CN106188178A - A kind of method preparing protodioscin - Google Patents
A kind of method preparing protodioscin Download PDFInfo
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- CN106188178A CN106188178A CN201610438510.6A CN201610438510A CN106188178A CN 106188178 A CN106188178 A CN 106188178A CN 201610438510 A CN201610438510 A CN 201610438510A CN 106188178 A CN106188178 A CN 106188178A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
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Abstract
The invention belongs to pharmaceutical technology field, relate to the separating and extracting process of chemical field compound, it is specifically related to a kind of preparation method of natural plant pharmacological active substance protodioscin, including with Rhizoma Dioscoreae Nipponicae medical material as raw material, uses column chromatography method to carry out the purification of protodioscin；The process for refining of the present invention is simple, it is easy to operation, and purification efficiency is high, and Refining times is short.
Description
Technical field
The invention belongs to pharmaceutical technology field, relate to the separating and extracting process of chemical field compound, be specifically related to plant
A kind of preparation method of natural pharmacological active substance protodioscin.
Background technology
Rhizoma Dioscoreae Nipponicae is the dry rhizome of Dioscoreaceae plant Dioscorea nipponica Mak. Ningpo Yam Rhizome Dioscorea nipponica Makino, warm in nature,
Sweet in the mouth, hardship, return liver, kidney, lung meridian, has the effect of expelling wind and removing dampness, channels sootheing and network vessel quickening, promoting blood circulation and stopping pain, relieving cough and asthma.Its bubble multiplex among the people
Wine or decoction, treatment rheumatism disadvantage, arthralgia, traumatic injury and lumbar sprain and QI divergeny.Modern study shows that Rhizoma Dioscoreae Nipponicae has regulation to exempt from
Epidemic disease, cardiovascular function of improving, antitussive, relieving asthma, the multiple pharmacological effect such as eliminate the phlegm, be clinically used for treating rheumatoid arthritis, hat
Cardiopathia, hypertension, myocardial infarction, bronchial asthma.In Rhizoma Dioscoreae Nipponicae, principle active component is steroidal saponin, and steroidal saponin is main
For dioscin and protodioscin.
Protodioscin (protodioscin), molecular formula is C51H84O22, structure is shown in Fig. 1, belongs to steroidal saponin, has another name called
Furan sterin saponin, has the strongest pharmacological action, as sexual function improving, effect for reducing blood fat, to the toxic action of cancerous cell and anti-
Leukemia effect.At present, the process route not yet having a kind of applicable industrialization production simultaneously to prepare high purity raw dioscin drapes over one's shoulders
Dew.On market, the yield of protodioscin is the lowest, and yield is less, it is difficult to meets scientific research or new drug development demand, thus seriously limits
Make its further investigation.The present invention utilizes macroporous adsorbent resin column chromatography, reversed-phase silica gel column chromatography and reversed-phase resin pilum chromatography
Technology, prepares protodioscin from Rhizoma Dioscoreae Nipponicae, and purity is good, and yield is higher, develops, for it, the material base providing good.
Summary of the invention
It is an object of the invention to provide a kind of method preparing high purity raw dioscin, the inventive method not only operates
Technique is simple, with short production cycle, and utilizes the present invention can prepare purity in a technological process and reach more than 90%
Protodioscin.
In order to solve the problems referred to above, the present invention provides a kind of method preparing protodioscin, including inhaling with macropore successively
The method of attached resin column chromatography, reversed-phase silica gel column chromatography, reversed-phase resin pilum chromatography separates in Rhizoma Dioscoreae Nipponicae herbal extract
Protodioscin.
A kind of method preparing protodioscin, comprises the following steps:
1) dry Rhizoma Dioscoreae Nipponicae medical material is joined in Extraction solvent, medical material is carried out extraction process, obtain Rhizoma Dioscoreae Nipponicae and carry
Take liquid, extracting solution is concentrated, stands, filters, takes filtrate；
2) filtrate uses eluant carry out eluting process by macroporous adsorptive resins method, collect, merge containing former potato
The eluent of Chinese yam saponin, obtains resin column eluent；
3) resin column eluent is concentrated, stands, filters, obtain filtrate；
4) filtrate uses eluant pass through 1-3 reversed-phase silica gel column chromatography process, collect, detect, merge eluent；
5) being concentrated by reverse phase silica gel post eluent, concentrated solution uses reversed-phase resin pilum Image processing, collects, detects, closes
And eluent, eluent is dried, obtains protodioscin.
