CN102973623A - Separation method of ginseng rare saponins in ginseng fibrils - Google Patents

Separation method of ginseng rare saponins in ginseng fibrils Download PDF

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CN102973623A
CN102973623A CN2012105553238A CN201210555323A CN102973623A CN 102973623 A CN102973623 A CN 102973623A CN 2012105553238 A CN2012105553238 A CN 2012105553238A CN 201210555323 A CN201210555323 A CN 201210555323A CN 102973623 A CN102973623 A CN 102973623A
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ginseng
radix ginseng
ethanol
rare
fibrous root
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刘淑莹
吴巍
秦秋杰
郭迎迎
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Abstract

The invention belongs to a method for separating ginseng rare saponins in ginseng fibrils. The method comprises the following steps of: taking fresh ginseng fibrils as raw materials; steaming and machining at a certain temperature; after crushing, heating and reflowing through ethanol with the concentration of 80% to obtain the ginseng rare total saponins; separating and purifying by macro-porous resin and collecting an eluting component of the ethanol with the concentration of 80%; then utilizing methanol to dissolve the eluting component of the ethanol with the concentration of 80% by utilizing the characteristics that the polarity of the rare saponins is small and the solubility difference exits in different solvents; and adding acetone to precipitate to further purify the obtained component to obtain the ginseng rare saponins with the stable component. Through RRLC-Q-TOF-MS detection analysis, the ginseng rare saponins comprise 20(S/R)-Rh1, Rg9, Rg8, F2, Rg6, Rg4, Rk3, Rh4, 20(S/R)-Rg3, 20(S/R)-Rs3, Rk1, Rg5, 20(S/R)-Rh2, Rs5, Rs4, Rk2 and Rh3. The method is low in cost, is simple and fast, is efficient and is easy to operate.

