CN1895313A - Extraction of total saponin from ginseng or American ginseng stem/leaf and its product - Google Patents
Extraction of total saponin from ginseng or American ginseng stem/leaf and its product Download PDFInfo
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- CN1895313A CN1895313A CN 200510082778 CN200510082778A CN1895313A CN 1895313 A CN1895313 A CN 1895313A CN 200510082778 CN200510082778 CN 200510082778 CN 200510082778 A CN200510082778 A CN 200510082778A CN 1895313 A CN1895313 A CN 1895313A
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Abstract
A process for extracting the gensinoside from the stem and/or leaf of ginseng or American ginseng includes such steps as ordinary-pressure extracting to obtain liquid extract, alkalizing, laying aside, filtering, flowing through H-type cationic adsorptive resin column, washing the resin column by water, stripping the resin column by alcohol to obtain the stripped liquid, desalting, decoloring, recovering alcohol, concentrating and drying. The content of ginsenoside in the product is more than 85%.
Description
Technical field
The present invention relates to extract method of total Saponin and products thereof by Radix Ginseng or Radix Panacis Quinquefolii stem/leaf, more particularly, is a kind of method of utilizing resin method suitability for industrialized production Radix Ginseng or total panaquilon and products thereof.
Background technology
As everyone knows, Radix Ginseng total saponins and total panaquilon are very ideal pure natural medicals.Show that through pharmacological testing it has obvious anti-fatigue, diuresis, oxygen lack resistant function, and nervous system is had Accommodation, ischemic myocardial cells and carbon tetrachloride damage are had protective effect, and the immunologic function of human body is had facilitation preferably.Find that in the clinical test of pesticide effectiveness Radix Ginseng total saponins and total panaquilon also have good curative effect to treatment neurasthenia, autonomic nervous dysfunction, climacteric syndrome.
Prove that through pharmacological research the total Saponin that extracts from Radix Ginseng or Radix Panacis Quinquefolii aerial parts has similar pharmacological action to total Saponin that its root is extracted, and all is the distinctive effective ingredient of Radix Ginseng, can be used as the natural drug of strengthening the body resistance.
By the distinctive effective ingredient-Radix Ginseng total saponins of Radix Ginseng that the Radix Ginseng aerial parts extracts, formal from 1981 by since country's evaluation, more existing so far manufacturer production Radix Ginseng total saponins extracts.This drug resource is extensive use of by fields such as medicine, health product, beverage and daily cosmetics.
The production technology of Radix Ginseng total saponins or total panaquilon has been taken advantage of two methods, water alcohol method, n-butyl alcohol method, salting out method from the bavin field, develop into more advanced resin method at present.But the content of total Saponin is generally 75-80% in Radix Ginseng total saponins or the total panaquilon extract.Even adopt advanced resin method, the content of total Saponin also can only reach 80-85% in the extract.
Summary of the invention
The objective of the invention is to: provide a kind of and extract method of total Saponin and products thereof by Radix Ginseng or Radix Panacis Quinquefolii stem/leaf, the total saponin content that makes products obtained therefrom is greater than 85%.
The method of extracting total Saponin by Radix Ginseng or Radix Panacis Quinquefolii stem/leaf provided by the present invention may further comprise the steps: (1) is carried out normal pressure to Rhizoma panacis majoris and/or ginseng stem and is extracted, to obtain extracting solution; (2) the resulting extracting solution that alkalizes; (3) extracting solution leaves standstill, and the extracting solution after the filtering and standing; (4) make gained filtrate pass through H
+Type cation-adsorption resin column; (5) wash this H with water
+Type cation-adsorption resin column; (6) resolve this H with ethanol
+Type cation-adsorption resin column obtains desorbed solution; (7) desorbed solution is carried out desalination, decolouring; (8) reclaim ethanol, concentrated, dry, to obtain Radix Ginseng or total panaquilon product.
The total Saponin product that is extracted by Radix Ginseng or Radix Panacis Quinquefolii stem/leaf provided by the invention is characterised in that: the content of total Saponin is greater than 85% in the described product.
Describe step of the present invention below one by one in detail, so that those skilled in the art's understanding.But therefore the method for the invention and products thereof is not subjected to any restriction.
