CN111040011A - Refining method of high-purity ginsenoside Rg1 - Google Patents
Refining method of high-purity ginsenoside Rg1 Download PDFInfo
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- CN111040011A CN111040011A CN201911356671.0A CN201911356671A CN111040011A CN 111040011 A CN111040011 A CN 111040011A CN 201911356671 A CN201911356671 A CN 201911356671A CN 111040011 A CN111040011 A CN 111040011A
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Abstract
The invention discloses a refining method of high-purity ginsenoside Rg1, which comprises the steps of crushing raw materials containing ginsenoside Rg1, carrying out enzymatic hydrolysis, adding ethanol, and carrying out heating reflux extraction to obtain an extracting solution; then, eluting by using a chromatographic column and respectively using low-concentration ethanol aqueous solution and medium-concentration ethanol aqueous solution as gradient eluents; and finally, collecting the eluent in sections, concentrating and drying to obtain the high-purity ginsenoside Rg 1. According to the refining method disclosed by the invention, the recovery rate of 85-95% can be realized, and the content of the total ginsenoside Rg1 in the product can reach more than 40-95%. The solvent used in the method can be recycled, and the whole industrial production is a typical green clean process. The production period of the product is short, the production cost is low, and the production process is non-toxic and safe and has no environmental pollution.
Description
Technical Field
The invention belongs to the field of medicines, and particularly relates to a method for refining high-purity ginsenoside Rg 1.
Background
The ginseng is a traditional and rare Chinese medicine in China, has strong efficacy of tonifying qi and generating blood, and the ginsenoside Rg1 is a main active ingredient of the ginseng. Pharmacological research shows that the ginsenoside Rgl has the effects of resisting aging, reducing nerve cell damage, promoting brain function recovery, promoting protein synthesis in brain, increasing synapse number, enhancing memory and the like, and promotes the proliferation and differentiation of chronic stress nerve stem cells. The ginsenoside Rg1 is also one of the main components in the panax notoginseng and the American ginseng, is usually used for activating blood circulation and removing blood stasis, dredging collaterals and activating collaterals, has pharmacological effects on hyperlipidemia, high blood viscosity and hypertension, has the effects of resisting myocardial ischemia, atherosclerosis, thrombus and heart and brain ischemia and the like, is mainly prepared from the total components of the panax notoginseng saponins clinically, and has no single component or combined preparation thereof.
The method for purifying the panax notoginseng saponins, the panax ginseng saponins and the panax quinquefolium saponins mainly adopts a chromatography purification process, is assisted by common impurity removal means such as alumina, activated carbon and the like, and has the main products of various saponins and sapogenins, the purity of which is about 85 percent, the content of a single component Rg1 is below 30 percent, and no extraction and purification method aiming at each component in the saponins and the sapogenins. At present, no extraction process for purifying the ginsenoside Rg1 to more than 40-95% is disclosed.
The silica gel and polymer as the matrix are two kinds of chromatographic medium with supplementary performance essential for chromatographic separation and analysis. The silica gel matrix has high mechanical strength, high column efficiency and good resolution, is widely applied to the analysis and large-scale preparation production of organic compounds and neutral molecules, but a large amount of toxic and harmful reagents are used in the preparation process; the polymer matrix filler has good chemical stability and no comparable acid-base resistance, so the polymer matrix filler has long service life and can be cleaned on line and is suitable for large-scale purification and separation of biomolecules. Researches prove that because of the difference of the materials in silica gel and polymer chromatographic packing, the silica gel and the polymer chromatographic packing have strong complementarity on the separation selectivity of target molecules, for example, substances which are difficult to separate by using the polymer packing can be well separated on the silica gel packing; conversely, some substances are difficult to separate on silica gel fillers, while efficient separation can be obtained with polymeric fillers. Aiming at the problem of low purity of the extraction method of ginsenoside Rg1 in the prior art, the inventor finally provides the invention through a large amount of research.
Disclosure of Invention
The invention aims to provide a refining method for obtaining high-purity ginsenoside Rg1 from panax notoginseng saponins through one-step separation.
The method for refining the high-purity ginsenoside Rg1 is characterized by comprising the following steps of:
2) pulverizing raw materials containing ginsenoside Rg1, performing enzyme hydrolysis, adding ethanol, heating and reflux extracting, filtering, and concentrating to obtain alcohol-free water solution;
2) taking the extracting solution obtained in the step 1) to pass through a chromatographic column filled with a separation medium;
3) removing impurities from the chromatographic column with low concentration ethanol water solution, performing gradient elution with medium concentration ethanol water solution, and monitoring the eluate by TLC;
4) collecting eluate by stages, concentrating, and drying to obtain high purity ginsenoside Rg 1.
