CN108126000B - Method for extracting and preparing panax notoginseng saponins from fresh panax notoginseng - Google Patents
Method for extracting and preparing panax notoginseng saponins from fresh panax notoginseng Download PDFInfo
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Abstract
The invention discloses a method for extracting and preparing panax notoginseng saponins from fresh panax notoginseng. The method takes fresh pseudo-ginseng as a raw material, adds ethanol into the fresh pseudo-ginseng for homogenization, filters, concentrates until no alcohol smell exists, adds macroporous adsorption resin, refines, decolors by active carbon, and dries to obtain a target product. The invention adopts fresh panax notoginseng as raw material for extraction, improves the yield of panax notoginseng saponins by a homogenate method, improves the content of each component of the panax notoginseng saponins by cold-leaching extraction, and reduces the loss of the panax notoginseng saponins in the drying process, the crushing process and the high-temperature reflux extraction process of the panax notoginseng. The method is simple and can be widely applied to the industrial production of the panax notoginseng saponins.
Description
Technical Field
The invention relates to a method for extracting and preparing panax notoginseng saponins from fresh panax notoginseng, belonging to the technical field of extraction and preparation of plant active ingredients.
Background
Pseudo-ginseng is a traditional and rare Chinese medicinal material, is a dried root and rhizome of Panax notoginseng (Burk.) F.H.Chen in Araliaceae, has the effects of stopping bleeding and enriching blood, dredging collaterals and removing blood stasis, reducing swelling and relieving pain, and regulating blood sugar and blood fat in two directions, and is mainly produced in Yunnan Wenshan, so that the pseudo-ginseng is named as Wenshan and the pseudo-ginseng is named as Wenshan. The pseudo-ginseng comprises the following main components: notoginseng radix total saponin, dencichine, flavone, Notoginseng radix polysaccharide, volatile oil, etc. Wherein the main effective component is panax notoginseng saponins, the content of the total saponins (PNS) can reach 12 percent, and the panax notoginseng saponins comprise the following main components: ginsenoside Rb1, ginsenoside Rg1, notoginsenoside R1, etc. The panax notoginseng saponins have wide application, and are mainly applied to medicaments and health care products for treating cardiovascular and cerebrovascular diseases, such as 'Xuesaitong' and 'Compound Danshen dripping pills', the main medicinal active component of the panax notoginseng saponins is the panax notoginseng saponins. At present, the extraction rate of panax notoginseng saponins in production is low, and the influence factors are as follows:
(1) influence of drying mode and drying temperature on Notoginseng radix total saponin content in fresh Notoginseng radix drying process. The drying mode of fresh pseudo-ginseng is natural airing and drying in a drying room. The long time for natural drying and the high temperature of the drying room can affect the content of the panax notoginseng saponins and cause the loss of the panax notoginseng saponins.
(2) Influence of mechanical pulverization on extraction yield and content of Panax notoginsenosides. The raw medicinal materials for extracting the panax notoginseng saponins are basically dry medicinal materials, and are crushed before feeding. The mechanical temperature is increased by long-time pulverization, so that the Panax notoginsenosides are chemically changed and inactivated. In addition, the non-uniform pulverization often results in low dissolution rate of some large-sized drugs, which affects the yield and content of panax notoginseng saponins.
(3) The influence of the extraction method on the extraction yield and content of the panax notoginseng saponins.
The method for extracting the panax notoginseng saponins mainly comprises the following steps: water decoction, alcohol reflux, percolation, ultrasonic extraction, etc. The method and the technology are mature, but the extraction rate is not high because of the following reasons: a. the panax notoginseng contains a large amount of starch, is easy to gelatinize in a hot water and ethanol system, causes high impurity content, brings difficulties to subsequent separation and purification, and is also easy to cause low content or purity of panax notoginseng saponins; b. the alcohol reflux extraction solvent has large consumption, many times of extraction, long heating and concentrating time, and the panax notoginseng saponins as heat-sensitive substances are easy to inactivate, so that the yield and the content are low.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for extracting and preparing panax notoginseng saponins from fresh panax notoginseng, which is used for solving the problems that the panax notoginseng saponins are easy to inactivate, the impurity content is high, and the purity of the panax notoginseng saponins is low.
