are usually removed by adopting a biological enzymolysis technology and a flocculation technology, and the complex treatment processes usually cause the components of amino acid, organic acid, cellulose and the like contained in panax notoginseng to promote the conversion between saponins, so that the content of main components is unstable, the loss of the main components is large, and the extraction yield of panax notoginseng saponins is low. The current pseudo-ginseng extraction process mainly has the following problems:
(1) the contents of starch, pectin, soluble fiber, protein and other components in the panax notoginseng are high, during the extraction process of the panax notoginseng saponins, the panax notoginseng saponins are gelatinized after being heated to generate swelling, the panax notoginseng saponins are wrapped, the extraction yield is influenced, the viscosity of the solution is increased, and the difficulty in technological operation is increased.
(2) Due to the complicated operation steps, during the extraction process, heating is carried out for a plurality of times for a long time, and the amino acid, organic acid, cellulose and other components contained in the panax notoginseng promote the conversion among saponins, so that the content of the main components is unstable, the loss of the main components is large, and the extraction yield of the panax notoginseng saponins is low.
(3) Ethanol is used as an extraction solvent or a macroporous resin elution solvent for multiple times, so that the ethanol consumption is large, the production cost and energy consumption are high, and the environmental protection pressure is large.
(4) The starch content in fresh panax notoginseng is about 8 percent, the starch content in panax notoginseng is more than 25 percent, the total saponins of panax notoginseng are extracted by adopting the conventional technology, and the contained starch is difficult to realize resource utilization and is often discarded along with dregs. Because starch can be used as a nutrient substance for microorganisms, discarded medicine dregs are easy to breed microorganisms, and odor is generated by fermentation and the environment is polluted.
Disclosure of Invention
In order to overcome the problems in the background art, the invention provides a method for extracting panax notoginseng saponins from fresh panax notoginseng, which takes fresh panax notoginseng as a raw material, and comprises the steps of cleaning, grinding into slurry, standing, collecting precipitates, filtering supernatant, decoloring by ion exchange resin, enriching by macroporous adsorption resin, concentrating ethanol eluent, and drying to obtain panax notoginseng saponins. The invention adopts the pulping technology to crush and grind the fresh panax notoginseng in a short time, which can lead the starch to be fully leached, in the process, the total panax notoginseng saponins are fully contacted with purified water and then transferred into the extracting solution because of the increase of the specific surface area, thus the effective components are retained to the maximum extent, simultaneously, the use of biological enzyme, flocculating agent and repeated heating treatment are avoided, and the promotion effect of the components such as amino acid, organic acid, cellulose and the like on the conversion between the saponins is reduced. Because the extraction process is carried out at normal temperature and the contact time is short, the extraction rate of substances such as cellulose, protein, colloid, polysaccharide and the like with poor water solubility in the extraction process is reduced, the extract is subjected to standing and filtering treatment step by step to remove suspended particles, submicron floccules and other impurities, the component starch with higher content in the pseudo-ginseng can be obtained, the pollution of macromolecular substances to decolorizing resin and macroporous adsorption resin in the subsequent treatment step is avoided, and the utilization rate of the resin is improved.
In order to realize the purpose, the invention is realized by the following technical scheme:
the method for extracting the panax notoginseng saponins from the fresh panax notoginseng comprises the following steps:
(1) cleaning fresh pseudo-ginseng, washing silt, washing with purified water, adding purified water 15 times the mass of the fresh pseudo-ginseng, grinding for 3 times, adding 3-8 times of water for each time, filtering with 200-300-mesh filter cloth, and finally removing filter residues to obtain fresh pseudo-ginseng pulp.
(2) Taking fresh pseudo-ginseng pulp, standing for 4-6 hours, collecting precipitate, washing with purified water for 1-2 times, wherein the water addition amount is 3-4 times of the mass of the precipitate each time, washing and standing for 1-2 hours each time, collecting precipitate, and drying at the temperature of below 50 ℃ to obtain pseudo-ginseng starch; the Notoginseng radix total saponin is easily dissolved in water, and enters water after washing.
(3) Taking supernatant after standing, filtering, and decolorizing filtrate with resin.
(4) Concentrating the decolorized filtrate with macroporous adsorbent resin, eluting the resin with ethanol solution, collecting eluate, recovering ethanol, concentrating, and drying to obtain Notoginseng radix total saponin.