In method provided by the present invention, the raw material that is adopted should be selected free from admixture for use, not have the Rhizoma panacis majoris and/or the ginseng stem that go mouldy, and wherein, greenery/Huang Ye is preferably greater than 60% in the described Rhizoma panacis majoris, further is preferably greater than 70%; Described ginseng stem is reuse after crushed preferably, and for example, the length that makes the ginseng stem is less than 10 centimetres, preferably less than 8 centimetres.
(1), Rhizoma panacis majoris and/or ginseng stem are carried out the normal pressure extraction
In method provided by the present invention, described normal pressure extracts and further may further comprise the steps: add described Rhizoma panacis majoris and/or ginseng stem raw material and water in extraction pot; In extraction pot, add flocculating agent and basifier; Temperature and extraction time are extracted in control; From extraction pot, tell extracting solution.
For the same a collection of raw material in the extraction pot, described normal pressure leaching process can repeat 1-5 time, preferred 2-3 time.And resulting extracting solution can carry out subsequent treatment separately, carries out subsequent treatment after also can merging again.
In method provided by the present invention, extracting the used water of total Saponin can be nature water, also can be deionized water, distilled water or pure water.Calcium in the water, the isoionic content of magnesium should be less than 40-50mg/L, and preferably less than 20-30mg/L, further preferably less than 8-10mg/L, its electrical conductivity is preferably less than 50S/cm.
In the normal pressure leaching process, the addition of described water is described Rhizoma panacis majoris and/or ginseng stem raw material weight 5-20 a times, and preferred 8-15 doubly makes the water surface exceed the raw material charge level and is advisable for about 10-15 centimetre.
In the normal pressure leaching process, described flocculating agent is selected from Na
2SO
4, Al
2(SO
4)
3Or FeSO
4In a kind of, preferred Al
2(SO
4)
3, its addition accounts for the 1-10% of raw material weight, preferred 2-8%.Described basifier is CaO or MgO, preferred CaO, and its addition accounts for the 1-10% of raw material weight, preferred 2-8%.If use powder-type CaO, CaCO in the powder
3Content must be less than 10-15%.
In the normal pressure leaching process, described extraction temperature is 60-95 ℃, preferred 70-85 ℃.In specific implementation process, can extraction pot be heated by the method that in the extraction pot interlayer, feeds steam, and the temperature of control extraction pot.Described extraction time is 1-4 hour, preferred 2-3 hour.Extraction time described here begins to calculate when extracting temperature from reaching.In the normal pressure leaching process, for the concentration that makes feed liquid is even as far as possible, can every interval certain hour, for example 30 minutes, open feed pump once, to realize the circulation of feed liquid in extraction pot.In addition,, should guarantee that Rhizoma panacis majoris, the ginseng stem raw material in the extraction pot is positioned at below the liquid level of extracting solution, can take measures such as mechanical pressure in case of necessity in order to obtain extraction effect preferably.
(2), the alkalization of extracting solution
In the resulting extracting solution of normal pressure leaching process, add Al
2(SO
4)
3, its addition is the 0.1-1% of extracting solution weight, preferred 0.2-0.5% makes it fully be dissolved in the extracting solution; PH value with basifier CaO adjusting extracting solution makes pH=7-14.Preferably adopt fine CaO, it is dissolved with a small amount of extracting solution earlier behind the deliquescence powdered, then it is added in extracting solution, and constantly stir.
(3), extracting solution leaving standstill and filtering
Feed liquid after the alkalization generally left standstill 6-15 hour, preferred 8-12 hour.In the process of leaving standstill, should make the temperature of extracting solution be lower than 50 ℃, preferably be lower than 45 ℃, further preferably be lower than 40 ℃.Rationally the control dwell temperature can make the alkalization effect very desirable.If dwell temperature is too high, can inject the cold water cooling.
The present invention does not have special requirement for the filtration of the extracting solution after leaving standstill, and adopts plate and frame filter, centrifugal filter or natural filtration etc. all can.If adopt the plate and frame filter, can adopt 621 type filter clothes.If when adopting filter press, operating pressure can be controlled in 0.15-0.2MPa.The transmittance that filters back gained filtrate should be greater than 90%.Described transmittance 721 spectrophotometer measurements, its value are the ratio of filtrate and distilled water or ethanol.If filtrate does not reach above-mentioned transmittance requirement, can adopt the method for circulating filtration, until reaching above-mentioned standard.