The technical scheme adopted by the invention is as follows:
1. the method for extracting and preparing the panax notoginseng saponins from the fresh panax notoginseng is characterized by comprising the following steps:
(1) adding 8-10 times of 75% ethanol into fresh Notoginseng radix, homogenizing, standing for 12-24 hr, filtering to obtain filtrate I, adding 5-8 times of 75% ethanol into residue, homogenizing, standing for 12-24 hr, filtering to obtain filtrate II, mixing filtrate I and II, and vacuum filtering to obtain clear filtrate;
(2) concentrating the filtrate at-0.08 Mpa at a temperature of less than or equal to 60 deg.C until no alcohol smell exists to obtain concentrated solution;
(3) diluting the concentrated solution with 5-8 times of water, adding 5-8 times of water, washing with water, adding 6-8 times of ethanol for flushing glycoside, passing ethanol eluate through decolorizing resin, concentrating until no alcohol smell exists, adding 2-3 times of ethanol, adding 3-6% of activated carbon, refluxing for 15-30min for decolorizing, vacuum filtering, and concentrating until the specific gravity of the extract is 1.13-1.20 to obtain target product;
(4) vacuum drying the target product at a temperature of less than or equal to 60 ℃ to obtain the panax notoginseng saponins.
2. The method for extracting and preparing panax notoginseng saponins from fresh panax notoginseng as described in the technical scheme 1 is characterized in that: the panax notoginseng saponins in the step (3) are more than 88.0 percent, and the yield is higher than 3.5 percent.
3. The method for extracting and preparing panax notoginseng saponins from fresh panax notoginseng as described in the technical scheme 1 is characterized in that: the macroporous adsorption resin is D101 or AB-8 macroporous adsorption resin.
4. The method for extracting and preparing panax notoginseng saponins from fresh panax notoginseng as described in the technical scheme 1 is characterized in that: the ethanol concentration in the ethanol eluent in the step (3) is 70-85% v/v.
5. The method for extracting and preparing panax notoginseng saponins from fresh panax notoginseng as described in the technical scheme 1 is characterized in that: and (3) the concentration of ethanol for decoloring the activated carbon is 95% ethanol v/v.
6. A method for extracting and preparing panax notoginseng saponins from fresh panax notoginseng is characterized by comprising the following steps:
(1) adding 75% v/v ethanol which is 8-10 times of the weight of fresh pseudo-ginseng into fresh pseudo-ginseng, homogenizing, standing for 12-24h, filtering to obtain a filtrate I, adding 75% v/v ethanol which is 5-8 times of the weight of filter residue into filter residue, homogenizing, standing for 12-24h, filtering to obtain a filtrate II, combining the filtrate I and the filtrate II, and performing suction filtration until the filtrate is clear to obtain a filtrate III;
(2) concentrating the filtrate III at a temperature of less than or equal to 60 deg.C and 0.08Mpa until no alcohol smell exists to obtain concentrated solution I;
(3) adding water which is 5-8 times of the weight of the concentrated solution I into the concentrated solution I to dilute the concentrated solution I, adding water which is 5-8 times of the weight of fresh pseudo-ginseng into the concentrated solution I, washing the concentrated solution I with water, adding 70% -85% v/v ethanol which is 6-8 times of the weight of the fresh pseudo-ginseng into the concentrated solution I to wash the solution I to obtain ethanol eluent, concentrating the ethanol eluent after passing through decolorizing resin until no alcohol smell exists to obtain concentrated solution II, adding 95% ethanol v/v ethanol which is 2-3 times of the weight of the concentrated solution II into the concentrated solution II, adding 3% -6% active carbon which is 3% -6% of the weight of the fresh pseudo-ginseng into the concentrated solution II, refluxing the mixture for 15-30min to decolorize, performing suction filtration;
(4) vacuum drying the target product at a temperature of less than or equal to 60 deg.C to obtain Notoginseng radix total saponin.
7. The method for extracting and preparing panax notoginseng saponins from fresh panax notoginseng according to claim 6, which is characterized in that: the macroporous adsorption resin in the step (3) is D101 macroporous adsorption resin or AB-8 macroporous adsorption resin.
8. The method for extracting and preparing panax notoginseng saponins from fresh panax notoginseng according to any one of claims 6 to 8, wherein the method comprises the following steps: before extracting notoginsenoside from fresh radix Notoginseng, slicing fresh radix Notoginseng, immersing in 75% v/v ethanol, sealing, and storing.
When the method is used for elution, water washing is firstly carried out, then alcohol washing is carried out, so that water-soluble substances such as polysaccharide can be removed by water washing, and then alcohol is used for eluting the panax notoginseng saponins so as to achieve the purpose of separation and purification; the reflux time is short during color removal, so that the effective components are not damaged.