Preferably, the decolorizing resin used in the step (3) is ion exchange resin, the model is LX-T5, the ratio of length to diameter of a mounted column is more than or equal to 3:1, the flow rate of supernatant passing through the column is 4-6 BV/h, the total volume of the passing through the column is less than or equal to 30BV, and the decolorizing solution passing through the decolorizing resin is colorless, so that a small amount of precipitate or white turbidity is allowed to appear due to the change of pH.
Preferably, the macroporous adsorption resin in the step (4) is medium-polarity macroporous adsorption resin with the model D-101, the length-diameter ratio of the installed column is more than or equal to 3:1, the flow speed of the decoloring liquid passing through the column is 4-6 BV/h, the effluent liquid passing through the column is discarded, and the total volume of the passing through the column is less than or equal to 12 BV; after the column passing is finished, eluting the macroporous adsorption resin by purified water with the flow rate of not less than 4BV/h and discarding the water washing solution, wherein the flow rate is 3-4 BV/h; eluting the resin with 2-3 BV of 70-80% ethanol solution at the flow rate of 1-2 BV/h, and collecting the eluent.
Preferably, the eluent in the step (4) is decompressed and concentrated at the temperature of below 60 ℃, ethanol is recovered, and the panax notoginseng saponins which meet the medical requirements are obtained after drying.
The invention has the beneficial effects that:
the invention adopts fresh panax notoginseng as raw material, directly grinds the pulp after cleaning, collects starch after standing, removes part of impurity components, filters supernatant, firstly carries out resin decoloration treatment, directly enriches panax notoginseng saponins by macroporous resin of decolored liquid, and carries out concentration and drying on ethanol eluent to obtain the panax notoginseng saponins meeting the medicinal requirements. Compared with the conventional technology, only 1 step uses ethanol as solvent, only 1 time of ethanol recovery and concentration treatment is carried out, the operation steps are simplified, the extraction efficiency reaches more than 99 percent, and the production cost and the energy consumption are greatly reduced; and the starch contained in the pseudo-ginseng is recycled, the content of the starch extracted from the fresh pseudo-ginseng reaches more than 80 percent, and the extraction rate exceeds 65 percent.
Drawings
FIG. 1 is a simplified process flow diagram of the present invention;
FIG. 2 is an HPLC chromatogram of a Panax notoginsenosides reference of the invention;
FIG. 3 is an HPLC chromatogram of fresh Notoginseng radix slurry used in the examples of the present invention;
FIG. 4 is an HPLC chromatogram of a finished product of Panax notoginsenosides extracted from fresh Panax notoginseng in example 2 of the present invention;
remarking: FIG. 2 is purchased from the China food and drug inspection institute, and the batch numbers 110870-201603 are respectively as follows according to the peak-appearance time sequence: 1. notoginsenoside R1; 2. ginsenoside Rg 1; 3. ginsenoside Re; 4. ginsenoside Rb 1; 5. ginsenoside Rd.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings to facilitate understanding of the skilled person.
As shown in fig. 1, the method for extracting panax notoginseng saponins from fresh panax notoginseng comprises the following steps:
cleaning fresh pseudo-ginseng, washing silt, washing with purified water, adding purified water 15 times the mass of the fresh pseudo-ginseng, grinding for 3 times, adding 3-8 times of water for each time, filtering with 200-300-mesh filter cloth, and finally removing filter residues to obtain fresh pseudo-ginseng pulp. The fresh panax notoginseng is ground into slurry by adding water, so that the cell wall breaking is more thorough, the starch leaching and the dissolution of the panax notoginseng saponins in water are promoted, and the extraction rate of the panax notoginseng saponins is improved.