(4), make filtrate pass through H
+Type cation-adsorption resin column
The resulting filtrate of above-mentioned steps is passed through H
+Type cation-adsorption resin column.Described H
+Type cation-adsorption resin can be selected 860021 resins of the anti-pharmaceutical factory in Shandong, Jining, Shandong production or the AB-8 resin that resin processing plant of Nankai University produces for use.Described H
+Type cation-adsorption resin also comprises the macroporous adsorbent resin that this area is commonly used.The preferred φ of the blade diameter length ratio of described cation-adsorption resin column: h=1: 6-8, for example, wherein φ can be 600-800mm.In adsorption separation process, should note controlling the speed and the time of adsorbing separation, for example, adsorb early stage, the flow velocity of feed liquid can be controlled at 500-600Kg/ hour, about 6-8 of time hour; Adsorb mid-term, the flow velocity of feed liquid can be controlled at 400-500Kg/ hour, about 6-8 of time hour; Adsorb latter stage, the flow velocity of feed liquid can be controlled at 200-300Kg/ hour, about 2-4 of time hour.In adsorption separation process, need the degree of saturation of monitoring adsorption resin column.When adsorption resin column when saturated, preferably stop the feed liquid exchange, and close post about 2 hours, proceed the adsorbing separation of feed liquid then, till adsorption resin column is saturated fully.
Whether can adopt following method to measure adsorption resin column saturated: adding exchanges about liquid 5ml effusive latter stage in the 20ml test tube, drips about 10 glacial acetic acid then in test tube, splashes into dense H along test tube wall again after the vibration
2SO
44-5 drips.If produce red or mauve ring, then to contain the glycoside amount very high for proof; If produce light red or peach ring, then to contain the glycoside amount very low for proof.To contain the glycoside amount very high if exchange liquid latter stage, can assert that the adion exchanger resin has been in saturation.
(5), wash H with water
+Type cation-adsorption resin column
The feed liquid that does not fully exchange in the adsorption resin column is turned back in the storage tank of storing feed liquid, be used for the adsorbing separation of following one-period; With natural water, deionized water, distilled water or pure water thorough washing resin, can adopt positive and negative both direction thorough washing in case of necessity, the resin flushing of caking is opened, simultaneously impurity and other water-soluble substances in the flush away resin; When washings were haze-free, it was qualified to wash post, and the water emptying in the adsorption resin column is got final product.
(6), resolve the cation-adsorption resin column with ethanol
Inject the ethanol of 50-80% in the resin column after above-mentioned washing, the ethanol of preferred 60-75%, its injection rate is 1.5-5 a times of amount of resin, preferred 2-3 times, further preferred 2-2.5 times.Described ethanol is injected by the top of resin column, and the effluent with reagent monitoring resin column below when in measuring effluent the Saponin of trace being arranged, closed post 2-3 hour, made the Saponin in the resin column be dissolved fully by ethanol.Resolution temperature is controlled at 20-60 ℃, and preferred 25-50 ℃, further preferred 30-45 ℃.After closing the end of post time, open the valve of resin column below, discharge desorbed solution, then by the remaining ethanol of the continuous adding in resin column top.After ethanol has all been annotated, continued to close post 1 hour, discharge ethanol in the post then.When the ethanol liquid level arrives the lower surface of resin column, in post, add nature water, deionized water or distilled water, carry out compression leg.With the effusive liquid of reagent and alcohol meter monitoring post below.Do not contain Saponin when measure effusive liquid with reagent, and the alcohol concentration of measuring effusive liquid with alcohol meter shows that less than 10% o'clock the adsorption column parsing finishes.
(7), desorbed solution is carried out desalination, decolouring
In order to remove the micro-residue in the above-mentioned desorbed solution, for example can adopting, the sand rod filters.The gained feed liquid is carried out desalination and decolouring processing.