Described step 1) in Extraction solvent choose the ethanol solution that mass percent concentration is 20%-90%, preferably
For 50%-75% aquiferous ethanol solution.Water, methanol or aqueous methanol should not be used to extract, and document report protodioscin is used
Instability when methanol eddy extracts, it may occur that conversion reaction (sees Kostova I, Dinchev D, Rentsch G H, et
Al.Z.Naturforsch.57c, 33-38 (2002)).
Described step 1) in extraction process be to carry out extraction process, wherein, Extraction solvent by being heated to reflux
The weight ratio of volume and medical material is 5-8: 1, and (if the weight of i.e. medical material is 1kg, then the volume of Extraction solvent is 5-8L；If
The weight of medical material is 1g, then the volume of Extraction solvent is 5-8mL)；Extraction time is 2-3 time, preferably 2 times；Extraction time is
2-3h/ time；It addition, step 1) described in be concentrated by extracting solution be that extracting solution is concentrated into relative density is 1.0-1.2；Described
Standing be concentrated extracting solution is stood overnight (the relative density scope of concentrated extracting solution and time of repose be conducive to impurity sink
Form sediment completely, it is simple to prepared by aftermentioned separation).
Described step 2) in the used D101 of macroporous adsorbent resin, AB-8, DM130H, XAD-2, D201, HP-20,
One in X-5, H103, DM11 or ADS-17 type resin, preferably HP-20, AB-8, D101 type macroporous adsorbent resin；Loading
Ratio is chosen as: the volume of macroporous adsorbent resin is 0.5-1.5: 1 with the ratio of Rhizoma Dioscoreae Nipponicae medical material weight (dry weight), i.e. works as Rhizoma Dioscoreae Nipponicae
Medical material weight is 100kg, then the column volume of macroporous resin column is 50-150L, preferably 0.7-1.0: 1；Further, macropore tree
During fat post separating treatment, the column diameter of macroporous resin column is 1: 8-20 with the ratio of post height.
Described step 2) in eluant choosing use water and aqueous ethanol solution successively, be flushing liquor initially with water
Being rinsed, the ethanol solution then using mass percent concentration to be 20%-50% is that eluant carries out eluting, collects, closes
And the resin column eluent containing protodioscin；Wherein, step 2) in adopt water as during flushing liquor is rinsed, water
It is 2-6: 1 with the ratio of the volume of macroporous adsorbent resin, preferably 2-3.5: 1；Using described ethanol solution is that eluant is washed
During Tuo, ethanol solution is 4-6: 1 with the ratio of the volume of macroporous adsorbent resin.
Step 3) described in by containing protodioscin eluent concentrate, it is 1.0-that extracting solution is concentrated into relative density
1.2；Described standing, can stand overnight concentrated extracting solution that (the relative density scope of concentrated extracting solution and time of repose have
It is beneficial to contamination precipitation complete, it is simple to prepared by aftermentioned separation).
Described step 4) in reversed-phase silica gel column chromatography use C18Reversed-phase column, described C18Reversed-phase column can be selected for prepackage
Post or DAC prepare post；Wherein, step 4) described in reverse phase silica gel post separate, be that eluant carries out eluting, then initially with water
The acetonitrile solution using mass percent concentration to be 10%-50% is that eluant carries out gradient elution, collects, merges containing former potato
The eluent of Chinese yam saponin or be that eluant carries out eluting initially with water, then using mass percent concentration is 20%-
The ethanol solution of 60% is that eluant carries out eluting, collects, merges the eluent containing protodioscin；Wherein, step 4) in
For the second time in reversed-phase silica gel column chromatography processing procedure, selecting acetonitrile is eluant with the mixed solvent of water, described acetonitrile solution
Mass percent concentration be 28%-40%, preferably 28%-35%.
When carrying out reversed-phase column separation, aquiferous ethanol is used repeatedly as eluting solvent or to contain water-acetonitrile as eluting solvent phase
In conjunction with, can further improve the purity of protodioscin；Such as, first use aquiferous ethanol as eluant, re-use aqueous second
Nitrile can reach more than 90% as eluant, the protodioscin purity obtained.As further used reversed phase column chromatography, use
Aquiferous ethanol or carry out eluting containing water-acetonitrile, can improve the purity of protodioscin further.
