CN111087438A - Preparation method of rare saponins of panax ginseng Rk1 and Rg5 - Google Patents
Preparation method of rare saponins of panax ginseng Rk1 and Rg5 Download PDFInfo
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- CN111087438A CN111087438A CN202010007323.9A CN202010007323A CN111087438A CN 111087438 A CN111087438 A CN 111087438A CN 202010007323 A CN202010007323 A CN 202010007323A CN 111087438 A CN111087438 A CN 111087438A
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Abstract
The invention relates to a preparation method of ginsenosides Rk1 and Rg5, wherein the content of the ginsenosides Rb1 is 12.5-19.4%, the content of the ginsenosides Rb2 is 10.3-13.4%, the content of the ginsenosides Rb3 is 26.1-31.4%, and the content of the ginsenosides Rd is 7.3-13.3%. The method comprises the following steps of preparing ginsenoside by using a macroporous resin column, treating the aqueous solution of ginsenoside acid at ultrahigh pressure, treating at low temperature, centrifuging, heating supernatant at high temperature after precipitation and filtration, centrifuging again to obtain precipitate, and drying the precipitate to obtain high-purity ginsenoside Rk1 and Rg 5.
Description
Technical Field
The invention relates to a method for converting and purifying ginsenoside, in particular to a method for converting and purifying rare ginsenoside Rk1 and Rg 5.
Background
Ginsenoside is a sterol compound, mainly comes from medicinal materials of ginseng, and traditional Chinese medicine considers that ginseng has the effects of greatly invigorating primordial qi, tonifying spleen and lung, promoting the production of body fluid, soothing nerves and improving intelligence, and belongs to a qi-tonifying top product, and the ginsenoside extracted from natural ginseng is more than 40, and has complex pharmacological action. According to the structural types of ginsenosides, ginsenosides are mainly divided into two types: panaxadiol saponins and panaxatriol saponins. At present, people have more researches on the antitumor effect of ginsenoside Rg3 and ginsenoside Rh2 in panaxadiol type, so that no enterprise can produce high-content (> 50%) rare ginsenosides Rg5 and RK1 in large scale even though rare ginsenosides Rg3 and Rh2 are produced in large scale in markets at home and abroad up to now. Therefore, the research on the preparation methods of the two low-polarity rare ginsenosides has important significance for finding ingredients with stronger activity and developing new antitumor drugs.
Disclosure of Invention
The invention aims to provide a method for preparing rare ginsenosides Rg5 and RK1, which has the advantages of simple operation, low production cost, high yield and high purity, through a series of condition optimization: the method comprises the following steps:
(1) extracting ginsenoside from cleaned caulis Et folium Ginseng, passing through macroporous resin column, eluting with 40-55% ethanol water solution, collecting eluate, and drying to obtain ginsenoside extract;
(2) dissolving the ginsenoside extract obtained in the step one with acid water, filling the dissolved ginsenoside extract into a plastic bag, exhausting air, sealing, filling the plastic bag into high-pressure equipment, pressurizing the solution in a high-pressure process, keeping the high pressure for a long time, relieving pressure, and taking out the plastic bag;
(3) heating the high-pressure ginsenoside at 50-60 deg.C for 30-70min, cooling, standing for 3-6 hr, and centrifuging to obtain supernatant and precipitate;
(4) and (3) freeze-drying the precipitate, adding the supernatant obtained in the step (3) into the reaction tank again, heating at 80-100 ℃ for 60-120min, cooling, standing for 1-2h, centrifuging after the precipitate is separated out to obtain supernatant and precipitate, removing the supernatant, and drying the precipitate to obtain the extracts of the ginsenosides Rk1 and Rg5, wherein the purity is 58.5-79.4% through HPLC detection, and the yield is 41.4-52.6%.
Further, the ginsenoside extract obtained in the step one has ginsenoside Rb1 content of 12.5-19.4%, Rb2 content of 10.3-13.4%, Rb3 content of 26.1-31.4%, and Rd content of 7.3-13.3%.