Taking fresh pseudo-ginseng pulp, standing for 4-6 hours, precipitating starch, cellulose, hemicellulose, high molecular polysaccharide, protein, glycoprotein and other cell structure components from the solution, collecting the precipitate, washing with purified water for 1-2 times, wherein the water addition amount is 3-4 times of the mass of the precipitate each time, standing for 1-2 hours each time, removing suspended particles and submicron impurities such as cellulose, hemicellulose, high molecular polysaccharide, protein, glycoprotein and cell structure components, collecting the precipitate, and drying at the temperature of below 50 ℃ to obtain the pseudo-ginseng starch. Meanwhile, in the process of grinding, washing and precipitating, part of enzyme is precipitated along with starch, and in the subsequent extraction, the influence of the part of enzyme on the panax notoginseng saponins is weakened or disappears. Fresh panax notoginseng pulp is filtered and precipitated, and then the panax notoginseng saponins are extracted and purified by resin from supernatant, and no heating treatment is carried out in the earlier treatment process, so that the influence of components such as starch, pectin, soluble fiber, protein and the like on the extraction of the panax notoginseng saponins is effectively solved,
taking supernatant after standing, filtering, and decolorizing filtrate with ion exchange resin; the model of the ion exchange resin LX-T5 is that the ratio of the length to the diameter of a packed column is more than or equal to 3:1, the flow rate of supernatant passing through the column is 4-6 BV/h, and the total volume of the passing through the column is less than or equal to 30 BV. The decolorized solution after passing through the decolorized resin should be colorless, allowing a small amount of precipitation or white turbidity to occur due to the change in the solution pH.
(4) Concentrating the decolorized filtrate with medium-polarity macroporous adsorbent resin, eluting the resin with ethanol solution, collecting eluate, recovering ethanol, concentrating, and drying to obtain Notoginseng radix total saponin. The model of the macroporous adsorption resin is D-101, the length-diameter ratio of a packed column is more than or equal to 3:1, the flow speed of a decoloring solution passing through the column is 4-6 BV/h, effluent liquid passing through the column is discarded, and the total volume of the passing through the column is less than or equal to 12 BV; after the column passing is finished, eluting the macroporous adsorption resin by purified water with the flow rate of not less than 4BV/h and discarding the water washing solution, wherein the flow rate is 3-4 BV/h; eluting the resin with 2-3 BV of 70-80% ethanol solution at the flow rate of 1-2 BV/h, and collecting the eluent. Concentrating the eluate at below 60 deg.C under reduced pressure, recovering ethanol, and drying to obtain Notoginseng radix total saponin meeting medicinal requirements.
In the extraction process, the operation steps are simplified, the heating times are reduced, the conditions for component conversion of the panax notoginseng saponins are reduced, the loss of main components is reduced, and the extraction efficiency of the panax notoginseng saponins is improved. In the whole extraction process, only ethanol is used when the macroporous adsorption resin is eluted, so that the concentration times are reduced, and the production cost and the energy consumption are greatly reduced.
Example 1
(1) Cleaning silt on fresh Notoginseng radix with drinking water, cleaning with purified water to obtain 500.2g of clean fresh Notoginseng radix, adding purified water, grinding into slurry for 3 times, wherein the adding amount of the purified water for 3 times is 3750ml, 2250ml and 1500ml, filtering with 200 mesh filter cloth after grinding into slurry for each time, mixing filtrates, and removing filter residue to obtain about 7500ml of fresh Notoginseng radix slurry.
(2) Taking fresh pseudo-ginseng pulp, standing for 6 hours, collecting 81.1g of precipitate, adding 320g of purified water, uniformly suspending, standing for 1 hour, collecting the precipitate, removing tawny impurities on the surface layer of the precipitate, and drying in an oven at 50 ℃ to obtain 36.0g of pseudo-ginseng starch.
(3) Taking supernatant after standing, filtering with filter paper under reduced pressure to obtain 7400ml of filtrate, decolorizing the clarified filtrate with pretreated LX-T5 resin with the resin content of 350 ml; the length-diameter ratio is about 3:1, and the flow velocity of the column passing is about 4BV/h, thus obtaining the destaining solution.
(4) About 7600ml of decolored liquid, enriching components by pretreated D-101 macroporous adsorption resin, wherein the volume of the resin is 750ml, the length-diameter ratio is about 5:1, the flow rate of the passing column is about 4BV/h, and the effluent of the passing column is discarded. 3000ml of purified water is taken to wash the resin with the flow rate of about 4BV/h, and water-soluble impurities are removed. Then eluting with 80% ethanol solution as eluent at 2000ml flow rate of 2 BV/h. Collecting eluate, concentrating under reduced pressure at 60 deg.C, recovering ethanol, and vacuum drying at 65 deg.C to obtain 10.8642g of Notoginseng radix total saponin.
