CN108310039A - A method of extraction Gypenosides - Google Patents
A method of extraction Gypenosides Download PDFInfo
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- CN108310039A CN108310039A CN201810458420.2A CN201810458420A CN108310039A CN 108310039 A CN108310039 A CN 108310039A CN 201810458420 A CN201810458420 A CN 201810458420A CN 108310039 A CN108310039 A CN 108310039A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/42—Cucurbitaceae (Cucumber family)
- A61K36/424—Gynostemma
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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Abstract
The invention discloses a kind of convenient, system, the methods of integrated extraction Gypenosides, and described method includes following steps：1st step：Gynostemma pentaphyllum is crushed, gynostemma pentaphyllum powder is obtained；2nd step：Gynostemma pentaphyllum powder is put and is extracted in ethanol, filtrate is obtained；3rd step：The upper resin column of filtrate is adsorbed, until resin is saturated；The saponin(e adsorbed in the resin column is desorbed using ethyl alcohol, obtains ethyl alcohol stripping liquid；The ethyl alcohol stripping liquid is distilled, ethyl alcohol is recycled, solid drying obtains Gypenosides powder；4th step：It is removed using the Impurity elution that resin regeneration solution is adsorbed resin, it is made to restore original composition and performance.This method have medicinal material pre-treatment, extraction, column chromatography, resin regeneration difference free of discontinuities separation engagement process, separative efficiency is high, separation process is stable, is convenient for Quality Control, and the Gypenosides of destination number can be obtained by the control of portion link.
Description
Technical field
The present invention relates to active ingredients from traditional Chinese medicinal extractive technique fields, and in particular to a kind of side of extraction Gypenosides
Method.
Background technology
Gypenosides, have the effects that reducing blood lipid, improve myocardial ischemia-anoxemia, cerebral ischemia is protected, anti-oxidant.Nourishing heart
Invigorating the spleen, QI invigorating and blood, eliminating phlegm stagnation resolvation are suitable for hyperlipidemia, see had palpitation shortness of breath, limb uncomfortable in chest fiber crops, dizziness and headache, forgetful ear
The hearts Spleen-Qi Deficiencies such as ring, unconsciously sweat and tire or abdominal fullness and distention, phlegm hinder blood stasis person.
The pharmacological action of Gypenosides：Drug composition mainly has Gypenosides.Have reducing blood lipid, platelet aggregation-against,
It is the effects that damage, anti-aging of resisting myocardial ischemia, specific as follows：
1. reducing blood lipid：Serum lipids in rats is induced with high glucose and high fat feed, gives Gypenosides treatment (7 days), as a result
Treatment group's serum cholesterol, triacylglycerol content are significantly reduced than control group；Its curative effect and dosage are in a linear relationship.Experiment in vitro
Show that Gypenosides can inhibit adipocyte and be decomposed to form free fatty, inhibit in adipocyte intake glucose synthesis
Property aliphatic acid.In addition, the medicine reduce blood fat simultaneously, also can antiatherosclerosis, make arterial wall plaque formed reduce, damage
Mitigate.
2. resist myocardial ischemia damage：Results of Animal shows that Gypenosides can not only reduce myocardial infarction model
Enclose, and can fight Post-ischemic Reperfusion damage (make cardiac muscle cell's marshalling, it is clear in structure, mitochondrial swelling mitigate,
Vacuole is reduced, and cell chromosome is uniform).
3. platelet aggregation-against：Experiment in vitro prove Gypenosides obviously inhibit platelet aggregation (collagen,
ADP, arachidonic acid) induction platelet aggregation；The visible blood platelet of Ultrastructural observation is in dispersed, and surface is smooth, no puppet
Foot-shape is at intracellular granular is more and clear.
4. the influence of pair haemodynamics：To dog intravenous injection Gypenosides (1mg/kg), it is seen that angiocarpy is in excitement
Effect, systolic pressure and diastolic pressure are shown in raising (systolic pressure, which increases, is more than diastolic pressure), and effect maintains 30 minutes or more；Changes in heart rate
Unobvious.In addition myocardial contraction and diastolic performance can be improved, minute output is made to increase, myocardium blood circulation improves.Escalated dose
To angiocarpy, in inhibiting effect, (blood pressure reduces intravenous (20mg/kg), and heart rate is slack-off, and myocardial contraction and diastolic performance reduce, and make defeated
Output is reduced).