The invention adopts the fresh panax notoginseng as the raw material for extracting the panax notoginseng saponins, avoids the component loss caused by the drying process, the crushing process and the reflux extraction process by taking the fresh panax notoginseng as the raw material, and can reserve the total component content of the panax notoginseng saponins to the maximum extent. The technicians in the field generally do not adopt fresh pseudo-ginseng as an extraction raw material, and are not only limited by production places and time, but also influenced by storage conditions, and the fresh pseudo-ginseng is not easy to store and needs to be preserved in a refrigeration house; in the invention, in order to store fresh pseudo-ginseng conveniently, the fresh pseudo-ginseng can be immersed and sealed by using 75% ethanol for storage after being sliced.
According to the invention, the ethanol is added into the fresh panax notoginseng to be homogenized at normal temperature or low temperature, so that the inactivation of the components of the panax notoginseng saponins caused by high temperature, high starch content and the like, or the low content of the panax notoginseng saponins caused by gelatinization is avoided.
Compared with the prior art, the invention also has the following beneficial effects: the invention directly uses fresh panax notoginseng and ethanol for homogenate extraction, reduces the loss of panax notoginseng saponins in the drying process, the crushing process and the high-temperature reflux extraction process, and determines that the total content of panax notoginseng saponins is more than 90.0 percent, and the content of each component is not lower than the injection content specified in the national formulary.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to the following specific examples, which are not intended to limit the present invention.
Example 1
Taking fresh pseudo-ginseng as a raw material, adding 75% v/v ethanol homogenate of 10 times of the weight of the fresh pseudo-ginseng into the fresh pseudo-ginseng, standing for 24 hours after homogenate, filtering to obtain a filtrate I, adding 75% v/v ethanol homogenate of 8 times of the weight of the filter residue into the filter residue, standing for 24 hours after homogenate, filtering to obtain a filtrate II, combining the filtrate I and the filtrate II, and performing suction filtration until the filtrate is clarified to obtain a filtrate III; concentrating the filtrate III at a temperature of less than or equal to 60 deg.C and 0.08Mpa until no alcohol smell exists to obtain concentrated solution I; adding water with the weight 8 times that of the concentrated solution I into the concentrated solution I to dilute the concentrated solution I, adding water with the weight 8 times that of fresh pseudo-ginseng (namely adding water with the weight 8 times that of the fed material), washing the concentrated solution I with water, adding 75% v/v ethanol with the weight 8 times that of the fresh pseudo-ginseng to flush glycoside to obtain ethanol eluent, concentrating the ethanol eluent after passing through decolorizing resin until no alcohol smell exists to obtain a concentrated solution II, adding 95% v/v ethanol with the weight 3 times that of the concentrated solution II into the concentrated solution II, adding 6% active carbon with the weight (namely the fed material) of the fresh pseudo-ginseng, refluxing for 30min to decolorize, performing suction filtration, and concentrating until the specific gravity of an extract is 1.20 to obtain a target product; vacuum drying the target product at a temperature of less than or equal to 60 deg.C to obtain Notoginseng radix total saponin. The total content of the panax notoginseng saponins is 89.8 percent, and the content of each component is not lower than the content specified in the national formulary for injection.
Example 2
Taking fresh pseudo-ginseng as a raw material, adding 75% v/v ethanol homogenate of 8 times of the weight of the fresh pseudo-ginseng into the fresh pseudo-ginseng, standing for 24 hours after homogenate, filtering to obtain a filtrate I, adding 75% v/v ethanol homogenate of 6 times of the weight of the filter residue into the filter residue, standing for 24 hours after homogenate, filtering to obtain a filtrate II, combining the filtrate I and the filtrate II, and performing suction filtration until the filtrate is clarified to obtain a filtrate III; concentrating the filtrate III at a temperature of less than or equal to 60 deg.C and 0.08Mpa until no alcohol smell exists to obtain concentrated solution I; adding water with the weight 6 times that of the concentrated solution I into the concentrated solution I to dilute the concentrated solution I, adding water with the weight 6 times that of the added material, washing with water, adding 85% v/v ethanol with the weight 6 times that of the added material to flush glycoside to obtain ethanol eluent, concentrating the ethanol eluent after passing through decolorizing resin until no alcohol smell exists to obtain concentrated solution II, adding 95% v/v ethanol with the weight 3 times that of the concentrated solution II into the concentrated solution II, adding activated carbon with the weight 4% of the added material, refluxing for 30min to decolorize, performing suction filtration, and concentrating until the specific gravity of an extract is 1.16 to obtain a target product; vacuum drying the target product at a temperature of less than or equal to 60 deg.C to obtain Notoginseng radix total saponin. The total content of Panax notoginsenosides is 89.4%, and the content of each component is not less than the content specified in the national formulary for injection.