Preferably, step 1) is carried out by: pulverizing raw materials containing ginsenoside Rg1, sieving, adding distilled water, adjusting pH to 3.0-5.0, adding a certain amount of complex enzyme preparation, performing enzymolysis at 35-50 deg.C for 1-3 hr, adding ethanol to obtain 50-70% ethanol, heating under reflux, extracting, filtering, and concentrating to obtain alcohol-free water solution.
Further preferably, the complex enzyme preparation in the step 1) comprises the following components in parts by weight based on 100 parts by weight of raw materials: 1-3 parts of cellulase, 2-3 parts of protease, 1-3 parts of amylase and 1-7 parts of pectinase mixture.
More preferably, the addition amount of the complex enzyme preparation is 0.02-0.08% of the weight of the extraction raw material powder.
Preferably, the separation medium packed in the chromatography column in step 2) is a small pore resin.
More preferably, the pore size of the small pore resin is 20 to 50 angstroms.
More preferably, the pore size of the separation medium is 30-40 angstroms.
More preferably, the small pore resin is a non-polar or weakly polar or a medium polar or reversed phase resin.
Preferably, the height ratio of the chromatographic column diameter in the step 2) is 1: 1-30.
More preferably, the ratio of the height to the diameter of the column is 1: 3.
Preferably, the concentration of the low-concentration ethanol used for the chromatographic column in the step 3) is 10-30% by mass, and is used for removing impurities; eluting with 30-60 wt% ethanol solution.
More preferably, the concentration of the low-concentration ethanol used for the chromatographic column is 20-30% by mass, and is used for removing impurities; eluting with 40-50 wt% ethanol solution.
Preferably, the content of the high-purity ginsenoside finally obtained in the step 4) is 40-95%.
More preferably, the content of the finally obtained high-purity ginsenoside is 60-95%.
More preferably, the content of the finally obtained high-purity ginsenoside is 70-95%.
More preferably, the content of the finally obtained high-purity ginsenoside is 80-95%.
More preferably, the content of the finally obtained high-purity ginsenoside is 90-95%.
More preferably, the content of the finally obtained high-purity ginsenoside is 90%.
More preferably, the content of the finally obtained high-purity ginsenoside is 95%.
More preferably, the content of the finally obtained high-purity ginsenoside is 92%.
The weight parts in the present invention may be ug, mg, g, kg or other known weight units.
The purity of the ginsenoside Rg1 is obtained by combining the fractions, the fractions are firstly detected by thin-layer chromatography, and the concentrated product is detected by high performance liquid chromatography.
Advantageous effects
The technical scheme is summarized by repeatedly groping through long-term practice, the used raw materials are easy to obtain, and the huge waste of the environment and resources caused by the treatment method for obtaining the high-content ginsenoside Rg1 by using toxic and harmful solvents can be solved. The invention is a high-efficiency extraction and separation technology, which can effectively separate high-content ginsenoside Rg1 from ginseng, pseudo-ginseng and American ginseng, the recovery rate reaches 85-95%, and the product content reaches more than 40-95%.
All the solvents can be recycled, and the whole industrial production is a typical green clean process. The production period of the product is short, the production cost is low, and the production process is non-toxic and safe and has no environmental pollution.
Detailed Description
Hereinafter, the present invention will be described in detail. Before the description is made, it should be understood that the terms used in the present specification and the appended claims should not be construed as limited to general and dictionary meanings, but interpreted based on the meanings and concepts corresponding to technical aspects of the present invention on the basis of the principle that the inventor is allowed to define terms appropriately for the best explanation. Accordingly, the description proposed herein is just a preferable example for the purpose of illustrations only, not intended to limit the scope of the invention, so it should be understood that other equivalents and modifications could be made thereto without departing from the spirit and scope of the invention.
The following examples are given by way of illustration of embodiments of the invention and are not to be construed as limiting the invention, and it will be understood by those skilled in the art that modifications may be made without departing from the spirit and scope of the invention. Unless otherwise specified, reagents and equipment used in the following examples are commercially available products.