Further, step 3) and step 4) described in the eluent containing protodioscin is concentrated, by extracting solution
Being concentrated into relative density is 1.0-1.2.
Reversed-phase resin based filler is than traditional C18Silica gel has higher chemical stability, can be at strong acid, highly basic medium
Lower use, can use in higher concentrations with multiple organic solvent as eluant, and the life-span is the longest；Anti-phase tree
Aliphatic radical filling adsorption amount is high, and granule is uniform, and mechanical strength is good, the most broken, and residue is few, with the C of same particle size18Fixing phase
Post effect quite, no matter to polarity or nonpolar sample, almost without Irreversible Adsorption, is highly suitable for preparative hplc isolated and purified micro-
Quantity of material, and C8And C18Post is due to the existence of silanol base, in sample Irreversible Adsorption to pillar, makes the response rate low.
In the present invention, reversed-phase resin pilum is used to chromatograph, i.e. further the product of reversed-phase silica gel column chromatography isolated
Step 5 described) in employing reversed-phase resin pilum chromatography, to improve further the purity of protodioscin；Selected anti-
Phase resin based filler can be the one in SMB, MCI, GEL, PRP type reversed-phase resin base chromatographic column, and pillar specification selects prepackage
Post or or DAC prepare post；Wherein, step 5) described in reversed-phase resin pilum Image processing during select the mixed of acetonitrile and water
Bonding solvent is eluant, and the mass percent concentration of the solution of its acetonitrile is 15%-35%.
Further, described Rhizoma Dioscoreae Nipponicae medical material is Chinese yam section plant Dioscorea nipponica Mak. Ningpo Yam Rhizome Dioscorea nipponica Makino
Dry rhizome.
The reverse phase silica gel particle diameter used due to reversed-phase silica gel column chromatography also has considerable influence, in theory, grain to separating effect
The reverse phase silica gel that particle diameter is the least, separating effect is the best, but post pressure can be significantly raised, and the requirement to equipment increases the most accordingly, and
The cost of reverse phase silica gel also can dramatically increase, so the reverse phase silica gel that the present invention preferred reverse phase silica gel particle diameter is 40-60 μm.
Also there is considerable influence in the reversed-phase resin basal granule footpath used due to reversed-phase resin pilum chromatography to separating effect, theoretical
On, the resin based filler that particle diameter is the least, separating effect is the best, but post pressure can be significantly raised, and the requirement to equipment increases the most accordingly
Add, and filler cost also can dramatically increase, so the reversed-phase resin based filler that preferable particle size of the present invention is 50-70 μm.
Wherein protodioscin purity detecting is as follows: sample through high performance liquid chromatograph at chromatographic condition is: flowing is mutually
Acetonitrile-water (26: 74), wavelength 203nm, chromatographic column is Kromasir C18Chromatographic column (4.6mm × 250mm, 5 μm), flow velocity is
1.0mL·min-1, column temperature is to detect at 35 DEG C, and sample is single symmetrical peak in HPLC chromatogram, area normalization method measure,
Purity is more than 98%, and chromatogram is shown in Fig. 2.
The method that protodioscin structure determines is as follows: uses nuclear magnetic resonance, NMR POP instrument, is analyzed sample, wherein
13C-NMR (400MHz, Pyridine-d5) δ: 37.5 (C-1), 30.2 (C-2), 78.2 (C-3), 39.0 (C-4), 140.9 (C-
5), 121.8 (C-6), 32.4 (C-7), 31.7 (C-8), 50.4 (C-9), 37.1 (C-10), 21.1 (C-11), 40.0 (C-12),
40.8 (C-13), 56.6 (C-14), 32.5 (C-15), 81.1 (C-16), 63.8 (C-17), 16.5 (C-18), 19.4 (C-19),
40.7 (C-20), 16.3 (C-21), 110.7 (C-22), 37.1 (C-23), 28.3 (C-24), 34.3 (C-25), 75.2 (C-
26), 17.4 (C-27)；C-3 sugar: 100.3 (GlcC-1 '), 77.9 (GlcC-2 ' (inner)), 78.2 (GlcC-3 '), 79.0
(Glc C-4 '), 76.8 (GlcC-5 ') 61.4 (GlcC-6 ')；102.0 (RhaC-1 "), 72.4 (RhaC-2 " (1 → 2)), 72.8
(Rha C-3 "), 74.1 (RhaC-4 "), 69.4 (RhaC-5 "), 18.4 (RhaC-6 "), 102.9 (Rha C-1 " '), 72.4
(Rha C-2 " ' (1 → 2)), 72.7 (Rha C-3 " '), 73.9 (Rha C-4 " '), 70.5 (Rha C-5 " '), 18.6 (Rha C-
6″′)；C-26 sugar moieties: 104.9 (Rha C-1 " '), 75.2 (Rha C-2 " '), 78.3 (RhaC-3 " '), 71.8 (RhaC-
4 " '), 78.6 (RhaC-5 " '), 62.9 (RhaC-6 " '),13C-NMR and13H-NMR reports nuclear-magnetism with the document of protodioscin
Data consistent, is accredited as protodioscin (protodioscin).