Example 3
Taking fresh pseudo-ginseng as a raw material, adding 75% v/v ethanol homogenate of 8 times of the weight of the fresh pseudo-ginseng into the fresh pseudo-ginseng, standing for 12 hours after the homogenate, filtering to obtain a filtrate I, adding 75% v/v ethanol homogenate of 5 times of the weight of the filter residue into the filter residue, standing for 12 hours after the homogenate, filtering to obtain a filtrate II, combining the filtrate I and the filtrate II, and performing suction filtration until the filtrate is clarified to obtain a filtrate III; concentrating the filtrate III at a temperature of less than or equal to 60 deg.C and 0.08Mpa until no alcohol smell exists to obtain concentrated solution I; adding water with the weight 5 times that of the concentrated solution I into the concentrated solution I to dilute the concentrated solution I, adding water with the weight 5 times that of the added material, washing with water, adding 80% v/v ethanol with the weight 6 times that of the added material, washing to obtain ethanol eluent, concentrating the ethanol eluent after passing through decolorizing resin until no alcohol smell exists to obtain a concentrated solution II, adding 95% v/v ethanol with the weight 3 times that of the concentrated solution II into the concentrated solution II, adding activated carbon with the weight 3% of the added material, refluxing for 20min to decolorize, performing suction filtration, and concentrating until the specific gravity of the extract is 1.13 to obtain a target product; vacuum drying the target product at a temperature of less than or equal to 60 deg.C to obtain Notoginseng radix total saponin. The total content of Panax notoginsenosides is 89.6%, and the content of each component is not less than the content specified in the national formulary for injection.
Example 4
Taking fresh pseudo-ginseng as a raw material, adding 75% v/v ethanol homogenate of which the weight is 10 times that of the fresh pseudo-ginseng into 10.0kg of the fresh pseudo-ginseng, standing for 24 hours after homogenate, filtering to obtain a filtrate I, adding 75% v/v ethanol homogenate of which the weight is 8 times that of the filter residue into the filter residue, standing for 24 hours after homogenate, filtering to obtain a filtrate II, combining the filtrate I and the filtrate II, and performing suction filtration until the filtrate is clarified to obtain a filtrate III; concentrating the filtrate III at a temperature of less than or equal to 60 deg.C and 0.08Mpa until no alcohol smell exists to obtain concentrated solution I; adding water with the weight 8 times that of the concentrated solution I into the concentrated solution I to dilute the concentrated solution I, adding D101 macroporous adsorption resin or AB-8 macroporous adsorption resin, adding water with the weight 8 times that of fresh pseudo-ginseng, washing the mixture with water, adding 80% v/v ethanol with the weight 8 times that of the fresh pseudo-ginseng to wash the mixture to obtain ethanol eluent, concentrating the ethanol eluent after passing through decolorizing resin until no alcohol smell exists to obtain a concentrated solution II, adding 95% v/v ethanol with the weight 3 times that of the concentrated solution II into the concentrated solution II, adding 6% active carbon with the weight of the fresh pseudo-ginseng, refluxing for 30min to decolorize, performing suction filtration, and concentrating until the specific gravity of an extract is 1.20 to obtain a target product; vacuum drying the target product at a temperature of less than or equal to 60 deg.C to obtain 355.7g of Notoginseng radix total saponin. The total content of the panax notoginseng saponins is 90.8 percent, and the content of each component is not lower than the content specified in the national formulary for injection.
Comparative example 1
(1) Taking 10.0kg of fresh pseudo-ginseng medicinal materials, cleaning, airing, air-drying or oven-drying; (2) slicing Notoginseng radix, extracting with 75% v/v ethanol solution, recovering ethanol from the extractive solution, adding water solution 6 times the weight of Notoginseng radix slice, diluting until no obvious oily substance floats, and filtering to obtain clear water solution; (3) putting the clear water solution obtained in the step 2 on a D101 macroporous adsorption resin column, washing for 1 time by using a water solution with the pH value of 4-6, and then eluting by using a 40-80 v% ethanol solution; (4) collecting eluate, recovering ethanol, and concentrating under reduced pressure to dry to obtain white powdered product notoginsenoside 256.5 g.