Further, the acid used in the second step is organic acid, the mass fraction of the organic acid is 15-20%, the pressure is 100-400 MPa, and the pressure maintaining time is 50-100 seconds.
The invention has the positive effects that: the technical scheme of the invention has the advantages of simple operation, low cost, shortened reaction period and high purity and yield of the ginsenoside Rk1 and Rg 5.
Drawings
Description of the drawings figure 1 HPLC chromatogram of high content ginsenoside Rk1 and Rg5
Description accompanying drawing 2 high content ginsenoside Rk1 and Rg5 powder diagram
The description refers to the HPLC chromatogram of ginsenoside in the ginsenoside extract obtained in step one of figure 3.
Example 1
(1) Extracting ginsenoside from cleaned caulis Et folium Ginseng, passing through macroporous resin column, eluting with 55% ethanol water solution, collecting eluate, and drying to obtain ginsenoside extract;
(2) dissolving the ginsenoside extract obtained in the step one with acid water, filling the dissolved ginsenoside extract into a plastic bag, exhausting air, sealing, filling the plastic bag into high-pressure equipment, pressurizing the solution in a high-pressure process, keeping the high pressure for a long time, relieving pressure, and taking out the plastic bag;
(3) heating the high-pressure ginsenoside at 500 deg.C for 70min, cooling, standing for 3 hr, and centrifuging to obtain supernatant and precipitate;
(4) and (3) freeze-drying the precipitate, adding the supernatant obtained in the step (3) into the reaction tank again, heating at 100 ℃, heating for 120min, cooling, standing for 2h, centrifuging after precipitation to obtain a supernatant and a precipitate, removing the supernatant, and drying the precipitate to obtain the extracts of the ginsenosides Rk1 and Rg5, wherein the purity of the extracts is 78.2% and the yield is 52.6% as detected by HPLC (high performance liquid chromatography), and the extract is shown in the attached figure 1 and the attached figure 2 of the specification.
Further, the ginsenoside extract obtained in the step one has ginsenoside Rb1 content of 12.5%, Rb2 content of 13.4%, Rb3 content of 31.4% and Rd content of 13.3%, which are shown in figure 3 of the specification.
Further, the acid used in the second step is an organic acid, the mass fraction of the organic acid is 15%, the pressure is 100 MPa, and the pressure holding time is 100 seconds.
Example 2
(1) Extracting ginsenoside from cleaned caulis Et folium Ginseng, passing through macroporous resin column, eluting with 55% ethanol water solution, collecting eluate, and drying to obtain ginsenoside extract;
(2) dissolving the ginsenoside extract obtained in the step one with acid water, filling the dissolved ginsenoside extract into a plastic bag, exhausting air, sealing, filling the plastic bag into high-pressure equipment, pressurizing the solution in a high-pressure process, keeping the high pressure for a long time, relieving pressure, and taking out the plastic bag;
(3) heating the high-pressure ginsenoside at 60 deg.C for 60min, cooling, standing for 4 hr, and centrifuging to obtain supernatant and precipitate;
(4) and (3) freeze-drying the precipitate, adding the supernatant obtained in the step (3) into the reaction tank again, heating at 90 ℃, heating for 60min, cooling, standing for 1h, centrifuging after precipitation to obtain a supernatant and a precipitate, removing the supernatant, and drying the precipitate to obtain the extracts of the ginsenosides Rk1 and Rg5, wherein the purity is 79.4% as detected by HPLC, and the yield is 40.6%.
Further, the ginsenoside extract obtained in the step one has ginsenoside Rb1 content of 12.5%, Rb2 content of 13.4%, Rb3 content of 30.4% and Rd content of 7.3%.
Further, the acid used in the second step is an organic acid, the mass fraction of the organic acid is 15%, the pressure is 300 MPa, and the pressure holding time is 100 seconds.