Description

The separation method of the rare saponin group of Radix Ginseng in a kind of fibrous root of Radix Ginseng
Technical field
The invention belongs to a kind of method of from fibrous root of Radix Ginseng, separating the rare saponin group of Radix Ginseng
Background technology
Radix Ginseng ( PanaxGinseng C. A. Meyer) be rare Chinese medicine, the history in existing more than 2,000 year of medication.Its main effective ingredient is the Radix Ginseng saponins compound, has resisting fatigue, slow down aging, adjusting central nervous system, improves immunity of organisms, improves the cardiovascular and cerebrovascular vessel blood supply insufficiency, the effect such as inhibition tumor cell growth.(Liyang etc., Chinese herbal medicine: Vol. 40 (1), and 2009,164-166).Studies show that the some of them rare ginsenoside has good pharmacologically active, more and more cause people's attention.(Zhao Liya etc., Journal of Dalian Institute of Light: Vol. 21 (2), 2002,112-115; Zhang Chunzhi etc., food and fermentation industries: Vol. 28 (4), and 2002,70-74) wherein rare ginsenoside Rg3, Rh2 have stronger active anticancer (Kimys, The International Journal of Biochemistry; Cell Biology, 30 (3): 340 – 341 (1998)).But the rare saponin of Radix Ginseng natural content in Radix Ginseng is extremely low, and content only accounts for ten thousand/to 5/10000ths, and separate difficult, yield poorly.The ginsenoside who has the scholar to separate enzymatic conversion by silicagel column obtain the rare saponin of Radix Ginseng (Tong Qingxuan etc., research and development of natural products: Vol. (6), 2009,1039-1044).The method can only obtain single rare saponin, and method is complicated, time-consuming, and separating needs to use a large amount of organic reagents.Song Changchun etc. mix the alcoholic solution of the low alcoholates of the aqueous solution of protopanoxadiol saponins and alkali metal or metal hydroxides under high-temperature and high-pressure conditions and extract with lower alcohol after reacting again.The method condition more complicated and rare saponin kind less (Song Changchun etc., Chinese patent: 98100297.8,2002-9-25).The Korea S scholar is by direct alkaline hydrolysis Folium Ginseng, afterwards by column chromatography for separation obtain the rare saponin of Radix Ginseng (CHA BC, Yakhak Hoechi:Vol. 38 (4), 1994,425-429.), the method impurity is very many, and the later stage purge process is complicated.Therefore, improve in the urgent need to the extraction separation to the rare saponin of Radix Ginseng at present.Because Radix Ginseng is expensive, it is higher to extract the saponin cost from Radix Ginseng, has the research and utilization fibrous root of Radix Ginseng to extract the ginsenoside.Fibrous root of Radix Ginseng is ramuscule root or the fibrous root of Radix Ginseng, and price generally only is the 1/l0~1/2 of Radix Ginseng, and the content of its total saponins generally is higher than the content of saponin in the Radix Ginseng main root, is about 4%.(Sun Hongxiang, Chinese veterinarian's medical magazine: Vol. (2), 2001,6-8).And when utilizing Radix Ginseng to produce the ginseng product such as Radix Ginseng Rubra, fibrous root of Radix Ginseng is often given it up.There is no at present the report that from fibrous root of Radix Ginseng, separates the rare saponin of Radix Ginseng.
Summary of the invention
The object of the invention provides a kind of method of separating the rare saponin group of Radix Ginseng from fibrous root of Radix Ginseng.
With the fresh ginseng fibrous root, be under 125 ℃ the condition, in steaming the ginseng case, to steam processing 9.5 hours in temperature, when naturally cooling to temperature and being 70 ℃, with fibrous root of Radix Ginseng take out pulverize for subsequent use.Extract 2 times each 1.5 hours with 10 times of amounts (W/V), 80% alcohol heating reflux.After Recycled ethanol was extremely done, lyophilizing obtained the thick total saponins of fibrous root of Radix Ginseng.Then by the separation and purification of D101 macroporous resin, use first the water elution of 8 times of column volumes, use respectively again 50% ethanol, 80% ethanol elution of 8 times of column volumes, collect 80% ethanol elution component.Utilize afterwards rare saponin polarity little, the dissolubility difference in different solvents is further purified the acquisition component.Behind collected 80% ethanol elution component solvent evaporate to dryness, use the dissolve with methanol sample, add 20 times of amount acetone precipitations, staticly settle 2-4 hour, cross the leaching supernatant, solvent evaporated namely gets the rare saponin group of Radix Ginseng of stable components.Detect analysis through RRLC-Q-TOF-MS, the rare saponin group of Radix Ginseng comprises 20 (S/R)-R H1, R G9, R G8, F 2, R G6, R G4, R K3, R H4, 20 (S/R)-R G3, 20 (S/R)-R S3, R K1, R G5, 20 (S/R)-R H2, R S5, R S4, R K2, R H3
This method takes full advantage of fibrous root of Radix Ginseng, and after it was simply steamed, by 80% ethanol extraction, the separation and purification of D101 macroporous resin, separated from solvent, separation and purification had gone out the rare saponin group of Radix Ginseng of stable components, and productive rate is more than 4.68%.The method cost is low, simple and efficient, efficient, easy to operate.
Description of drawings
Accompanying drawing 1 is the RRLC-Q-TOF-MS total ion current figure of the thick total saponin extracts of fibrous root of Radix Ginseng.The thick total saponins composition of fibrous root of Radix Ginseng is more as seen from the figure, comprises common ginsenoside and rare ginsenoside.
Accompanying drawing 2 is the RRLC-Q-TOF-MS total ion current figure of the rare saponin group of Radix Ginseng after separating.By analysis, comprise 20 (S/R)-R H1, R G9, R G8, F 2, R G6, R G4, R K3, R H4, 20 (S/R)-R G3, 20 (S/R)-R S3, R K1, R G5, 20 (S/R)-R H2, R S5, R S4, R K2, R H3The mixture of rare saponin does not comprise common ginsenoside, illustrates that separation is more complete, obtains the rare saponin group of Radix Ginseng of stable components, and productive rate is higher.
The specific embodiment
Embodiment 1:
Be under 125 ℃ the condition, in steaming the ginseng case, to steam processing 9.5 hours in temperature with 1500 gram fresh ginseng fibrous roots, when naturally cooling to temperature and being 70 ℃, with fibrous root of Radix Ginseng take out pulverize for subsequent use.Adding concentration of volume percent is 80% ethanol, and addition is 10 times of amounts (W/V) of quality of medicinal material, 85 ° of C heating and refluxing extraction 2 times, each 1.5 hours.Extracting solution decompression is steamed ethanol after do, and lyophilizing obtains thick total saponins 53.7 grams of fibrous root of Radix Ginseng.Separate with the D101 macroporous resin column, use first the water elution of 8 times of column volumes, use respectively again 50% ethanol, 80% ethanol elution of 8 times of column volumes, collect 80% ethanol elution.Behind collected 80% ethanol elution component solvent evaporate to dryness, use the dissolve with methanol sample, add 20 times of amount acetone precipitations, staticly settle 2-4 hour, cross the leaching supernatant, solvent evaporated, the rare saponin group of the Radix Ginseng 0.7g(yield that namely gets stable components is 4.68%).Utilize RRLC-Q-TOF-MS to detect, the rare saponin composition of Radix Ginseng divides as shown in Figure 2, does not contain common ginsenoside.
Embodiment 2:
Be under 125 ℃ the condition, in steaming the ginseng case, to steam processing 9.5 hours in temperature with 3000 gram fresh ginseng fibrous roots, when naturally cooling to temperature and being 70 ℃, with fibrous root of Radix Ginseng take out pulverize for subsequent use.Adding concentration of volume percent is 80% ethanol, and addition is 10 times of amounts (W/V) of quality of medicinal material, 85 ° of C heating and refluxing extraction 2 times, each 1.5 hours.The extracting solution decompression is steamed ethanol to doing, and lyophilizing obtains thick total saponins 107.4 grams of fibrous root of Radix Ginseng.Separate with the D101 macroporous resin column, use first the water elution of 8 times of column volumes, use respectively again 50% ethanol, 80% ethanol elution of 8 times of column volumes, collect 80% ethanol elution.Behind collected 80% ethanol elution component solvent evaporate to dryness, use the dissolve with methanol sample, add 20 times of amount acetone precipitations, staticly settle 2-4 hour, cross the leaching supernatant, solvent evaporated, the rare saponin group of the Radix Ginseng 1.4g(yield that namely gets stable components is 4.68%).Utilize RRLC-Q-TOF-MS to detect, the rare saponin composition of Radix Ginseng divides as shown in Figure 2, does not contain common ginsenoside.