Comparative example 2
Comparative example 2 the same procedure as in example 4 was followed except that 10.0kg of fresh Panax notoginseng was washed, air-dried or oven-dried, and the air-dried or oven-dried sliced Panax notoginseng was used as the starting material. 277.0g of white powdery product notoginsenoside is obtained.
The results of comparing the contents of panax notoginseng saponins obtained in the comparative example and example 4 are shown in table 1.
TABLE 1 comparative example and example 4
As can be seen from Table 1, the weight of the panax notoginseng saponins obtained in example 4 and the content of the panax notoginseng saponins are higher than those of the comparative examples, and in comparative example 1, the panax notoginseng saponins as heat-sensitive substances are easily inactivated by a heat extraction method, so that the yield and the content are lower, and the panax notoginseng saponins are easily gelatinized in a hot water and ethanol system, so that the impurity content is high. Comparative example 2 is a method for extracting notoginsenoside from sliced fresh notoginseng air-dried or oven-dried, which is the same as in example 4, but in example 4, the fresh notoginseng is used as a raw material to avoid component loss caused by a drying process, a crushing process and a reflux extraction process, so that the yield and the content of each effective component in example 4 are higher than those in comparative example 2 and also higher than those in comparative example 1.
Claims (3)
1. A method for extracting and preparing panax notoginseng saponins from fresh panax notoginseng is characterized by comprising the following steps:
(1) adding 75% v/v ethanol 8-10 times the weight of fresh radix Notoginseng into fresh radix Notoginseng, homogenizing, standing for 12-24 hr, filtering to obtain filtrate I, adding 75% v/v ethanol 5-8 times the weight of filter residue into filter residue, homogenizing, standing for 12-24 hr, filtering to obtain filtrate II, mixing filtrate I and II, and vacuum filtering to obtain filtrate III;
(2) concentrating the filtrate III at a temperature of less than or equal to 60 deg.C and 0.08Mpa until no alcohol smell exists to obtain concentrated solution I;
(3) adding water which is 5-8 times of the weight of the concentrated solution I into the concentrated solution I to dilute the concentrated solution I, adding water which is 5-8 times of the weight of fresh pseudo-ginseng into the concentrated solution I, washing the concentrated solution I with water, adding 70% -85% v/v ethanol which is 6-8 times of the weight of the fresh pseudo-ginseng into the concentrated solution I to wash the solution I to obtain ethanol eluent, concentrating the ethanol eluent after passing through decolorizing resin until no alcohol smell exists to obtain concentrated solution II, adding 95% v/v ethanol which is 2-3 times of the weight of the concentrated solution II into the concentrated solution II, adding 3% -6% of active carbon which is 3% -6% of the weight of the fresh pseudo-ginseng into the concentrated solution II, refluxing the solution II for 15-30min to decolorize, performing suction;
(4) vacuum drying the target product at a temperature of less than or equal to 60 deg.C to obtain Notoginseng radix total saponin.
2. The method for extracting and preparing 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 D101 macroporous adsorption resin or AB-8 macroporous adsorption resin.
3. The method for extracting and preparing panax notoginseng saponins from fresh panax notoginseng according to any one of claims 1 to 2, wherein the method comprises the following steps: before extracting notoginsenoside from fresh radix Notoginseng, slicing fresh radix Notoginseng, immersing in 75% v/v ethanol, sealing, and storing.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102145034A (en) * | 2011-04-14 | 2011-08-10 | 云南文山七丹药业股份有限公司 | Fresh radix notoginseng extract, preparation method and medicinal prescription of fresh radix notoginseng extract |
| CN103565866A (en) * | 2012-07-30 | 2014-02-12 | 昆明制药集团股份有限公司 | Preparation method of panax notoginseng saponins |
| CN104490967A (en) * | 2014-12-06 | 2015-04-08 | 云南云药医药研究有限公司 | High-efficiency high-yield preparation method of panax notoginseng extract |
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| CN102145034A (en) * | 2011-04-14 | 2011-08-10 | 云南文山七丹药业股份有限公司 | Fresh radix notoginseng extract, preparation method and medicinal prescription of fresh radix notoginseng extract |
| CN103565866A (en) * | 2012-07-30 | 2014-02-12 | 昆明制药集团股份有限公司 | Preparation method of panax notoginseng saponins |
| CN104490967A (en) * | 2014-12-06 | 2015-04-08 | 云南云药医药研究有限公司 | High-efficiency high-yield preparation method of panax notoginseng extract |
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