CN101244104B - Method for increasing rare saponin content in panax ginseng total saponin extract - Google Patents
Method for increasing rare saponin content in panax ginseng total saponin extract Download PDFInfo
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- CN101244104B CN101244104B CN2008100505354A CN200810050535A CN101244104B CN 101244104 B CN101244104 B CN 101244104B CN 2008100505354 A CN2008100505354 A CN 2008100505354A CN 200810050535 A CN200810050535 A CN 200810050535A CN 101244104 B CN101244104 B CN 101244104B
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Abstract
The invention provides a method for increasing the rare saponin content in the extraction of total ginsenoside, which adopts the dried root of ginseng as the raw material, wherein, the method comprises the following steps: the ginseng root is degreased, extracted and concentrated with organic reagent, and then is mixed with water and organic reagent, then is put into high-pressure steam cabinet for steaming; the ginseng root after steaming is concentrated, extracted and re-concentrated to obtain the extraction of ginsenoside with high content of rare saponin in the total ginsenoside. The obtained extraction of total ginsenoside has the advantages that the content of rare saponin comprising 20R-Rg3, 20S-Rg3,Rk1 and Rg5 is increased obviously through high-pressure liquid chromatography, wherein, the content of 20R-Rg3, 20S-Rg3,Rk1 and Rg5 is increased by 50 to 100 times than the saponin extraction of common ginseng dried root.
Description
Technical field
The present invention relates to a kind of method that increases rare saponin content in the Radix Ginseng total saponins extract, be specifically related to increase the method for content in Radix Ginseng total saponins such as 20R-Rg3,20S-Rg3, Rk1, Rg5.
Background technology
Ginsenoside 20R-Rg3,20S-Rg3, Rk1, Rg5 are a kind of diol type ginsenosides of containing in the Radix Ginseng.Have very high active anticancer and improving memory activity (list of references: Zhang Jing, Wang Shirong, Chen Quancheng, etc.Ginsenoside Rg3 (R), Rg3 (S), Rg5/Rk1 causes the influence that mouse memory hinders the improvement effect to ethanol.Jilin Agriculture University's journal, 2006,28 (3): 283～284).Owing to do not have Rk1, Rg5 (find out by the Radix Ginseng high-efficient liquid phase chromatogram, see Figure of description: figure one) in the natural ginseng, so how to prepare 20R-Rg3,20S-Rg3 in a large number, Rk1, Rg5 have important researching value and application prospects.
Summary of the invention
The invention provides a kind of method that increases rare saponin content in the Radix Ginseng total saponins extract, be can be directly by the method for the rare saponin 20R-Rg3 of Radix Ginseng dry root powder preparation, 20S-Rg3, Rk1, Radix Ginseng total saponins extract that Rg5 content is high.Its step and condition are as follows:
The Radix Ginseng dry root is processed into powder, add chloroform, petroleum ether or ether organic solvent, carry out defat with apparatus,Soxhlet's, chloroform, the volume of petroleum ether or ether (milliliter): the proportioning of Radix Ginseng dry root powder quality (gram) is 10-100, extraction time is 3 hours, extract the end hypsokinesis and go out chloroform, petroleum ether or ether, residue extracts with the n-butyl alcohol saturation water, n-butyl alcohol water saturation liquor capacity (milliliter): Radix Ginseng powder quality (gram) is 10-100, carry out ultrasonic extraction, extraction conditions is: power is at 300W to 500W, temperature is 20 ℃ to 50 ℃, extraction time is 0.5 hour to 2 hours, extract and finish after-filtration, the filtrate evaporate to dryness, residue water suspendible, the volume of water is (milliliter): the quality of Radix Ginseng powder (gram) is 10-100, in suspension, add glacial acetic acid solution again, the volume of glacial acetic acid (milliliter): the quality of Radix Ginseng powder (gram) is 4-20, putting into steaming ginseng case steams, steaming temperature is 120 ℃ to 130 ℃, steaming time is 1 hour to 6 hours, after steaming end suspension solution is taken out, concentrate, be concentrated into and steam 1/5th of preceding suspension solution volume, suspension solution after concentrating extracts with the n-butyl alcohol saturated aqueous solution, and the adding volume (milliliter) of n-butyl alcohol saturated aqueous solution: the quality of Radix Ginseng powder (gram) is 30-100, after extraction finishes, reclaim under reduced pressure n-butyl alcohol saturated aqueous solution obtains containing saponin 20R-Rg3,20S-Rg3, Rk1, the ginsenoside extract of Rg5.