5. enhancing sexual function acts on：Herb Gynostemmae Pentaphylli extract gavage can make the testis and prostate, female mice of male mice
Uterus weight is significantly increased compared with the control group, illustrates that gynostemma pentaphylla has male, the effect of female hormone sample.
6. enhancing muscle power and antifatigue effect：(1) Gypenosides, water extract are experiments have shown that can extend mouse swimming time
And pole-climbing time and loading swimming time.Continuous 14 days of the Herb Gynostemmae Pentaphylli extract gavage of larger dose can make to swim for a long time big
Mouse keeps, compared with elevated blood glucose levels, reducing muscle glycogen loss, this may be the antifatigue major reason of gynostemma pentaphylla；(2) gynostemma pentaphylla can
Mouse is improved to the time-to-live under the higher environment of tolerance and temperature of normobaric hypoxia.
7. enhancing immunization gynostemma pentaphylla can increase normal mouse spleen and thymic weight；Gypenoside can also fight ring
Mouse spleen and thymic weight caused by phosphamide decline.And Phagocytosis By The Peritoneal Macrophages In Mice can be enhanced.
8. anti-free radical effects：(1) gypenoside can be substantially reduced naturally-aged and experiment aging rats liver
With plasma adherence (LPO) content.Clinical research reports that LPO values obviously increase in old man's patients with coronary heart disease blood, take
It is substantially reduced with LPO values after compound gynostemma pentaphylla preparation, is restored to the level of healthy male the elderly；(2) Gypenosides can make
Malonaldehyde (MDA) is reduced in exhausted movemeat mouse core nephridial tissue, superoxide dismutase compound mutase (SOD) activity in nephridial tissue
It increases, SOD/MDA ratios are opposite to be increased, and has the function that protect heart nephridial tissue that radical damage is immunized.With gynostemma pentaphylla alcohol extract
It feeds mouse and not only improves Mouse Liver SOD activity, while also enhancement of SOD is heat-resisting, acid resistance, plays the role of protecting SOD.
9. life test --- " cell-activating effect "：Gynostemma pentaphylla and its compound preparation can extend mouse average life span and
Maximum life span.According to another report, gynostemma pentaphylla extends the biological cell proliferation of composition and passes on, in the culture solution containing total glycosides 200mg/ml,
The fibroblast of the in vitro normal diploid of human fetal is set to breed to 59 generations, and control group only reached for 51 generations and just stops growing, and prolonged
Long 15.7%；Receive the Skin Cell cultured in vitro of syndrome patient to Xiong Er, control group was only multiplied for 22 generations, and gynostemma pentaphylla group extends to
In 27 generations, extended 22%, therefore have the title of cell-activating agent.
The extraction process of original Gypenosides is handled before medicinal material, is extracted, there is larger defect in column chromatography, tool
Body is shown as：Of high cost, low output, total glycosides type lack and then curative effect are caused to decline.
Invention content
The purpose of the present invention is to provide a kind of methods of extraction Gypenosides, to solve existing Gypenosides
The problem of extraction process is of high cost, low output, total glycosides type lack and then curative effect caused to decline.
To achieve the above object, the technical scheme is that：
A method of extraction Gypenosides, described method includes following steps：
(1) step：Gynostemma pentaphyllum is crushed, gynostemma pentaphyllum powder is obtained；
(2) step：The gynostemma pentaphyllum powder that (1) step obtains is put and is extracted in ethanol, filtrate is obtained；
(3) step：The upper resin column of the filtrate is adsorbed, after resin saturation, stops filtrate upper prop；Using ethyl alcohol solution
The saponin(e adsorbed in the resin column is inhaled, ethyl alcohol stripping liquid is obtained；The ethyl alcohol stripping liquid is distilled, ethyl alcohol, solid are recycled
Drying obtains water-soluble and liposoluble ingredient Gypenosides powder (A powder)；The resin column by being sequentially connected in series from top to bottom
D101 large pore resin absorption columns, the first cationic resin column, resin anion (R.A.) column and the second cationic resin column composition；
(4) step：It is removed using the Impurity elution that resin regeneration solution is adsorbed resin, the resin is made to restore original
Composition and performance.
As a preferred solution, the D101 large pore resin absorption columns being sequentially connected in series from top to bottom, first sun from
The column volume ratio of sub- resin column, resin anion (R.A.) column and the second cationic resin column is 1：1：3：1.