Example 1
1) Crushing 10 kg of ginseng raw material, sieving, adding 30L of distilled water, adjusting the pH value to be 3.0, adding 8g of a mixture of 1 part of cellulase, 2 parts of protease, 3 parts of amylase, 4 parts of pectinase and a complex enzyme preparation, performing enzymatic hydrolysis at the temperature of 40 ℃, hydrolyzing for 1 hour, adding ethanol to prepare an ethanol aqueous solution with the mass percentage concentration of 50% of ethanol, heating, refluxing, stirring and extracting, filtering by using a plate frame, and extracting filtrate for the first time; extracting the filter residue with 50% ethanol, filtering with plate and frame, filtering the second filtrate, mixing the first and second filtrates, concentrating to obtain ethanol-free water solution, and adding water to obtain 10L extractive solution;
2) the extract obtained in step 1) was passed through a chromatography column (diameter/height ratio 1: 3) resin pore size is 20 angstroms);
3) removing impurities from the chromatographic column with 10% ethanol water solution, respectively eluting with 30% ethanol, and monitoring the eluate by TLC; collecting the ethanol flow with the mass percent concentration of 60 percent.
4) Collecting eluate by thin layer chromatography with Rg1 of high purity, concentrating, and drying to obtain ginsenoside Rg 160% (HPLC liquid phase detection), with recovery rate of 70.2%.
Example 2
1) Crushing 10 kg of pseudo-ginseng raw materials, sieving the crushed raw materials by a sieve of 20 meshes, adding 30L of distilled water, adjusting the pH value to be 3.0, adding 8g of a mixture of 1 part of cellulase, 2 parts of protease, 3 parts of amylase, 4 parts of pectinase and a complex enzyme preparation, performing enzymatic hydrolysis for 1 hour, adding ethanol to prepare an ethanol aqueous solution with the mass percentage concentration of 50% of ethanol, heating, refluxing, stirring and extracting, filtering by a plate frame, and extracting filtrate for the first time; extracting the filter residue with 50% ethanol, filtering with plate and frame, filtering the second filtrate, mixing the first and second filtrates, concentrating to obtain ethanol-free water solution, and adding water to obtain 10L extractive solution;
2) the extract obtained in step 1) was passed through a chromatography column (diameter/height ratio 1:3, the pore diameter of the resin is 20 angstroms);
3) removing impurities from the chromatographic column by using 10% by mass of ethanol water solution, respectively eluting 30% and 60% by mass of ethanol water solution, and monitoring the eluent by TLC; collecting ethanol flow with the mass percent concentration of 60 percent.
4) Collecting eluate by thin layer chromatography with Rg1 of high purity, concentrating, and drying to obtain ginsenoside Rg 160% (HPLC liquid phase detection), with recovery rate of 70.2%.
Example 3
1) Crushing 10 kg of American ginseng raw material, sieving with a 30-mesh sieve, adding 40L of distilled water, adjusting the pH value to 5.0, adding 2g of a mixture of 3 parts of cellulase, 3 parts of protease, 3 parts of amylase, 1 part of pectinase and a complex enzyme preparation, performing enzymatic hydrolysis for 2 hours, adding ethanol to prepare an ethanol aqueous solution with the mass percentage concentration of 70% of ethanol, heating, refluxing, stirring and extracting, filtering with a plate frame, and extracting filtrate for the first time; extracting the filter residue with 70% ethanol, filtering with plate and frame, filtering the second filtrate, mixing the first and second filtrates, concentrating to obtain ethanol-free water solution, and adding water to obtain 15L extractive solution;
2) the extract obtained in step 1) was passed through a chromatography column (diameter/height ratio 1: 5, the pore diameter of the resin is 50 angstroms);
3) removing impurities from the chromatographic column by using 30% by mass of ethanol water solution, eluting by using 50% by mass of ethanol water solution, and monitoring the eluent by using TLC (thin layer chromatography); the 50% ethanol fractions were collected.
4) Collecting eluate by thin layer chromatography with Rg1 of high purity, concentrating, and drying to obtain ginsenoside Rg 190% (HPLC liquid phase detection), with recovery rate of 60.2%.