Utilize high pressure liquid chromatography, measure the content of 20R-Rg3 in the total saponins, 20S-Rg3, Rk1, Rg5 by chromatographic peak area.
Have a mind to effect: the invention provides a kind of method that increases rare saponin 20R-Rg3,20S-Rg3, Rk1, Rg5 content in the Radix Ginseng total saponins, can get rare saponin 20R-Rg3,20S-Rg3, Rk1, ginsenoside extract that Rg5 content is very high.Wherein the Radix Ginseng total saponins of Huo Deing passes through high pressure liquid chromatographic analysis, and the content of 20R-Rg3,20S-Rg3 increases 20-50 doubly than general Radix Ginseng dry root in the Radix Ginseng total saponins.And produced the Rk1, the Rg5 that do not have in the Radix Ginseng dry root, the method is convenient, efficient, easy operating, and with low cost, can satisfy the development and utilization of medicine, field of food, uses, exploitation is worth greatly.
Description of drawings
Fig. 1 utilizes the high-efficient liquid phase chromatogram of the total saponin extracts of conventional method preparation for the Radix Ginseng dry root.Wherein the content of 20R-Rg3 is considerably less, and does not find the chromatographic peak of 20S-Rg3, Rk1, Rg5
Fig. 2 is the high-efficient liquid phase chromatogram that utilizes the Radix Ginseng total saponins extract of method preparation provided by the invention.(20S)-Rg as can be seen
3With (20R)-Rg
3Content significantly improve Rg wherein
3Content increase by 20～50 times than general Radix Ginseng dry root, and obtained the Rk1, the Rg5 that do not have in the Radix Ginseng dry root.
1,2,3, No. 4 chromatographic peak is represented monomer saponin: 20S-Rg3,20R-Rg3, Rk1, Rg5 respectively in the high-efficient liquid phase chromatogram of Fig. 1 and Fig. 2.
The specific embodiment
Add 2 gram Radix Ginseng dry root powder in 50 milliliters of chloroforms, carry out defat reaction 3 hours with apparatus,Soxhlet's, incline and residue is carried out ultrasonic extraction with 50 milliliters of water-saturated n-butanols after chloroform, at 500 watts, supersound extraction is 1 hour under 30 ℃ the condition, extract and finish after-filtration, with the filtrate evaporate to dryness, residue is with 50 ml water suspendibles, add 10 milliliters of glacial acetic acid solutions in the suspension, aqueous suspension is put into high temperature steam the ginseng case and steam, under 120 ℃ condition, steam 1 hour, suspension solution is taken out after steaming end, suspension solution is concentrated into 20 milliliters, with the saturated butanol solution extraction of 100 ml waters, coextraction three times, three times water-saturated n-butanol consumption is respectively 30 milliliters, 30 milliliters, 40 milliliters.Extraction finishes back reclaim under reduced pressure n-butyl alcohol, residue with 9 ml methanol and 1 milliliter of pyridine standardize solution in 10 milliliters volumetric flask, shake up, can get the ginsenoside extract that 20R-Rg3,20S-Rg3, Rk1, Rg5 content significantly improve, wherein 20R-Rg3,20S-Rg3 are respectively than having increased by 55,85 times in common people's conopsea extraction.These two kinds of monomer saponins of Rk1, Rg5 are newly-generated chemical compound.