As a preferred solution, first cationic resin column is sulfonic group cation exchange column；It is described it is cloudy from
Sub- resin column is strong-base anion-exchange resin column；Second cationic resin column is sulfonic group cation exchange column.
D101 macroporous absorbent resins are a kind of polymer absorbants with the synthesis of porous spongy structure artificial, by tree
Van der Waals force between fat skeleton and the molecule (adsorbate) adsorbed carries out physical absorption by the huge specific surface area of resin
And achieve the purpose that the water-soluble poor organic macromolecule of separation and Extraction from aqueous solution.Medium-height grass is extracted using macroporous absorbent resin
Pharmaceutically active ingredient such as soaping agents, flavonoids, alkaloids, have easy to operate, cost is relatively low, resin can Reusability etc. it is excellent
Point is suitable for industrial-scale production.
Sulfonic group cation exchange column is to be bonded a kind of novel sulfonic acids base sun in the inertia Silica Surface of high-purity
Ion exchange ligand.This unique bonding structure is a kind of polymerization capsule structure of stabilization, than common polymer ions
Exchange column column imitates higher, and has better mechanical strength and reproducibility.Grain size 5um, aperture 300A, specific surface area 50m2/g。
Resin anion (R.A.) column is strong-base anion-exchange resin, styrene/divinylbenzene copolymer chlorion type ratio
1.04 to 1.10 are weighed, single-size, (chlorine type) containing wet ratio 45 to 55%.
As a preferred solution, described (4) step includes the following steps：
(4.1) step：Dose volume score is 3%-7% acidity alcohol solutions；Acid is hydrogen chloride, and alcohol is ethyl alcohol；
(4.2) step：Measure the sodium hydroxide solution that dose volume score is 2%-6%；
(4.3) step：By the acidity alcohol solution upper prop, by column group series system followed by each column；When acid alcohol is molten
After liquid is all added, pure water is sequentially added, keeps identical flow velocity, acid alcohol is all replaced, until column group end efflux PH
When=0.67-7, stop into pure water；
(4.4) step：D101 macroporous resin columns, the first cationic resin column and the second cationic resin column are closed, is opened
Resin anion (R.A.) column；Sodium hydroxide addition resin anion (R.A.) column is allowed to make the transition；After whole lye are into column, replaced using pure water
Lye in column, until column bottom efflux PH=6.5~7 are stopped；
(4.5) step：According to column group series sequence, the ethyl alcohol for being 80%-95% with volume fraction is followed by the first sun
Ion exchange resin column, resin anion (R.A.) column and the second cationic resin column, dosage 4-8BV close column group.
As a preferred solution, in (4.3) step, flow velocity of the acidity alcohol solution in column is 0.5-1.5BV/
h；In (4.4) step, flow velocity of the lye in column is 0.5-1.5BV/h；In (4.5) step, volume fraction 80%-
Flow velocity of 95% ethyl alcohol in each column is 1.5-2.5BV/h.
As a preferred solution, described (4) step further includes (4.6) step：Remaining saponin(e in reclaiming liquid,
The acidity alcohol solution flowed out in (4.3) step and the lye flowed out in (4.4) step are neutralized, ethyl alcohol is recycled, remaining solid dries
Dry, cycle applications are in (2) step.
As a preferred solution, in (3) step, flow velocity of the filtrate in resin column is 1.5-2.5BV/h；
The filtrate treating capacity of the resin column is 25~30BV；The dosage for desorbing the ethyl alcohol of absorption saponin(e in resin column is 3-7BV, flow velocity
For 1.5-2.5BV/h.
As a preferred solution, the volume fraction of the ethyl alcohol employed in (2) step and (3) step is 60-85%.
As a preferred solution, described (2) step includes the following steps：
(2.1) step：Gynostemma pentaphyllum powder is packed into pot for solvent extraction, the ethyl alcohol that volume fraction is 60-85%, dipping is added；Leaching
After 4-8 hours sufficient, liquid is discharged, filters, obtains liquid；The ethyl alcohol that volume fraction is 60-85%, leaching is added in second time dipping
Stain 3-7 hours, filtering, obtains liquid；Merge secondary liquid, it is spare；
(2.2) step：It is separately added into the ethyl alcohol that volume fraction is 60-85% and carries out third time and the 4th time dipping, respectively
Dipping 3-7 hours；Liquid merges after coarse filtration, and cycle applications are in (2) step；
(2.3) step：The residual ethanol in the dregs of a decoction is recycled, the dregs of a decoction (B powder) are continued to employ.The B powder is：Except gynostemma pentaphyllum total
The part mucopolysaccharide and cellulose of indissolubility outside glucoside, trace element and the cellulose absorption influenced by isothermal compressibility
Substance.