Example 2
(1) Cleaning fresh Notoginseng radix with drinking water, washing with purified water, weighing 1000.3g of fresh Notoginseng radix, adding purified water, grinding into slurry for 3 times, wherein the addition amount of the purified water for 3 times is 7.5L, 4.5L and 3L, filtering with 300 mesh filter cloth, mixing filtrates, and removing residue to obtain fresh Notoginseng radix slurry of about 15L;
(2) taking fresh pseudo-ginseng pulp, standing for 4 hours, collecting precipitate of about 112.3g, adding purified water of 350g for uniformly suspending, standing for 2 hours, collecting precipitate, removing yellow brown impurities on the surface layer of the precipitate, and drying in a 50 ℃ oven to obtain 67.8g of pseudo-ginseng starch;
(3) taking supernatant after standing, adding 1% diatomite filter paper, and performing vacuum filtration to obtain about 15L of filtrate, decolorizing the clarified filtrate by pretreated LX-T5 resin, wherein the resin content is 750 ml; the length-diameter ratio is about 4.5:1, the flow speed of the column passing is about 6BV/h, and the decolored liquid is obtained.
(4) And (3) enriching components of about 15L of decolorized liquid by using pretreated D-101 macroporous adsorption resin, wherein the volume of the resin is 1875ml, the length-diameter ratio is about 5:1, the flow rate of passing through the column is about 6BV/h, and the effluent of passing through the column is discarded. 5600ml of purified water was taken and the resin was washed with water at a flow rate of about 4BV/h to remove water soluble impurities. Eluting with 70% ethanol solution 3750ml, and eluting at flow rate of 1 BV/h. Collecting eluate, concentrating under reduced pressure at 60 deg.C, recovering ethanol, and vacuum drying at 65 deg.C to obtain 21.2528g of Notoginseng radix total saponin.
The HPLC chromatogram of the panax notoginseng saponins obtained in the embodiment is shown in figure 4, and can be seen by comparing figure 3 with figure 4: the fresh panax notoginseng pulp has high impurity content, more impurity peaks appear in a map except for 5 main peaks of panax notoginseng saponins, the area ratio of the impurity peaks is high, and the separation degrees of ginsenoside Rg1 and ginsenoside Re are poor. After the process treatment, the finished product of the panax notoginseng saponins with higher content is obtained, the HPLC chromatogram is consistent with that of a reference substance, and the proportion of the peak area of impurities is obviously reduced.
Example 3
(1) Cleaning fresh Notoginseng radix with drinking water, washing with purified water, weighing clean fresh Notoginseng radix 1000.0g, adding purified water, grinding into slurry for 3 times, wherein the addition amount of the purified water for 3 times is 7.5L, 4.5L and 3L, filtering with 300 mesh filter cloth, mixing filtrates, and removing residue to obtain fresh Notoginseng radix slurry about 15L.
(2) Taking fresh pseudo-ginseng pulp, standing for 4h, collecting precipitate of about 124.3g, adding purified water of 400g, uniformly suspending, standing for 2h, collecting precipitate, removing yellow brown impurities on the surface layer of the precipitate, and drying in an oven at 50 ℃ to obtain pseudo-ginseng starch of 73.1 g.
(3) Taking supernatant after standing, adding 1% diatomite filter paper, and performing vacuum filtration to obtain about 15L of filtrate, decolorizing the clarified filtrate by pretreated LX-T5 resin, wherein the resin content is 600 ml; the length-diameter ratio is about 3.6:1, the flow speed of the column passing is about 5BV/h, and the decolored liquid is obtained.
(4) And (3) enriching components of about 15L of decolorized solution by using pretreated D-101 macroporous adsorption resin, wherein the volume of the resin is 1670ml, the length-diameter ratio is about 4.5:1, the flow rate of the passing column is about 5BV/h, and the effluent of the passing column is discarded. 5000ml of purified water is taken to flush the resin, and the water-soluble impurities are removed at a flow rate of about 4 BV/h. Eluting with 75% ethanol solution 4200ml at flow rate of 1.5 BV/h. Collecting eluate, concentrating under reduced pressure at 60 deg.C, recovering ethanol, and vacuum drying at 65 deg.C to obtain 21.6416g of Notoginseng radix total saponin.