Desalination can be selected cation exchange resin for use, for example, can select the 001X16 resin of the anti-pharmaceutical factory in Shandong, Jining, Shandong production or the D-72 resin that resin processing plant of Nankai University produces for use.The purpose of desalination is to slough heavy metal elements such as calcium, magnesium, aluminum plasma and arsenic in the desorbed solution, lead, hydrargyrum, thereby improves the quality of products.
Decolouring can be selected anion exchange resin for use, for example, can select the D-941 resin of the anti-pharmaceutical factory in Shandong, Jining, Shandong production or the D-280 resin that resin processing plant of Nankai University produces for use.The purpose of decolouring is to slough pigments such as chlorophyll in the desorbed solution, flavochrome, brown pigment, thereby improves the quality of product, makes the color of resulting Saponin more pure.
In desorbed solution desalination, decolorization, feed liquid is flowed through behind the desalination ion exchange resin column, under the effect of gravity, flow automatically in the decolouring ion exchange resin column.Feed liquid can adopt in the desalination ion exchange resin column and just exchange and contrary exchange.The preferred φ of blade diameter length ratio of described desalination and decolouring ion exchange resin column: h=1: 6-8.
In described desalination, decolorization, the flow velocity of desorbed solution preferably was controlled at 100-150Kg/ hour, can monitor by effusion meter, surveyed electrical conductivity less than 50S/cm.When desorbed solution by desalination, decolorizing resin post, its liquid level arrive the decolorizing resin post bottom the time, can add nature water, deionized water or distilled water by desalination exchange resin column top, carry out compression leg.With the effusive exchange liquid in reagent and alcohol meter monitoring decolouring ion exchange resin column below, do not contain Saponin when measure effusive liquid with reagent, and the concentration of its ethanol is less than 10% o'clock, illustrate that desalination, decolorization finish.Because of containing a large amount of ethanol in resulting desalination, the decolouring exchange liquid, so exchange liquid preferably is stored in the airtight container.
(8), reclaim ethanol, product concentrate drying
Can utilize ethanol recovery tower or concentrating under reduced pressure equipment or other similar devices to reclaim ethanol, recovered temperature can be controlled in about 75-80 ℃, and pressure recovery can be controlled between the 0.05-0.08MPa, and the ethanol that is reclaimed can cycling and reutilization.The density of gained extractum is generally 1.04-1.06g/cm behind the recovery ethanol
3Extractum is concentrated, for example concentrate under normal pressure, temperature is controlled at 90-95 ℃, and the steam pressure of indirect is controlled at 0.05-0.1MPa, and can obtain density is 1.20-1.30g/cm
3Equivalent extract.Ethanol with 40% or pure water transfer to 1.07-1.10g/cm with the density of equivalent extract
3Between, can make total Saponin finished product by means of spray drying device.The compressed air of described spray drying device can be controlled in 4MPa, and the material outlet temperature is 110-130 ℃, and its inlet temperature is 180-210 ℃.Resulting total Saponin finished product can carry out quality inspection and packing according to conventional method.
The content that adopts total Saponin in total Saponin product that said method extracts by Radix Ginseng or Radix Panacis Quinquefolii stem/leaf is preferably greater than 90% greater than 85%, further is preferably greater than 95%.
The content of described total Saponin adopts the thin plate chromatography to measure.
Compared with prior art, beneficial effect of the present invention is mainly reflected in following aspect: method provided by the invention is applicable to commercial process, and adopt this method can make high-quality Radix Ginseng total saponins and total panaquilon, total saponin content is greater than 85% even can be greater than 90% in its product.Because the prepared total Saponin product of the present invention has passed through strict desalination, decolouring is handled, not only more thorough to removing of harmful heavy metal element such as calcium, magnesium, aluminum plasma and arsenic, lead, hydrargyrum, and having removed pigments such as chlorophyll, flavochrome, brown pigment, the color of resulting Saponin product is more pure.Make ginsenoside and Radix Panacis Quinquefolii Saponin can be applied even more extensively, bring into play its curative effect of medication better in fields such as medicine, health product, beverage, daily cosmetics.Therefore, method provided by the present invention has tangible economic benefit and good social benefit.