As a preferred solution, in (1) step, the particle size of the gynostemma pentaphyllum powder is 2-10 mesh.
The invention has the advantages that：
The present invention provides a kind of convenient, system, the method for integrated extraction Gypenosides, this method has medicinal material
The separation engagement process of the difference free of discontinuities of saponin(e recycling is remained in pre-treatment, extraction, column chromatography, resin regeneration, regenerated liquid, point
From efficient, separation process is stable, is convenient for Quality Control, the gynostemma pentaphyllum total of destination number can be obtained by the control of portion link
Glucoside.
The present invention is using currently advanced reverse resin regeneration, extractive technique.Conventional method is spent ion exchange resin
It goes to adsorb useless ingredient, useful ingredient is obtained in distillate.And the present invention is useful using ion exchange resin absorption
The ingredient Gypenosides of liposoluble ingredient (water-soluble and), be then rinsed again with ethyl alcohol.
The present invention uses very safe D101 large pore resin absorption columns in biological medicine, sulfonic group cation exchange column and strong
Alkalescence anion-exchange resin will not cause Gypenosides to be denaturalized, and very short time is by Gypenosides and other compositions
Separation, substantially increases the purity of Gypenosides, reduces loss late.
Present invention employs classification to extract processing method, the full product utilization of overall process.Form A powder, water-soluble and liposoluble at
The Gypenosides divided.B powder, the part mucopolysaccharide and cellulose of the indissolubility in addition to Gypenosides, trace element, with
And the cellulose adsorbent influenced by isothermal compressibility.Totally 2 kinds of analytical products.
Acid alcohol preparation method, 4% Alkali liquid compounding method are applied in the method for extraction Gypenosides by the present invention.It is first
First, the small-molecule substances component such as water soluble, a large amount of saponins of fat solubility, mucopolysaccharide, fat corpuscles, albumen corpusculum contains largely
Beneficial.Secondly, in industrializing the compound production for preparing extraction Gypenosides preparation, due to experienced a series of life
Production. art process, molecules align character has changed, and becomes to lose activity, so the also property of carrying out brokenly and renaturation technology
Afterwards, it just can get and original source, the Gypenosides of biologically active high-purity.The above-mentioned preparation side that the present invention uses
Decree Gypenosides keep the pharmaceutical activity of very high degree, make domestic Gypenosides industrialization development, industrialized production at
To be possible, while also ensuring the high activity and high-quality of Gypenosides.
Specific implementation mode
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Embodiment 1
The present invention provides a kind of methods of extraction Gypenosides, and described method includes following steps：
(1) step：Gynostemma pentaphyllum is crushed, gynostemma pentaphyllum powder is obtained；The particle size of the gynostemma pentaphyllum powder is 2-10 mesh.
(2) step：The gynostemma pentaphyllum powder that (1) step obtains is put and is extracted in ethanol, filtrate is obtained；
Described (2) step includes the following steps：
(2.1) step：Gynostemma pentaphyllum powder is packed into pot for solvent extraction, the ethyl alcohol that volume fraction is 80% is added, dipping；Leaching foot 6
After hour, liquid is discharged, filters, obtains liquid；The ethyl alcohol that volume fraction is 80% is added in second time dipping, impregnates 5 hours,
Filtering, obtains liquid；Merge secondary liquid, it is spare；
(2.2) step：It is separately added into the ethyl alcohol that volume fraction is 80% and carries out third time and the 4th time dipping, impregnate respectively
5 hours；Liquid merges after coarse filtration, and cycle applications are in (2) step；
(2.3) step：The residual ethanol in the dregs of a decoction is recycled, the dregs of a decoction (B powder) are continued to employ.The B powder is：Except gynostemma pentaphyllum total
The part mucopolysaccharide and cellulose of indissolubility outside glucoside, trace element and the cellulose absorption influenced by isothermal compressibility
Substance.