Example 4
(1) Cleaning fresh Notoginseng radix with drinking water, washing with purified water, weighing 1000.3g of fresh Notoginseng radix, adding purified water, grinding into slurry for 3 times, wherein the addition amount of the purified water for 3 times is 7.5L, 4.5L and 3L, filtering with 300 mesh filter cloth, mixing filtrates, and removing residue to obtain fresh Notoginseng radix slurry of about 15L;
(2) taking fresh pseudo-ginseng pulp, standing for 4 hours, collecting about 135.3g of precipitate, adding 500g of purified water, uniformly suspending, standing for 2 hours, collecting the precipitate, removing tawny impurities on the surface layer of the precipitate, adding 400g of purified water again, uniformly suspending, standing for 1 hour, collecting the precipitate, and drying in a 50 ℃ oven to obtain 74.8g of pseudo-ginseng starch;
(3) taking supernatant after standing, adding 1% diatomite filter paper, and performing vacuum filtration to obtain about 15L of filtrate, decolorizing the clarified filtrate by pretreated LX-T5 resin, wherein the resin content is 500 ml; the length-diameter ratio is about 3:1, and the flow velocity of the column passing is about 4BV/h, thus obtaining the destaining solution.
(4) And (3) enriching components of about 15L of decolorized liquid by using pretreated D-101 macroporous adsorption resin, wherein the volume of the resin is 1500ml, the length-diameter ratio is about 4:1, the flow rate of passing through the column is about 4BV/h, and the effluent of passing through the column is discarded. 4500ml of purified water was taken and the resin was washed with water at a flow rate of about 4BV/h to remove water soluble impurities. Eluting with 75% ethanol solution at 4500ml flow rate of 2 BV/h. Collecting eluate, concentrating under reduced pressure at 60 deg.C, recovering ethanol, and vacuum drying at 65 deg.C to obtain 22.9145g of Notoginseng radix total saponin.
Analysis of test data for each example
Analysis and detection method
(1) Determination of total saponin content in notoginseng
The sample treatment and content determination were carried out according to the methods of Panax notoginseng and Panax notoginseng saponins of the first edition of the Chinese pharmacopoeia 2015, the reference was purchased from the institute of Chinese food and drug inspection, lot number 110870 201603, the content of Panax notoginseng saponins (notoginsenoside R17.40%, ginsenoside Rg 126.30%, ginsenoside Re 3.70%, ginsenoside Rb127.70%, and ginsenoside Rd 7.60%) was 72.70%, and the analysis results of the reference are shown in Table 1.
TABLE 1 Total arasaponin reference substance component content and peak area
(2) Starch content determination
Referring to the iodine color development method reported in the literature (Zhang Qin Song et al. iodine color development method for determining starch content [ J ] in tobacco, tobacco science and technology/tobacco chemistry, 2004(5):24-26), 10mg of sample is precisely weighed, placed in a 10ml test tube, added with 5ml of purified water, water-bathed until complete gelatinization, kept for 5min, cooled to room temperature, transferred to a 100ml measuring flask, added with water to dilute to the scale, shaken up to be used as a sample stock solution. Taking 10ml of iodine-added solution (2.6 g of iodine and 5.0g of potassium iodide are weighed and placed in a beaker, dissolved by a proper amount of water, added with water to 1000ml, shaken up and newly dispensed), 0.5ml of the iodine-added solution is uniformly mixed to be used as a sample measuring solution, the absorbance is measured at the wavelength of 575nm, the sample measuring solution is compared with a standard curve drawn by soluble starch with different concentrations, the starch content in the sample is calculated, and the analysis result of the standard curve is shown in table 2.
TABLE 2 standard curve drawing table for starch content determination
Second, analysis of Notoginseng radix materials used in examples 1 to 4
(1) Moisture determination
Measuring according to the second method of 0832 in the fourth part of 2015 edition of Chinese pharmacopoeia, weighing 103.8521g of clean fresh radix Notoginseng, placing in an electric heating air blast drying oven, drying at 105 ℃ until the weight loss is not more than 5mg after two times of continuous weighing, obtaining 28.3517g of dried radix Notoginseng, and calculating the drying yield to be 27.30%.
(2) Determination of total saponin content in notoginseng
The detection shows that the content of the panax notoginseng saponins in the dried panax notoginseng is 6.15 percent, the content of the panax notoginseng saponins in the fresh panax notoginseng is 1.68 percent according to the drying yield, and the analysis result is shown in table 3.
(3) Starch content determination
The starch content in the fresh panax notoginseng is 7.98 percent and the content is 29.23 percent in terms of dry panax notoginseng through determination, and the analysis results are shown in table 4.
Analysis of Panax notoginsenosides obtained in examples 1-4
The contents of the panax notoginseng saponins obtained in the examples 1-4 are 78.14%, 78.70%, 80.04% and 80.49%, respectively, and the analysis results are shown in table 3.