The specific embodiment
The following examples will further specify method provided by the present invention and products thereof, but therefore the present invention is not subjected to any restriction.
Embodiment 1
This embodiment explanation: adopt method of the present invention, can make content is the Radix Ginseng total saponins product of 86-98%.
With the Rhizoma panacis majoris of Radix Ginseng and pulverize back length less than 10 centimetres ginseng stem totally 100 kilograms add in the extraction pot, and in extraction pot, inject 1000 kilograms of deionized waters, add flocculating agent A l
2(SO
4)
3(industrial goods are through pulverizing＜10 orders) 3 kilograms adds basifier CaO (high-quality product is used behind the deliquescence powdered) 3 kilograms.Extracting temperature is 70-80 ℃, and extraction time is 2 hours.The 30 minutes unlatching feed pumps in every interval are beaten circulation primary in the leaching process.After the above-mentioned first time, normal pressure extracted end, by discharging extracting solution in the extraction pot.Re-inject 900 kilograms of deionized waters in above-mentioned extraction pot, begin to carry out the normal pressure extraction second time, repeat above-mentioned normal pressure extraction step, extraction time is 3 hours.After normal pressure extracts and finishes for the second time, by discharging secondary raffinate in the extraction pot.Inject 600 kilograms of deionized waters for the third time in above-mentioned extraction pot, begin to carry out normal pressure extraction for the third time, repeat above-mentioned normal pressure extraction step, extraction time is 1 hour.In normal pressure leaching process for the third time, can not add flocculating agent and basifier.After normal pressure extracts and finishes for the third time, by discharging extracting solution for the third time in the extraction pot.
Above-mentioned three normal pressures extract resulting extracting solution and inject the extracting solution storage tank, and the extracting solution that takes a morsel dissolving accounts for the Al of extracting solution weight 0.3%
2(SO
4)
3, then it is added in the storage tank, and fully stirs.With basifier CaO the pH value of extracting solution is adjusted to pH=13.After extracting solution leaves standstill 12 hours, adopt flame filter press to filter, the filter cloth model is 621 types, and the transmittance of gained filtrate is greater than 90%.
Use H
+Type cation-adsorption resin column carries out adsorbing separation to filtrate, and the model of used resin is 860021, and its manufacturer is the anti-pharmaceutical factory in Shandong, Jining, Shandong, and the blade diameter length ratio of resin column is 1: 6.In adsorption separation process, note the speed and the time of control adsorbing separation.Absorption early stage, the flow speed control of feed liquid is at 500Kg/ hour, about 8 hours of time; Absorption mid-term, the flow speed control of feed liquid is at 400Kg/ hour, about 6 hours of time; Adsorb latter stage, the flow velocity of feed liquid can be controlled in 200Kg/ hour, about 2 hours of time.In adsorption separation process, the degree of saturation of monitoring adsorption resin column.When adsorption resin column when saturated, stop the feed liquid exchange, close post about 2 hours, proceed the feed liquid exchange then, till adsorption resin column is saturated fully.With deionized water thorough washing resin column.
Inject 70% ethanol in the resin column after above-mentioned washing, its injection rate is 2.5 times of amount of resin.When in measuring effluent, the Saponin of trace being arranged, closed post 2-3 hour, make the Saponin in the resin column be dissolved fully by ethanol.Resolution temperature is controlled at about 40 ℃.
In order to remove the micro-residue in the gained desorbed solution, gained filtrate is carried out desalination and decolouring processing.The model of selected desalination ion exchange resin is 001X16, and manufacturer is the anti-pharmaceutical factory in Shandong, Jining, Shandong, the blade diameter length ratio φ of its resin column: h=1: 6, and the desorbed solution flow velocity is 100-150Kg/ hour.The model of selected decolouring ion exchange resin is D-941, and manufacturer is the anti-pharmaceutical factory in Shandong, Jining, Shandong, the blade diameter length ratio φ of its resin column: h=1: 6, and the desorbed solution flow velocity is 100-150Kg/ hour.Do not contain Saponin when measure effusive liquid with reagent, and the concentration of its ethanol is less than 10% o'clock, illustrates that desalination, decolorization finish.Reclaim ethanol, the products obtained therefrom spray drying can obtain the Radix Ginseng total saponins product A.Adopt the thin plate chromatography to measure the total saponin content of product, its result is referring to table 1.