Claims (3)
1. The preparation method of the rare ginsenoside is characterized by comprising the following steps:
(1) extracting ginsenoside from cleaned caulis Et folium Ginseng, passing through macroporous resin column, eluting with 40-55% ethanol water solution, collecting eluate, and drying to obtain ginsenoside extract;
(2) dissolving the ginsenoside extract obtained in the step one with acid water, filling the dissolved ginsenoside extract into a plastic bag, exhausting air, sealing, filling the plastic bag into high-pressure equipment, pressurizing the solution in a high-pressure process, keeping the high pressure for a long time, relieving pressure, and taking out the plastic bag;
(3) heating the high-pressure ginsenoside at 50-60 deg.C for 30-70min, cooling, standing for 3-6 hr, and centrifuging to obtain supernatant and precipitate;
(4) and (3) freeze-drying the precipitate, adding the supernatant obtained in the step (3) into the reaction tank again, heating at 80-100 ℃ for 60-120min, cooling, standing for 1-2h, centrifuging after the precipitate is separated out to obtain supernatant and precipitate, removing the supernatant, and drying the precipitate to obtain the extracts of the ginsenosides Rk1 and Rg5, wherein the purity is 58.5-79.4% through HPLC detection, and the yield is 41.4-52.6%.
2. The method for preparing rare saponins of panax ginseng Rk1 and Rg5 as claimed in claim 1, wherein the ginsenoside extract obtained in step one contains ginsenoside Rb1 12.5-19.4%, ginsenoside Rb2 10.3-13.4%, ginsenoside Rb3 26.1-31.4%, and ginsenoside Rd 7.3-13.3%.
3. The method for preparing rare saponins of panax ginseng Rk1 and Rg5 as claimed in claim 1, wherein the acid used in the second step is an organic acid, the mass fraction of the organic acid is 15-20%, the pressure is 100 and 400 MPa, and the pressure holding time is 50-100 seconds.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1463980A (en) * | 2002-06-04 | 2003-12-31 | 中国科学院大连化学物理研究所 | Process for preparing panaxoside Rk1 and Rg5 by by panaxadiol type saponins acid hydrolysis |
| CN105968160A (en) * | 2016-05-05 | 2016-09-28 | 杨桂芹 | Method for rapidly preparing highly-active ginseng rare saponins |
| CN107793465A (en) * | 2017-09-22 | 2018-03-13 | 昆明理工大学 | A kind of extracting method and the application of ginsenoside Rg 5 and ginsenoside Rk1 |
| CN108191941A (en) * | 2018-01-12 | 2018-06-22 | 辽宁省荣欣药物研发有限公司 | A kind of preparation method of ginseng sapoglycoside Rg 3 |
| CN108822178A (en) * | 2018-04-13 | 2018-11-16 | 深圳以诺生物制药有限公司 | The preparation method of low polarity rare ginsenoside Rg5/Rk1 and Rh3/Rk2 |
-
2020
- 2020-01-04 CN CN202010007323.9A patent/CN111087438A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1463980A (en) * | 2002-06-04 | 2003-12-31 | 中国科学院大连化学物理研究所 | Process for preparing panaxoside Rk1 and Rg5 by by panaxadiol type saponins acid hydrolysis |
| CN105968160A (en) * | 2016-05-05 | 2016-09-28 | 杨桂芹 | Method for rapidly preparing highly-active ginseng rare saponins |
| CN107793465A (en) * | 2017-09-22 | 2018-03-13 | 昆明理工大学 | A kind of extracting method and the application of ginsenoside Rg 5 and ginsenoside Rk1 |
| CN108191941A (en) * | 2018-01-12 | 2018-06-22 | 辽宁省荣欣药物研发有限公司 | A kind of preparation method of ginseng sapoglycoside Rg 3 |
| CN108822178A (en) * | 2018-04-13 | 2018-11-16 | 深圳以诺生物制药有限公司 | The preparation method of low polarity rare ginsenoside Rg5/Rk1 and Rh3/Rk2 |
Non-Patent Citations (2)
| Title |
|---|
| 关大朋: "高温热裂解人参皂苷Rk1和Rg5的制备工艺优化", 《上海中医药杂志》 * |
| 李伟 等: "人参热裂解皂苷研究进展", 《吉林农业大学学报》 * |
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