(3) step：The upper resin column of the filtrate is adsorbed, after resin saturation, stops filtrate upper prop；Using ethyl alcohol solution
The saponin(e adsorbed in the resin column is inhaled, ethyl alcohol stripping liquid is obtained；The ethyl alcohol stripping liquid is distilled, ethyl alcohol, solid are recycled
Drying obtains water-soluble and liposoluble ingredient Gypenosides powder (A powder)；Flow velocity of the filtrate in resin column is 2BV/
h；The filtrate treating capacity of the resin column is 27BV；The dosage for desorbing the ethyl alcohol of absorption saponin(e in resin column is 5BV, and flow velocity is
2BV/h。
The resin column is by D101 large pore resin absorption columns, the first cationic resin column, the moon for being sequentially connected in series from top to bottom
Ion exchange resin column and the second cationic resin column composition；
The D101 large pore resin absorption columns being sequentially connected in series from top to bottom, the first cationic resin column, resin anion (R.A.)
The column volume ratio of column and the second cationic resin column is 1：1：3：1.
First cationic resin column is sulfonic group cation exchange column；The resin anion (R.A.) column be strong basicity the moon from
Sub-exchange resin column；Second cationic resin column is sulfonic group cation exchange column.
(4) step：It is removed using the Impurity elution that resin regeneration solution is adsorbed resin, the resin is made to restore original
Composition and performance.
Described (4) step includes the following steps：
(4.1) step：Dose volume score is 5% acidity alcohol solution；Acid is hydrogen chloride, and alcohol is ethyl alcohol；
(4.2) step：Measure the sodium hydroxide solution that dose volume score is 4%；
(4.3) step：By the acidity alcohol solution upper prop, by column group series system followed by each column；When acid alcohol is molten
After liquid is all added, pure water is sequentially added, keeps identical flow velocity, acid alcohol is all replaced, until column group end efflux PH
When=0.67-7, stop into pure water；Flow velocity of the acidity alcohol solution in column is 1BV/h；
(4.4) step：D101 macroporous resin columns, the first cationic resin column and the second cationic resin column are closed, is opened
Resin anion (R.A.) column；Sodium hydroxide addition resin anion (R.A.) column is allowed to make the transition；After whole lye are into column, replaced using pure water
Lye in column, until column bottom efflux PH=6.5~7 are stopped；Flow velocity of the lye in column is 1BV/h；
(4.5) step：According to column group series sequence, the ethyl alcohol for being 95% with volume fraction is set followed by the first cation
Fat column, resin anion (R.A.) column and the second cationic resin column, dosage 6BV close column group.The ethyl alcohol that volume fraction is 95% is each
Flow velocity in column is 2BV/h.
Described (4) step further includes (4.6) step：Remaining saponin(e in reclaiming liquid, by what is flowed out in (4.3) step
The lye flowed out in acidity alcohol solution and (4.4) step neutralizes, and recycles ethyl alcohol, remaining solid drying, cycle applications are in (2)
Step.
Embodiment 2
The present invention provides a kind of methods of extraction Gypenosides, and described method includes following steps：
(1) step：Gynostemma pentaphyllum is crushed, gynostemma pentaphyllum powder is obtained；The particle size of the gynostemma pentaphyllum powder is 2-10 mesh.
(2) step：The gynostemma pentaphyllum powder that (1) step obtains is put and is extracted in ethanol, filtrate is obtained；
Described (2) step includes the following steps：
(2.1) step：Gynostemma pentaphyllum powder is packed into pot for solvent extraction, the ethyl alcohol that volume fraction is 60% is added, dipping；Leaching foot 4
After hour, liquid is discharged, filters, obtains liquid；The ethyl alcohol that volume fraction is 60% is added in second time dipping, impregnates 3 hours,
Filtering, obtains liquid；Merge secondary liquid, it is spare；
(2.2) step：It is separately added into the ethyl alcohol that volume fraction is 60% and carries out third time and the 4th time dipping, impregnate respectively
3 hours；Liquid merges after coarse filtration, and cycle applications are in (2) step；
(2.3) step：The residual ethanol in the dregs of a decoction is recycled, the dregs of a decoction (B powder) are continued to employ.The B powder is：Except gynostemma pentaphyllum total
The part mucopolysaccharide and cellulose of indissolubility outside glucoside, trace element and the cellulose absorption influenced by isothermal compressibility
Substance.