Adopt the main operating parameters described in the table 1, and with reference to the extracting method of product A, preparing product B, C and D.
Table 1
| Product A | Product B | Products C | Product D | |
| H +The model blade diameter length ratio of type cation-adsorption resin | 860021 1∶6 | AB-8 1∶6 | 860021 1∶6 | 860021 1∶6 |
| Adsorbing separation flow velocity and time: | ||||
| The flow velocity in early stage, Kg/ hour | 500 | 600 | 550 | 550 |
| Time, hour | 8 | 8 | 7 | 8 |
| The flow velocity in mid-term, Kg/ hour | 400 | 500 | 400 | 450 |
| Time, hour | 6 | 6 | 6 | 6 |
| The flow velocity in latter stage, Kg/ hour | 200 | 200 | 200 | 200 |
| Time, hour | 2 | 2 | 2 | 2 |
| The model blade diameter length ratio of desalination ion exchange resin | 001X16 1∶6 | D-72 1∶6 | 001X16 1∶6 | 001X16 1∶6 |
| The model blade diameter length ratio of decolouring ion exchange resin | D-941 1∶6 | D-280 1∶6 | D-941 1∶6 | D-941 1∶8 |
| Total saponin content, heavy % | 86 | 90.5 | 93.1 | 98 |
| The end product yield, heavy % | 6.6 | 6.2 | 5.8 | 5.6 |
Embodiment 2
This embodiment explanation: adopt method of the present invention, can make content greater than 95% total panaquilon.
With the Rhizoma panacis majoris of Radix Panacis Quinquefolii and pulverize back length less than 10 centimetres ginseng stem totally 100 kilograms add in the extraction pot, and in extraction pot, inject 1000 kilograms of deionized waters, add flocculating agent A l
2(SO
4)
3(industrial goods are through pulverizing＜10 orders) 3 kilograms adds basifier CaO (high-quality product is used behind the deliquescence powdered) 3 kilograms.Extracting temperature is 70-80 ℃, and extraction time is 2 hours.The 30 minutes unlatching feed pumps in every interval are beaten circulation primary in the leaching process.After the above-mentioned first time, normal pressure extracted end, by discharging extracting solution in the extraction pot.Re-inject 900 kilograms of deionized waters in above-mentioned extraction pot, begin to carry out the normal pressure extraction second time, repeat above-mentioned normal pressure extraction step, extraction time is 3 hours.After normal pressure extracts and finishes for the second time, by discharging secondary raffinate in the extraction pot.Inject 600 kilograms of deionized waters for the third time in above-mentioned extraction pot, begin to carry out normal pressure extraction for the third time, repeat above-mentioned normal pressure extraction step, extraction time is 1 hour.In normal pressure leaching process for the third time, can not add flocculating agent and basifier.After normal pressure extracts and finishes for the third time, by discharging extracting solution for the third time in the extraction pot.
Above-mentioned three normal pressures extract resulting extracting solution and inject the extracting solution storage tank, and the extracting solution that takes a morsel dissolving accounts for the Al of extracting solution weight 0.3%
2(SO
4)
3, then it is added in the storage tank, and fully stirs.With basifier CaO the pH value of extracting solution is adjusted to pH=13.After extracting solution leaves standstill 12 hours, adopt flame filter press to filter, the filter cloth model is 621 types, and the transmittance of gained filtrate is greater than 90%.
Use H
+Type cation-adsorption resin column carries out adsorbing separation to filtrate, and the model of used resin is 860021, and its manufacturer is the anti-pharmaceutical factory in Shandong, Jining, Shandong, and the blade diameter length ratio of resin column is 1: 8.In adsorption separation process, note control exchange velocity and swap time.In the absorption early stage of feed liquid, exchange velocity is controlled at 600Kg/h, about 8 hours of swap time; In the absorption mid-term of feed liquid, exchange velocity is controlled at 500Kg/h, about 6 hours of swap time; In the absorption latter stage of feed liquid, exchange velocity can be controlled at 300Kg/h, about 2 hours of swap time.With deionized water thorough washing resin column.