TABLE 3 determination of the Total saponins of Panax notoginseng in the dried Panax notoginseng and the samples of examples 1-4
Fourth, measurement of starch content obtained in examples 1 to 4
The starch samples obtained in examples 1-4 were determined to have a content of 81.50%, 80.70%, 82.26%, 86.76%, respectively, and the analytical results are shown in Table 4.
TABLE 4 determination of starch content in fresh Notoginseng radix and samples of examples 1-4
Note: weighing 10g of fresh pseudo-ginseng, adding water, fully grinding the mixture into pulp, fixing the volume to 1000ml, gelatinizing the pulp in a water bath, and measuring the starch content according to the method.
Fifth, statistics of results of examples 1-4
Through the treatment of the process technology, the content of the finished product of the panax notoginseng saponins prepared in the embodiments 1 to 4 is more than or equal to 78 percent and meets the requirements of Chinese pharmacopoeia; the content of the panax notoginseng saponins in the medicinal materials is taken as a reference, and the extraction rate of the panax notoginseng saponins reaches more than 99 percent; the content of starch extracted from fresh pseudo-ginseng reaches more than 80%, the extraction rate exceeds 65%, and the analysis result is shown in table 5.
Table 5 statistical table of experimental data of examples 1 to 4
Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the invention as defined by the appended claims.
Claims (4)
1. A method for extracting panax notoginseng saponins from fresh panax notoginseng is characterized in that: the method for extracting the panax notoginseng saponins from the fresh panax notoginseng comprises the following steps:
(1) cleaning fresh pseudo-ginseng, washing silt, washing with purified water, adding 15 times of purified water of fresh pseudo-ginseng, grinding for 3 times, adding 3-8 times of water for each time, filtering with 200-300 mesh filter cloth, and removing filter residue to obtain fresh pseudo-ginseng pulp;
(2) taking fresh pseudo-ginseng pulp, standing for 4-6 hours, collecting precipitate, washing with purified water for 1-2 times, adding water in an amount which is 3-4 times of the amount of the precipitate each time, washing and standing for 1-2 hours each time, collecting precipitate, and drying at the temperature of below 50 ℃ to obtain pseudo-ginseng starch and supernatant;
(3) taking supernatant after standing, filtering, and decolorizing filtrate with resin;
(4) concentrating the decolorized filtrate with macroporous adsorbent resin, eluting the resin with ethanol solution, collecting eluate, recovering ethanol, concentrating, and drying to obtain Notoginseng radix total saponin.
2. The method for extracting panax notoginseng saponins from fresh panax notoginseng according to claim 1, which is characterized in that: the decolorizing resin used in the step (3) is ion exchange resin with the model number LX-T5, the ratio of length to diameter of a packed column is more than or equal to 3:1, the flow rate of supernatant passing through the column is 4-6 BV/h, and the total volume of the passing through the column is less than or equal to 30 BV.
3. The method for extracting panax notoginseng saponins from fresh panax notoginseng according to claim 1, which is characterized in that: the macroporous adsorption resin in the step (3) is medium-polarity macroporous adsorption resin with the model D-101, the ratio of length to diameter of a packed column is more than or equal to 3:1, the flow rate of a decoloring solution passing through the column is 4-6 BV/h, effluent liquid passing through the column is discarded, and the total volume of the passing through the column is less than or equal to 12 BV; after the column passing is finished, eluting the macroporous adsorption resin by purified water with the flow rate of not less than 4BV/h and discarding the water washing solution, wherein the flow rate is 3-4 BV/h; eluting the resin with 2-3 BV of 70-80% ethanol solution at the flow rate of 1-2 BV/h, and collecting the eluent.
4. The method for extracting panax notoginseng saponins from fresh panax notoginseng according to claim 1 or 3, wherein the method comprises the following steps: and (4) concentrating the eluent at the temperature of below 60 ℃ under reduced pressure, recovering ethanol, and drying to obtain the panax notoginseng saponins meeting the medicinal requirements.
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| CN115177977A (en) * | 2022-08-01 | 2022-10-14 | 湖南凯耀生物科技有限公司 | Method and device for batch extraction of gypenoside from whole gynostemma pentaphylla |
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| CN108126000A (en) * | 2017-03-16 | 2018-06-08 | 楚雄云植药业有限公司 | Arasaponin extracts preparation method in fresh Radix Notoginseng |
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