(3) step：The upper resin column of the filtrate is adsorbed, after resin saturation, stops filtrate upper prop；Using ethyl alcohol solution
The saponin(e adsorbed in the resin column is inhaled, ethyl alcohol stripping liquid is obtained；The ethyl alcohol stripping liquid is distilled, ethyl alcohol, solid are recycled
Drying obtains water-soluble and liposoluble ingredient Gypenosides powder (A powder)；Flow velocity of the filtrate in resin column be
1.5BV/h；The filtrate treating capacity of the resin column is 25BV；The dosage for desorbing the ethyl alcohol of absorption saponin(e in resin column is 3BV, stream
Speed is 1.5BV/h.
The resin column is by D101 large pore resin absorption columns, the first cationic resin column, the moon for being sequentially connected in series from top to bottom
Ion exchange resin column and the second cationic resin column composition；
The D101 large pore resin absorption columns being sequentially connected in series from top to bottom, the first cationic resin column, resin anion (R.A.)
The column volume ratio of column and the second cationic resin column is 1：1：3：1.
First cationic resin column is sulfonic group cation exchange column；The resin anion (R.A.) column be strong basicity the moon from
Sub-exchange resin column；Second cationic resin column is sulfonic group cation exchange column.
(4) step：It is removed using the Impurity elution that resin regeneration solution is adsorbed resin, the resin is made to restore original
Composition and performance.
Described (4) step includes the following steps：
(4.1) step：Dose volume score is 3% acidity alcohol solution；Acid is hydrogen chloride, and alcohol is ethyl alcohol；
(4.2) step：Measure the sodium hydroxide solution that dose volume score is 2%；
(4.3) step：By the acidity alcohol solution upper prop, by column group series system followed by each column；When acid alcohol is molten
After liquid is all added, pure water is sequentially added, keeps identical flow velocity, acid alcohol is all replaced, until column group end efflux PH
When=0.67-7, stop into pure water；Flow velocity of the acidity alcohol solution in column is 0.5BV/h；
(4.4) step：D101 macroporous resin columns, the first cationic resin column and the second cationic resin column are closed, is opened
Resin anion (R.A.) column；Sodium hydroxide addition resin anion (R.A.) column is allowed to make the transition；After whole lye are into column, replaced using pure water
Lye in column, until column bottom efflux PH=6.5~7 are stopped；Flow velocity of the lye in column is 0.5BV/h；
(4.5) step：According to column group series sequence, the ethyl alcohol for being 80% with volume fraction is set followed by the first cation
Fat column, resin anion (R.A.) column and the second cationic resin column, dosage 4BV close column group.The ethyl alcohol that volume fraction is 80% is each
Flow velocity in column is 1.5BV/h.
Described (4) step further includes (4.6) step：Remaining saponin(e in reclaiming liquid, by what is flowed out in (4.3) step
The lye flowed out in acidity alcohol solution and (4.4) step neutralizes, and recycles ethyl alcohol, remaining solid drying, cycle applications are in (2)
Step.
Embodiment 3
The present invention provides a kind of methods of extraction Gypenosides, and described method includes following steps：
(1) step：Gynostemma pentaphyllum is crushed, gynostemma pentaphyllum powder is obtained；The particle size of the gynostemma pentaphyllum powder is 2-10 mesh.
(2) step：The gynostemma pentaphyllum powder that (1) step obtains is put and is extracted in ethanol, filtrate is obtained；
Described (2) step includes the following steps：
(2.1) step：Gynostemma pentaphyllum powder is packed into pot for solvent extraction, the ethyl alcohol that volume fraction is 85% is added, dipping；Leaching foot 8
After hour, liquid is discharged, filters, obtains liquid；The ethyl alcohol that volume fraction is 85% is added in second time dipping, impregnates 7 hours,
Filtering, obtains liquid；Merge secondary liquid, it is spare；
(2.2) step：It is separately added into the ethyl alcohol that volume fraction is 85% and carries out third time and the 4th time dipping, impregnate respectively
7 hours；Liquid merges after coarse filtration, and cycle applications are in (2) step；
(2.3) step：The residual ethanol in the dregs of a decoction is recycled, the dregs of a decoction (B powder) are continued to employ.The B powder is：Except gynostemma pentaphyllum total
The part mucopolysaccharide and cellulose of indissolubility outside glucoside, trace element and the cellulose absorption influenced by isothermal compressibility
Substance.