Embodiment 2
Add 2 gram Radix Ginseng dry root powder in 100 milliliters of chloroforms, carry out defat reaction 3 hours with apparatus,Soxhlet's, incline and residue is carried out ultrasonic extraction with 50 milliliters of water-saturated n-butanols after chloroform, at 500 watts, supersound extraction is 40 minutes under 30 ℃ the condition, extract and finish after-filtration, with the filtrate evaporate to dryness, residue is with 70 ml water suspendibles, add 20 milliliters of glacial acetic acid solutions in the suspension, aqueous suspension is put into high temperature steam the ginseng case and steam, under 125 ℃ condition, steam 1.5 hours, suspension solution is taken out after steaming end, suspension solution is concentrated into 20 milliliters, with the saturated butanol solution extraction of 120 ml waters, coextraction three times, three times water-saturated n-butanol consumption is respectively 40 milliliters, 40 milliliters, 40 milliliters.Extraction finishes back reclaim under reduced pressure n-butyl alcohol, residue with 9 ml methanol and 1 milliliter of pyridine standardize solution in 10 milliliters volumetric flask, shake up, can get the ginsenoside extract that 20R-Rg3,20S-Rg3, Rk1, Rg5 content significantly improve, wherein 20R-Rg3,20S-Rg3 have increased by 50,100 times than 20R-Rg3,20S-Rg3 in ordinary people's conopsea extraction respectively.These two kinds of monomer saponins of Rk1, Rg5 are newly-generated chemical compound.
Add 2 gram Radix Ginseng dry root powder in 100 milliliters of chloroforms, carry out defat reaction 3 hours with apparatus,Soxhlet's, incline and residue is carried out ultrasonic extraction with 100 milliliters of water-saturated n-butanols after chloroform, at 500 watts, supersound extraction is 60 minutes under 30 ℃ the condition, extract and finish after-filtration, with the filtrate evaporate to dryness, residue is with 70 ml water suspendibles, add 15 milliliters of glacial acetic acid solutions in the suspension, aqueous suspension is put into high temperature steam the ginseng case and steam, under 125 ℃ condition, steam 2 hours, suspension solution is taken out after steaming end, suspension solution is concentrated into 20 milliliters, with the saturated butanol solution extraction of 90 ml waters, coextraction three times, three times water-saturated n-butanol consumption is respectively 30 milliliters, 30 milliliters, 30 milliliters.Extraction finishes back reclaim under reduced pressure n-butyl alcohol, residue with 9 ml methanol and 1 milliliter of pyridine standardize solution in 10 milliliters volumetric flask, shake up, can get the ginsenoside extract that 20R-Rg3,20S-Rg3, Rk1, Rg5 content significantly improve, wherein 20R-Rg3,20S-Rg3 are respectively than having increased by 60,75 times in the common extract of Radix Ginseng.These two kinds of monomer saponins of Rk1, Rg5 are newly-generated chemical compound.
Embodiment 4
Add 2 gram Radix Ginseng dry root powder in 150 milliliters of chloroforms, carry out defat reaction 3 hours with apparatus,Soxhlet's, incline and residue is carried out ultrasonic extraction with 50 milliliters of water-saturated n-butanols after chloroform, at 400 watts, supersound extraction is 50 minutes under 30 ℃ the condition, extract and finish after-filtration, with the filtrate evaporate to dryness, residue is with 150 ml water suspendibles, add 20 milliliters of glacial acetic acid solutions in the suspension, aqueous suspension is put into high temperature steam the ginseng case and steam, under 125 ℃ condition, steam 6 hours, suspension solution is taken out after steaming end, suspension solution is concentrated into 20 milliliters, with the saturated butanol solution extraction of 150 ml waters, coextraction three times, three times water-saturated n-butanol consumption is respectively 50 milliliters, 50 milliliters, 50 milliliters.Extraction finishes back reclaim under reduced pressure n-butyl alcohol, residue with 9 ml methanol and 1 milliliter of pyridine standardize solution in 10 milliliters volumetric flask, shake up, can get the ginsenoside extract that 20R-Rg3,20S-Rg3, Rk1, Rg5 content significantly improve, wherein 20R-Rg3,20S-Rg3 have increased by 55,70 times than ordinary people's conopsea extraction respectively.These two kinds of monomer saponins of Rk1, Rg5 are newly-generated chemical compound.