Example 4
1) Crushing 10 kg of pseudo-ginseng raw material, sieving with a 40-mesh sieve, adding 30L of distilled water, adjusting the pH value to 3.5, adding 6g of a mixture of 2 parts of cellulase, 2 parts of protease, 1 part of amylase, 5 parts of pectinase and a complex enzyme preparation, performing enzymatic hydrolysis for 2.5 hours, adding ethanol to prepare an ethanol aqueous solution with the ethanol mass percentage concentration of 60%, heating, refluxing, stirring and extracting, filtering with a plate frame, and extracting filtrate for the first time; extracting the filter residue with 60% ethanol, filtering with plate and frame, filtering the second filtrate, mixing the first and second filtrates, concentrating to obtain ethanol-free water solution, and adding water to obtain 10L extractive solution;
2) the extract obtained in step 1) was passed through a chromatography column (diameter/height ratio 1:3, the pore diameter of the resin is 30 angstrom);
3) removing impurities from the chromatographic column by using an ethanol water solution with the mass percent concentration of 28%, eluting by using an ethanol water solution with the mass percent concentration of 60%, and monitoring the eluent by using TLC (thin layer chromatography); the 60% ethanol fractions were collected.
4) Collecting eluate by thin layer chromatography with Rg1 of high purity, concentrating, and drying to obtain ginsenoside Rg 195% (HPLC liquid phase detection), with recovery rate of 40.2%.
Example 5
1) Crushing 10 kg of pseudo-ginseng raw material, sieving with a 40-mesh sieve, adding 30L of distilled water, adjusting the pH value to 3.0, adding 4g of a mixture of 3 parts of cellulase, 2 parts of protease, 1 part of amylase, 4 parts of pectinase and a complex enzyme preparation, performing enzymatic hydrolysis for 3 hours, adding ethanol to prepare an ethanol aqueous solution with the ethanol mass percentage concentration of 70%, heating, refluxing, stirring and extracting, filtering with a plate frame, and extracting filtrate for the first time; extracting the filter residue with 70% ethanol, filtering with plate and frame, filtering the second filtrate, mixing the first and second filtrates, concentrating to obtain ethanol-free water solution, and adding water to obtain 10L extractive solution;
2) the extract obtained in step 1) was passed through a chromatography column (diameter/height ratio 1: 3.5, the pore diameter of the resin is 30 angstroms);
3) removing impurities from the chromatographic column by using an ethanol aqueous solution with the mass percent concentration of 26%, eluting by using an ethanol aqueous solution with the mass percent concentration of 45%, and monitoring the eluent by using TLC (thin layer chromatography); the 45% ethanol fractions were collected.
4) Collecting eluate by thin layer chromatography with Rg1 of high purity, concentrating, and drying to obtain ginsenoside Rg 190% (HPLC liquid phase detection), with recovery rate of 38% from raw material to product.
Example 6
1) Crushing 10 kg of pseudo-ginseng raw materials, sieving the crushed raw materials by a 40-mesh sieve, adding 30L of distilled water, adjusting the pH value to 2.5, adding 7g of a mixture of 3 parts of cellulase, 2 parts of protease, 1 part of amylase, 4 parts of pectinase and a complex enzyme preparation, performing enzymatic hydrolysis for 1 hour, adding ethanol to prepare an ethanol aqueous solution with the ethanol mass percentage concentration of 65%, heating, refluxing, stirring and extracting, filtering by a plate frame, and extracting filtrate for the first time; extracting the filter residue with 65% ethanol, filtering with plate and frame, filtering the second filtrate, mixing the first and second filtrates, concentrating to obtain ethanol-free water solution, and adding water to obtain 10L extractive solution;
2) the extract obtained in step 1) was passed through a chromatography column (diameter/height ratio 1: 4, the pore diameter of the resin is 35 angstroms);
3) removing impurities from the chromatographic column by using 28 mass percent ethanol water solution, eluting by using 45 mass percent ethanol water solution, and monitoring the eluent by using TLC (thin layer chromatography); the 45% ethanol fractions were collected.
4) Collecting eluate by thin layer chromatography with Rg1 of high purity, concentrating, and drying to obtain ginsenoside Rg 192% (HPLC liquid phase detection), with recovery rate of 38.2%.