(3) step：The upper resin column of the filtrate is adsorbed, after resin saturation, stops filtrate upper prop；Using ethyl alcohol solution
The saponin(e adsorbed in the resin column is inhaled, ethyl alcohol stripping liquid is obtained；The ethyl alcohol stripping liquid is distilled, ethyl alcohol, solid are recycled
Drying obtains water-soluble and liposoluble ingredient Gypenosides powder (A powder)；Flow velocity of the filtrate in resin column be
2.5BV/h；The filtrate treating capacity of the resin column is 30BV；The dosage for desorbing the ethyl alcohol of absorption saponin(e in resin column is 7BV, stream
Speed is 2.5BV/h.
The resin column is by D101 large pore resin absorption columns, the first cationic resin column, the moon for being sequentially connected in series from top to bottom
Ion exchange resin column and the second cationic resin column composition；
The D101 large pore resin absorption columns being sequentially connected in series from top to bottom, the first cationic resin column, resin anion (R.A.)
The column volume ratio of column and the second cationic resin column is 1：1：3：1.
First cationic resin column is sulfonic group cation exchange column；The resin anion (R.A.) column be strong basicity the moon from
Sub-exchange resin column；Second cationic resin column is sulfonic group cation exchange column.
(4) step：It is removed using the Impurity elution that resin regeneration solution is adsorbed resin, the resin is made to restore original
Composition and performance.
Described (4) step includes the following steps：
(4.1) step：Dose volume score is 7% acidity alcohol solution；Acid is hydrogen chloride, and alcohol is ethyl alcohol；
(4.2) step：Measure the sodium hydroxide solution that dose volume score is 6%；
(4.3) step：By the acidity alcohol solution upper prop, by column group series system followed by each column；When acid alcohol is molten
After liquid is all added, pure water is sequentially added, keeps identical flow velocity, acid alcohol is all replaced, until column group end efflux PH
When=0.67-7, stop into pure water；Flow velocity of the acidity alcohol solution in column is 1.5BV/h；
(4.4) step：D101 macroporous resin columns, the first cationic resin column and the second cationic resin column are closed, is opened
Resin anion (R.A.) column；Sodium hydroxide addition resin anion (R.A.) column is allowed to make the transition；After whole lye are into column, replaced using pure water
Lye in column, until column bottom efflux PH=6.5~7 are stopped；Flow velocity of the lye in column is 1.5BV/h；
(4.5) step：According to column group series sequence, the ethyl alcohol for being 95% with volume fraction is set followed by the first cation
Fat column, resin anion (R.A.) column and the second cationic resin column, dosage 8BV close column group.The ethyl alcohol that volume fraction is 95% is each
Flow velocity in column is 2.5BV/h.
Described (4) step further includes (4.6) step：Remaining saponin(e in reclaiming liquid, by what is flowed out in (4.3) step
The lye flowed out in acidity alcohol solution and (4.4) step neutralizes, and recycles ethyl alcohol, remaining solid drying, cycle applications are in (2)
Step.
Although above having used general explanation and specific embodiment, the present invention is described in detail, at this
On the basis of invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Therefore,
These modifications or improvements without departing from theon the basis of the spirit of the present invention belong to the scope of protection of present invention.
Claims (9)
1. a kind of method of extraction Gypenosides, which is characterized in that described method includes following steps：
(1) step：Gynostemma pentaphyllum is crushed, gynostemma pentaphyllum powder is obtained；
(2) step：The gynostemma pentaphyllum powder that (1) step obtains is put and is extracted in ethanol, filtrate is obtained；
(3) step：The upper resin column of the filtrate is adsorbed, after resin saturation, stops filtrate upper prop；Institute is desorbed using ethyl alcohol
The saponin(e adsorbed in resin column is stated, ethyl alcohol stripping liquid is obtained；The ethyl alcohol stripping liquid is distilled, ethyl alcohol is recycled, solid is dried,
Obtain water-soluble and liposoluble ingredient Gypenosides powder；
The resin column is by the D101 large pore resin absorption columns, the first cationic resin column, the anion that are sequentially connected in series from top to bottom
Resin column and the second cationic resin column composition；
(4) step：It is removed using the Impurity elution that resin regeneration solution is adsorbed resin, the resin is made to restore original group
At and performance.
2. the method for extraction Gypenosides according to claim 1, which is characterized in that described to be sequentially connected in series from top to bottom
D101 large pore resin absorption columns, the first cationic resin column, resin anion (R.A.) column and the second cationic resin column column volume
Ratio is 1：1：3：1.