Claims (1)
1. method that increases rare saponin content in the Radix Ginseng total saponins extract, it is characterized in that, step and condition are as follows: the Radix Ginseng dry root is processed into powder, add chloroform, carry out defat with apparatus,Soxhlet's, the milliliter number of the volume of chloroform: the proportioning of the gram number of Radix Ginseng dry root powder quality is 10-100, extraction time is 3 hours, extract the end hypsokinesis and go out chloroform, residue extracts with the n-butyl alcohol saturation water, the milliliter number of n-butyl alcohol water saturation liquor capacity: the gram number of Radix Ginseng powder quality is 10-100, carry out ultrasonic extraction, extraction conditions is: power is at 300W to 500W, temperature is 20 ℃ to 50 ℃, extraction time is 0.5 hour to 2 hours, extract and finish after-filtration, the filtrate evaporate to dryness, residue water suspendible, the milliliter number of the volume of water: the gram number of the quality of Radix Ginseng powder is 10-100, in suspension, add glacial acetic acid solution again, the milliliter number of the volume of glacial acetic acid: the gram number of the quality of Radix Ginseng powder is 4-20, putting into steaming ginseng case steams, steaming temperature is 120 ℃ to 130 ℃, steaming time is 1 hour to 6 hours, steams after the end suspension solution is taken out, and concentrates, be concentrated into and steam 1/5th of preceding suspension solution volume, suspension solution after concentrating extracts with the n-butyl alcohol saturated aqueous solution, and the milliliter number of the adding volume of n-butyl alcohol saturated aqueous solution: the gram number of the quality of Radix Ginseng powder is 30-100, after extraction finishes, reclaim under reduced pressure n-butyl alcohol saturated aqueous solution obtains containing saponin 20R-Rg3,20S-Rg3, Rk1, the ginsenoside extract of Rg5.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101928671B (en) * | 2009-12-03 | 2012-07-25 | 延边大学 | Alternaria spp and method thereof for preparing ginsenoside Rg3 from fermented ginseng stem-leaf total saponin |
| KR101359078B1 (en) | 2011-03-08 | 2014-02-05 | 이홍식 | Method of processing roots of wild ginseng |
| KR101260047B1 (en) * | 2012-05-25 | 2013-05-06 | 한국과학기술연구원 | Panax spp. plant extract with increased content ratio of ginsenoside rg3, rg5 and rk1 produced by microwave irradiation, a process for the preparation thereof, and a composition comprising the same |
| CN102973623A (en) * | 2012-12-20 | 2013-03-20 | 刘淑莹 | Separation method of ginseng rare saponins in ginseng fibrils |
| CN104324062A (en) * | 2014-11-26 | 2015-02-04 | 任贵兴 | American ginseng conversion saponin, traditional Chinese medicine mouth care composition thereof and preparation method and application |
| CN105601694B (en) * | 2016-03-16 | 2018-11-06 | 吉林省彩森仁生物科技有限责任公司 | A method of extraction ginsenoside Rg 5 |
| CN106109482A (en) * | 2016-07-29 | 2016-11-16 | 陕西巨子生物技术有限公司 | A kind of glycol group rare ginsenoside compositions with anti-tumor activity |
| CN106360715B (en) * | 2016-09-08 | 2020-07-10 | 刘廷强 | A method for processing Ginseng radix Rubri product |
| CN110403967B (en) * | 2019-06-13 | 2022-05-10 | 康美（北京）药物研究院有限公司 | A method for increasing ginsenoside Rg3、Rh2Method for processing ginseng with high content, processed ginseng obtained by the method and application of the processed ginseng |
| CN112656828B (en) * | 2020-09-29 | 2023-09-19 | 吉林瑞诺科技有限公司 | Pseudo-ginseng leaf product |
| CN112876528A (en) * | 2021-01-15 | 2021-06-01 | 吉林农业大学 | Method for obtaining ginsenoside |
| CN114869925A (en) * | 2022-04-29 | 2022-08-09 | 中国药科大学 | Ginseng radix Rubri processing method for increasing content of rare saponins in Ginseng radix |
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