Claims (7)

1. a method of separating the rare saponin group of Radix Ginseng from fibrous root of Radix Ginseng is characterized in that, take the fresh ginseng fibrous root as raw material, be under 125 ℃ the condition in temperature, in steaming the ginseng case, steam processing 9.5 hours, when naturally cooling to temperature and being 70 ℃, with fibrous root of Radix Ginseng take out pulverize for subsequent use.
2. extract 2 times each 1.5 hours with 10 times of amounts (W/V), 80% alcohol heating reflux.
3. Recycled ethanol is to doing, and lyophilizing obtains the thick total saponins of fibrous root of Radix Ginseng.
4. then by the separation and purification of D101 macroporous resin, use first the water elution of 8 times of column volumes, use respectively again 50% ethanol, 80% ethanol elution of 8 times of column volumes, collect 80% ethanol elution component.
5. utilize afterwards rare saponin polarity little, the dissolubility difference in different solvents is further purified the acquisition component.
6. with behind the collected 80% ethanol elution component solvent evaporate to dryness, use the dissolve with methanol sample, add 20 times of amount acetone precipitations, staticly settle 2-4 hour, cross the leaching supernatant, solvent evaporated namely gets the rare saponin group of Radix Ginseng of stable components.
7. detect through RRLC-Q-TOF-MS and analyze, the rare saponin group of Radix Ginseng comprises 20 (S/R)-R H1, R G9, R G8, F 2, R G6, R G4, R K3, R H4, 20 (S/R)-R G3, 20 (S/R)-R S3, R K1, R G5, 20 (S/R)-R H2, R S5, R S4, R K2, R H3
CN2012105553238A 2012-12-20 2012-12-20 Separation method of ginseng rare saponins in ginseng fibrils Pending CN102973623A (en)

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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
CN105769891A (en) * 2016-04-12 2016-07-20 深圳以诺生物制药有限公司 Low-polarity rare ginsenoside mixture and application thereof
CN110314174A (en) * 2018-03-28 2019-10-11 长春中医药大学 A kind of red ginseng extract and preparation method with anti-aging effects

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN105769891A (en) * 2016-04-12 2016-07-20 深圳以诺生物制药有限公司 Low-polarity rare ginsenoside mixture and application thereof
CN105769891B (en) * 2016-04-12 2018-08-03 深圳以诺生物制药有限公司 Low polarity rare ginsenoside mixture and application thereof
CN110314174A (en) * 2018-03-28 2019-10-11 长春中医药大学 A kind of red ginseng extract and preparation method with anti-aging effects

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Application publication date: 20130320