Beneficial effect: advantages of the present invention comprise following some:
1) application the inventive method, can prepare highly purified protodioscin, and protodioscin content reaches 90-
99.9%；
2) application the inventive method, the protodioscin of available feather weight；
3) process of preparing of the present invention is simple, and purification efficiency is high, consumes energy low, environmental protection, and operating procedure condition is easily controlled,
Quality controllability is strong；
4) the comprehensive reversed-phase silica gel column chromatography of the present invention and the isolation technics of reversed-phase resin pilum chromatography, yield is high, the removal of impurity
Effective with pigment；
5) high purity raw dioscin of the present invention, no solvent residue, safety is high, can be separately as preparing medicine
Product and the raw material of health product, it is possible to use to relevant pharmacological component mutual reinforcement between, to reach the merit of Synergistic.
Accompanying drawing explanation
Fig. 1 is the protodioscin structure chart of the present invention.
Fig. 2 is the protodioscin sample purity detection chromatogram of the present invention.
Detailed description of the invention
Below by specific embodiment, the present invention is further described:
Specific embodiment one:
Prepare the Rhizoma Dioscoreae Nipponicae medical material 150kg being dried, after being ground into coarse powder, load in rustless steel Chinese medicine extracting tank, use quality
Percent concentration is 70% ethanol solution, heating and refluxing extraction 3 times, each 8 times amount, each 2h；Secondly, united extraction liquid, mistake
Filter, filtrate reduced in volume to relative density is 1.08 (40 DEG C), lets cool, and after standing overnight, filters, and filtrate is through AB-8 macroporous absorption
Resin column chromatographs, and in macroporous adsorptive resins, the column volume of macroporous adsorbent resin is 200L (column diameter 0.4m, post height 1.6m), its
After center pillar volume refers to macroporous adsorbent resin dress post, from the base plate of post to the volume on pitch deposition surface；Resin in resin column
Volume is 4: 3 with the ratio of medical material weight (dry weight), after filtrate fully flows into resin column, first washs with the water of 2.5 times of column volumes
To effluent as clear as crystal after, then with the ethanol solution elution wash that mass percent concentration is 20% of 3 times of column volumes to stream
Go out liquid as clear as crystal after, be then followed by with the ethanol solution eluting that mass percent concentration is 20% of 5 times of column volumes, collection is washed
De-liquid, elution flow rate is 150L/h, and every 50L eluent is collected as a flow point, liquid phase tracing detection, merges containing protodioscin
Stream part, obtains macroporous resin column eluent.It is 1.13 (40 DEG C) that macroporous resin column eluent is evaporated to relative density, puts
Cold, stand overnight, take supernatant；Then by supernatant through C18Post (diameter 500mm, highly 800mm, 50-70 μm) column chromatography, point
Do not wash with water, 25% acetonitrile eluting, 34% acetonitrile eluting, liquid phase tracing detection, merge containing stream part of protodioscin, dense
Contracting；Carry out second time C again18Post (100mm × 250mm, 50 μm) column chromatography, respectively with 25% acetonitrile and 34% acetonitrile eluting, liquid
Phase tracing detection, merges the stream part containing protodioscin, concentrates；Then reversed-phase resin pilum (200mm × 250mm, 50 μ are utilized
M) separate, successively with 25% acetonitrile and 30% acetonitrile eluting, liquid phase tracing detection, merge target flow point, decompression and solvent recovery is extremely
Dry, lyophilization, obtain protodioscin 0.72 kilogram (purity 95.2%).