Example 7
1) Crushing 10 kg of pseudo-ginseng raw material, sieving with a 40-mesh sieve, adding 30L of distilled water, adjusting the pH value to 3.5, adding 8g of a mixture of 3 parts of cellulase, 2 parts of protease, 1 part of amylase, 4 parts of pectinase and a complex enzyme preparation, performing enzymatic hydrolysis for 1.5 hours, adding ethanol to prepare an ethanol aqueous solution with the ethanol mass percentage concentration of 70%, heating, refluxing, stirring and extracting, filtering with a plate frame, and extracting filtrate for the first time; extracting the filter residue with 70% ethanol, filtering with plate and frame, filtering the second filtrate, mixing the first and second filtrates, concentrating to obtain ethanol-free water solution, and adding water to obtain 10L extractive solution;
2) the extract obtained in step 1) was passed through a column (diameter/height ratio 1:3, the pore diameter of the resin is 50 angstroms);
3) removing impurities from the chromatographic column by using an ethanol aqueous solution with the mass percent concentration of 28%, eluting by using an ethanol aqueous solution with the mass percent concentration of 45%, and monitoring the eluent by using TLC (thin layer chromatography); the 45% ethanol fractions were collected.
4) Collecting eluate by thin layer chromatography with Rg1 of high purity, concentrating, and drying to obtain ginsenoside Rg 192% (HPLC liquid phase detection), with recovery rate of 38.2%.
Conclusion
The refining method can efficiently obtain the high-purity ginsenoside Rg 1.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (6)
1. A refining method of high-purity ginsenoside Rg1 is characterized by comprising the following steps:
1) pulverizing raw materials containing ginsenoside Rg1, performing enzyme hydrolysis, adding ethanol, heating and reflux extracting, filtering, and concentrating to obtain alcohol-free water solution;
2) taking the extracting solution obtained in the step 1) to pass through a chromatographic column filled with a separation medium;
3) removing impurities from the chromatographic column with low concentration ethanol water solution, performing gradient elution with medium concentration ethanol water solution, and monitoring the eluate by TLC;
4) collecting eluate by stages, concentrating, and drying to obtain high purity ginsenoside Rg 1.
2. The refining process according to claim 1, characterized in that step 1) is carried out by: pulverizing raw materials containing ginsenoside Rg1, sieving, adding distilled water into the raw material powder, adjusting pH to 3.0-5.0, adding a certain amount of complex enzyme preparation, performing enzymolysis at 35-50 deg.C for 1-3 hr, adding ethanol to obtain 50-70% ethanol by weight percentage, heating, reflux extracting, filtering, and concentrating to obtain alcohol-free water solution;
preferably, the complex enzyme preparation in the step 1) comprises the following components in parts by weight based on 100 parts by weight of raw materials: 1-3 parts of cellulase, 2-3 parts of protease, 1-3 parts of amylase and 1-7 parts of pectinase mixture;
more preferably, the addition amount of the complex enzyme preparation is 0.02-0.08% of the weight of the extraction raw material powder.
3. The purification method according to claim 1, wherein the separation medium packed in the chromatography column in step 2) is a small pore resin;
the pore diameter of the small-pore resin is 20-50 angstroms, and preferably, the pore diameter of the separation medium is 30-40 angstroms;
the small-pore resin is nonpolar or low-polarity or medium-polarity or reversed-phase resin.
4. The purification method according to claim 1, wherein the ratio of the height to the diameter of the chromatography column in step 2) is 1:1 to 30, preferably 1: 3.
5. The refining method as claimed in claim 1, wherein the concentration of the low concentration ethanol used for the chromatography column in step 3) is 10-30% by mass for removing impurities; eluting with 30-60 wt% ethanol;
more preferably, the concentration of the low-concentration ethanol used for the chromatographic column is 20-30% by mass, and is used for removing impurities; eluting with 40-50 wt% ethanol solution.
6. The refining method according to claim 1, wherein the content of the high-purity ginsenoside finally obtained in the step 4) is 40 to 95%, preferably 60 to 95%, more preferably 70 to 95%, more preferably 80 to 95%, more preferably 90 to 95%, and most preferably 90%, 92% or 95%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112168750A (en) * | 2020-08-31 | 2021-01-05 | 长春罗兰生物科技有限公司 | Preparation method of ginsenoside extract and application of ginsenoside extract in skin care product |
| CN113913409A (en) * | 2021-10-25 | 2022-01-11 | 抚松县安东参业有限公司 | Compound protease for extracting ginseng extract, preparation method and application process thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112168750A (en) * | 2020-08-31 | 2021-01-05 | 长春罗兰生物科技有限公司 | Preparation method of ginsenoside extract and application of ginsenoside extract in skin care product |
| CN113913409A (en) * | 2021-10-25 | 2022-01-11 | 抚松县安东参业有限公司 | Compound protease for extracting ginseng extract, preparation method and application process thereof |
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Application publication date: 20200421 |