3. the method for extraction Gypenosides according to claim 1, which is characterized in that first cationic resin column
For sulfonic group cation exchange column；The resin anion (R.A.) column is strong-base anion-exchange resin column；Second cation
Resin column is sulfonic group cation exchange column.
4. the method for extraction Gypenosides according to claim 1, which is characterized in that described (4) step includes as follows
Step：
(4.1) step：Dose volume score is 3%-7% acidity alcohol solutions；
(4.2) step：Measure the sodium hydroxide solution that dose volume score is 2%-6%；
(4.3) step：By the acidity alcohol solution upper prop, by column group series system followed by each column；When acidity alcohol solution is complete
After portion is added, pure water is sequentially added, keeps identical flow velocity, acid alcohol is all replaced, until column group end efflux PH=
When 0.67-7, stop into pure water；
(4.4) step：Close D101 macroporous resin columns, the first cationic resin column and the second cationic resin column, open it is cloudy from
Sub- resin column；Sodium hydroxide addition resin anion (R.A.) column is allowed to make the transition；After whole lye are into column, using in pure water column precipitator
Lye, until column bottom efflux PH=6.5~7 are stopped；
(4.5) step：According to column group series sequence, the ethyl alcohol for being 80%-95% with volume fraction is followed by the first cation
Resin column, resin anion (R.A.) column and the second cationic resin column, dosage 4-8BV close column group.
5. the method for extraction Gypenosides according to claim 4, which is characterized in that in (4.3) step, the acidity
Flow velocity of the alcoholic solution in column is 0.5-1.5BV/h；In (4.4) step, flow velocity of the lye in column is 0.5-1.5BV/
h；In (4.5) step, the flow velocity of ethyl alcohol that volume fraction is 80%-95% in each column is 1.5-2.5BV/h.
6. the method for extraction Gypenosides according to claim 4, which is characterized in that described (4) step further includes the
(4.6) step：The acidity alcohol solution flowed out in (4.3) step and the lye flowed out in (4.4) step are neutralized, ethyl alcohol is recycled, is remained
Remaining solid drying, cycle applications are in (2) step.
7. the method for extraction Gypenosides according to claim 1, which is characterized in that in (3) step, the filtrate
Flow velocity in resin column is 1.5-2.5BV/h；The filtrate treating capacity of the resin column is 25~30BV；Desorb resin column interior suction
The dosage of the ethyl alcohol of attached saponin(e is 3-7BV, flow velocity 1.5-2.5BV/h.
8. the method for extraction Gypenosides according to claim 1, which is characterized in that
Described (2) step includes the following steps：
(2.1) step：Gynostemma pentaphyllum powder is packed into pot for solvent extraction, the ethyl alcohol that volume fraction is 60-85%, dipping is added；Soak foot 4-8
After hour, liquid is discharged, filters, obtains liquid；The ethyl alcohol that volume fraction is 60-85% is added in second time dipping, impregnates 3-7
Hour, filtering obtains liquid；Merge secondary liquid, it is spare；
(2.2) step：It is separately added into the ethyl alcohol that volume fraction is 60-85% and carries out third time and the 4th time dipping, impregnate respectively
3-7 hours；Liquid merges after coarse filtration, and cycle applications are in (2) step；
(2.3) step：The residual ethanol in the dregs of a decoction is recycled, the dregs of a decoction are continued to employ.
9. the method for extraction Gypenosides according to claim 1, which is characterized in that institute in (2) step and (3) step
The volume fraction of the ethyl alcohol used is 60-85%.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103520256A (en) * | 2013-10-15 | 2014-01-22 | 曹远东 | Preparation method of high-purity gynostemma pentaphylla total saponin for veterinary drug |
| CN104774238A (en) * | 2015-04-03 | 2015-07-15 | 泉州市奈斯材料科技有限公司 | Method for refining soapnut saponin by using ion exchange resin method |
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2018
- 2018-05-14 CN CN201810458420.2A patent/CN108310039A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103520256A (en) * | 2013-10-15 | 2014-01-22 | 曹远东 | Preparation method of high-purity gynostemma pentaphylla total saponin for veterinary drug |
| CN104774238A (en) * | 2015-04-03 | 2015-07-15 | 泉州市奈斯材料科技有限公司 | Method for refining soapnut saponin by using ion exchange resin method |
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Application publication date: 20180724 |