Inject 70% ethanol in the resin column after above-mentioned washing, its injection rate is 2.5 times of amount of resin.When in measuring effluent, the Saponin of trace being arranged, closed post 2-3 hour, make the Saponin in the resin column be dissolved fully by ethanol.Resolution temperature is controlled at about 40 ℃.
Micro-residue in the filtering gained desorbed solution carries out desalination and decolouring processing to gained filtrate.The model of selected desalination ion exchange resin is 001X16, and manufacturer is the anti-pharmaceutical factory in Shandong, Jining, Shandong, the blade diameter length ratio φ of its resin column: h=1: 8, and exchange velocity is 100-150Kg/h.The model of selected decolouring ion exchange resin is D-941, and manufacturer is the anti-pharmaceutical factory in Shandong, Jining, Shandong, the blade diameter length ratio φ of its resin column: h=1: 8, and exchange velocity is 100-150Kg/h.Do not contain Saponin when measure effusive liquid with reagent, and the concentration of its ethanol is less than 10% o'clock, illustrates that desalination, decolorization finish.Reclaim ethanol, it is 96.4% total panaquilon product that the products obtained therefrom spray drying can obtain content.Adopt the total saponin content of thin plate chromatography testing product, testing agency is: the institute for drug control, Jilin Province.
Claims (10)
1. one kind is extracted the method for total Saponin by Radix Ginseng or Radix Panacis Quinquefolii stem/leaf, may further comprise the steps: (1) is carried out normal pressure to Rhizoma panacis majoris and/or ginseng stem and is extracted, to obtain extracting solution; (2) the resulting extracting solution that alkalizes; (3) extracting solution leaves standstill, and the extracting solution after the filtering and standing; (4) make gained filtrate pass through H
+Type cation-adsorption resin column; (5) wash this H with water
+Type cation-adsorption resin column; (6) resolve this H with ethanol
+Type cation-adsorption resin column obtains desorbed solution; (7) desorbed solution is carried out desalination, decolouring; (8) reclaim ethanol, concentrated, dry, to obtain Radix Ginseng or total panaquilon product.
2. according to the described extracting method of claim 1, it is characterized in that described normal pressure extracts and may further comprise the steps: in extraction pot, add Rhizoma panacis majoris and/or ginseng stem raw material and water; Described wet concentration is from any one in natural water, deionized water, distilled water or the pure water, and the addition of water be described Rhizoma panacis majoris and/or ginseng stem weight 5-20 doubly; In extraction pot, add flocculating agent and basifier; It is 60-95 ℃ that temperature is extracted in control, and extraction time is 1-4 hour; Tell extracting solution.
3. according to the described extracting method of claim 2, it is characterized in that described flocculating agent is selected from Na
2SO
4, Al
2(SO
4)
3Or FeSO
4In a kind of, its addition is the 1-10% of Rhizoma panacis majoris and/or ginseng stem weight; Described basifier is CaO or MgO, and its addition is the 1-10% of Rhizoma panacis majoris and/or ginseng stem weight.
4. according to the described extracting method of claim 1, it is characterized in that the step of described alkalization extracting solution is to add the Al that accounts for extracting solution weight 0.1-1% in extracting solution
2(SO
4)
3, and with basifier the pH value of extracting solution is transferred to and to be alkalescence, described basifier is through deliquescent CaO.
5. according to the described extracting method of claim 1, it is characterized in that described leaving standstill with filtration step is that extracting solution is left standstill 6-15 hour, and leave standstill that the temperature of extracting solution is lower than 40 ℃ in the process; Extracting solution after the filtering and standing makes the transmittance of resulting filtrate greater than 90%.
6. according to the described extracting method of claim 1, it is characterized in that described H
+The blade diameter length ratio φ of type cation-adsorption resin column: h=1: 6-8.
7. according to the described extracting method of claim 6, it is characterized in that, use H described filtrate
+In the process of type cation-adsorption resin column adsorbing separation, absorption filtrate flow velocity in earlier stage is 500-600Kg/ hour, and the time is 6-8 hour; The filtrate flow velocity that adsorbs mid-term is 400-500Kg/ hour, time 6-8 hour; The filtrate flow velocity that adsorbs latter stage is 200-300Kg/ hour, and the time is 2-4 hour.