Specific embodiment two:
Prepare the Rhizoma Dioscoreae Nipponicae medical material 90kg being dried, after being ground into coarse powder, load in rustless steel Chinese medicine extracting tank, by quality hundred
Proportion by subtraction concentration is 50% ethanol solution, heating and refluxing extraction 3 times, each 8 times amount, each 2h.United extraction liquid, filters, filtrate
Being evaporated to relative density is 1.01 (40 DEG C), lets cool, and after standing overnight, filters, and filtrate is through AB-8 macroporous adsorptive resins
Chromatography, in macroporous adsorptive resins, the column volume of macroporous adsorbent resin is 120L, and wherein column volume refers to that macroporous adsorbent resin fills
After post, from the base plate of post to the volume on gel deposition surface.After filtrate fully flows into resin column, first with 2.5 times of column volumes
Water washing to effluent as clear as crystal after, then wash with the ethanol solution eluting that mass percent concentration is 20% of 3 times of column volumes
Wash to effluent as clear as crystal after, be then followed by with the ethanol solution eluting that mass percent concentration is 30% of 5 times of column volumes,
Collecting eluent, elution flow rate is 90L/h, and every 50L eluent is collected as a flow point, liquid phase tracing detection, merges containing former Rhizoma Dioscoreae
Stream part of saponin, being evaporated to relative density is 1.07 (40 DEG C), lets cool, stands overnight, takes supernatant；Then by supernatant
Through C18Post (200mm × 250mm, 50-70 μm) column chromatography, washes with water, 25% acetonitrile eluting, 34% acetonitrile eluting respectively, liquid
Phase tracing detection, merges, and merges the stream part containing protodioscin, and being evaporated to relative density is 1.11 (40 DEG C), lets cool, so
After utilize reversed-phase resin pilum (200mm × 250mm, 70 μm) to separate, successively with 20% acetonitrile and 30% acetonitrile eluting, liquid phase with
Track detects, and merges target flow point, and decompression and solvent recovery is the most dry, and lyophilization obtains 0.4 kilogram of (purity of protodioscin
91.2%).
Specific embodiment three:
Prepare the Rhizoma Dioscoreae Nipponicae medical material 120kg being dried, after being ground into coarse powder, load in rustless steel Chinese medicine extracting tank, use quality
Percent concentration is 70% ethanol solution, heating and refluxing extraction 3 times, each 8 times amount, each 2h.United extraction liquid, filters, filter
It is 1.05 (40 DEG C) that liquid is evaporated to relative density, lets cool, and after standing overnight, filters, and filtrate is through AB-8 macroporous adsorbent resin
Column chromatography, in macroporous adsorptive resins, the column volume of macroporous adsorbent resin is 160L, and wherein column volume refers to macroporous adsorbent resin
After dress post, from the base plate of post to the volume on gel deposition surface；After filtrate fully flows into resin column, first with 2.5 times of column volumes
Water washing to effluent as clear as crystal after, then with the ethanol solution eluting that mass percent concentration is 20% of 3 times of column volumes
Wash to effluent as clear as crystal after, be then followed by washing with the ethanol solution that mass percent concentration is 20% of 5 times of column volumes
De-, collect eluent, elution flow rate is 120L/h, and every 50L eluent is collected as a flow point, liquid phase tracing detection, merges containing former
Stream part of dioscin, being evaporated to relative density is 1.07 (40 DEG C), lets cool, stands overnight, takes supernatant；Then by upper
Clear liquid is through C18Post (500mm × 800mm, 50-70 μm) column chromatography, washes with water, 35% ethanol elution, 55% ethanol are washed respectively
De-, liquid phase tracing detection, merge the stream part containing protodioscin, concentrate, carry out second time C18Post (500mm × 800mm, 50-70
μm) column chromatography, respectively with 25% acetonitrile and 32% acetonitrile eluting, liquid phase tracing detection, merge the stream part containing protodioscin, subtract
It is 1.14 (40 DEG C) that pressure is concentrated into relative density, lets cool, and then utilizes reversed-phase resin pilum (200mm × 250mm, 70 μm) point
From, successively with 20% acetonitrile and 30% acetonitrile eluting, liquid phase tracing detection, merge target flow point, decompression and solvent recovery is to dry, cold
Lyophilizing is dry, obtains protodioscin 0.55 kilogram (purity 96.8%).
Specific embodiment four:
First the step first passing through specific embodiment one obtains protodioscin 0.5 kilogram, then dissolves with 20% ethanol,
Then through C18Post (500mm × 800mm, 50-70 μm) column chromatography, successively with 450L 20% ethanol elution, 450L 40% ethanol
Eluting, 750L 50% ethanol elution, liquid phase tracing detection, merge the stream part containing protodioscin, decompression and solvent recovery is the most dry,
Lyophilization, obtains protodioscin 0.43 kilogram (purity 98.7%).
The above, be only presently preferred embodiments of the present invention, and not the technical scope to the present invention makes any limit
System, therefore every any trickle amendment, equivalent variations and modification above example made according to the technical spirit of the present invention, all
Still fall within the range of technical scheme.
Claims (9)
1. the method preparing protodioscin, it is characterised in that: include successively with macroporous adsorbent resin column chromatography, anti-phase silicon
The method of plastic column chromatography, reversed-phase resin pilum chromatography separates the protodioscin in Rhizoma Dioscoreae Nipponicae herbal extract.
2. the method preparing protodioscin, it is characterised in that: comprise the following steps:
1) dry Rhizoma Dioscoreae Nipponicae medical material is joined in Extraction solvent, medical material is carried out extraction process, obtain Rhizoma Dioscoreae Nipponicae extracting solution,
Extracting solution is concentrated, stands, filters, takes filtrate；
2) filtrate uses eluant carry out eluting process by macroporous adsorptive resins method, collect, merge containing former Rhizoma Dioscoreae soap
The eluent of glycosides, obtains resin column eluent；
3) resin column eluent is concentrated, stands, filters, obtain filtrate；
4) filtrate uses eluant pass through 1-3 reversed-phase silica gel column chromatography process, collect, detect, merge eluent；
5) being concentrated by reverse phase silica gel post eluent, concentrated solution uses reversed-phase resin pilum Image processing, collects, detects, merges and wash
De-liquid, eluent is dried, obtains protodioscin.
A kind of method preparing protodioscin the most according to claim 2, it is characterised in that: described step 1) in
It is 20%-90% aquiferous ethanol solution that Extraction solvent chooses mass percent concentration, and preferably 50%-75% aquiferous ethanol is molten
Liquid.
A kind of method preparing protodioscin the most according to claim 2, it is characterised in that: described step 1) in
Extraction process is to carry out extraction process by being heated to reflux.
A kind of method preparing protodioscin the most according to claim 2, it is characterised in that: described step 2) in
Macroporous adsorbent resin used D101, AB-8, DM130H, XAD-2, D201, HP-20, X-5, H103, DM11 or ADS-17 type tree
One in fat.
A kind of method preparing protodioscin the most according to claim 2, it is characterised in that: described step 2) in
Eluant uses water and aqueous ethanol solution successively.
A kind of method preparing protodioscin the most according to claim 2, it is characterised in that: described step 4) in
Reversed-phase silica gel column chromatography uses C18Reversed-phase column, described C18Reversed-phase column is the prepacked column with reverse phase filler as carrier or prepared by DAC
Post.
A kind of method preparing protodioscin the most according to claim 2, it is characterised in that: described step 5) in
Reversed-phase resin pilum chromatography selects the one in SMB, MCI, GEL, PRP type reversed-phase resin base chromatographic column, in pillar specification selects
The prepacked column of footpath 5cm or the prepacked column of internal diameter 10cm or DAC prepare post.
A kind of method preparing protodioscin the most according to claim 2, it is characterised in that: described step 4) in
The eluant of 1-3 reversed phase column chromatography process is aqueous acetonitrile solution or aquiferous ethanol solution.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111116700A (en) * | 2019-11-25 | 2020-05-08 | 华南农业大学 | Method for extracting, separating and purifying dioscin from chrysanthemum leaves |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111116700A (en) * | 2019-11-25 | 2020-05-08 | 华南农业大学 | Method for extracting, separating and purifying dioscin from chrysanthemum leaves |
| CN111116700B (en) * | 2019-11-25 | 2021-08-03 | 华南农业大学 | Method for extracting, separating and purifying dioscin from chrysanthemum leaves |
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Application publication date: 20161207 |
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| WD01 | Invention patent application deemed withdrawn after publication |