8. according to the described extracting method of claim 1, it is characterized in that, in the described process of desorbed solution being carried out desalination, decolouring, cation exchange resin is selected in desalination for use, its model is 001 * 16 or D-72, the blade diameter length ratio φ of its resin column: h=1: 6-8, desorbed solution flow velocity are 100-150Kg/ hour; It is D-941 or D-280 that anion exchange resin, its model are selected in decolouring for use, the blade diameter length ratio φ of its resin column: h=1: 6-8.The desorbed solution flow velocity is 100-150Kg/ hour.
9. according to the described extracting method of claim 8, it is characterized in that, in described desorbed solution desalination, decolorization, desorbed solution is flowed through behind the ion exchange resin column of desalination, under the effect of gravity, flow automatically in the ion exchange resin column of decolouring.
10. a total Saponin product that is extracted by Radix Ginseng or Radix Panacis Quinquefolii stem/leaf is characterized in that the content of total Saponin is greater than 85% in described total Saponin product.
Priority Applications (1)
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|---|---|---|---|
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012088777A1 (en) * | 2010-12-31 | 2012-07-05 | 浙江省中医院 | Effective part of ginseng, preparing method and use thereof |
| JP2014114220A (en) * | 2012-12-06 | 2014-06-26 | Kao Corp | Cgrp responsiveness promoter |
| CN107536918A (en) * | 2016-06-23 | 2018-01-05 | 上海医药集团股份有限公司 | A kind of Chinese medicine composition, preparation method and the usage treated and/or prevent cardiac neurosis |
| JP2018538286A (en) * | 2015-11-25 | 2018-12-27 | ナチュラル レスポンス、エセ．ア．Ｎａｔｕｒａｌ Ｒｅｓｐｏｎｓｅ， Ｓ．Ａ． | How to get saponin from plants |
| CN111938126A (en) * | 2019-05-17 | 2020-11-17 | 清馨(北京)科技有限公司 | Preparation method of compound sweetener |
| CN113288839A (en) * | 2021-06-25 | 2021-08-24 | 广东真丽斯化妆品有限公司 | Method for extracting ginseng extract for preparing cosmetics |
| CN113648681A (en) * | 2021-08-27 | 2021-11-16 | 湖南华康生物科技股份有限公司 | Method for extracting and separating ginsenoside from Korean ginseng |
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2005
- 2005-07-12 CN CN 200510082778 patent/CN1895313A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012088777A1 (en) * | 2010-12-31 | 2012-07-05 | 浙江省中医院 | Effective part of ginseng, preparing method and use thereof |
| JP2014114220A (en) * | 2012-12-06 | 2014-06-26 | Kao Corp | Cgrp responsiveness promoter |
| JP2018538286A (en) * | 2015-11-25 | 2018-12-27 | ナチュラル レスポンス、エセ．ア．Ｎａｔｕｒａｌ Ｒｅｓｐｏｎｓｅ， Ｓ．Ａ． | How to get saponin from plants |
| JP7120921B2 (en) | 2015-11-25 | 2022-08-17 | ナチュラル レスポンス、エセ．ア． | How to get saponin from plants |
| US11510954B2 (en) | 2015-11-25 | 2022-11-29 | Desert King Chile S.A. | Method for obtaining saponins from plants |
| CN107536918A (en) * | 2016-06-23 | 2018-01-05 | 上海医药集团股份有限公司 | A kind of Chinese medicine composition, preparation method and the usage treated and/or prevent cardiac neurosis |
| CN111938126A (en) * | 2019-05-17 | 2020-11-17 | 清馨(北京)科技有限公司 | Preparation method of compound sweetener |
| CN113288839A (en) * | 2021-06-25 | 2021-08-24 | 广东真丽斯化妆品有限公司 | Method for extracting ginseng extract for preparing cosmetics |
| CN113648681A (en) * | 2021-08-27 | 2021-11-16 | 湖南华康生物科技股份有限公司 | Method for extracting and separating ginsenoside from Korean ginseng |
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