CN106860631A - A kind of method for efficiently separating purifying jujuboside - Google Patents
A kind of method for efficiently separating purifying jujuboside Download PDFInfo
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- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/72—Rhamnaceae (Buckthorn family), e.g. buckthorn, chewstick or umbrella-tree
- A61K36/725—Ziziphus, e.g. jujube
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Abstract
The present invention relates to a kind of method for efficiently separating purifying jujuboside, it is by after the type macroporous absorbent resin complete swellings of nonpolar D 101 with deionized water, ultrasonically treated 30min, is dried under vacuum to 10~30wt% of water content, then impregnate to complete swelling with methyl alcohol, wet method preparative chromatography post, add the thick saponin(e of spina date seed methanol extract liquid fully adsorb, with methyl alcohol as eluent, be eluted to eluent it is colourless after, collect eluent, the jujuboside that evaporation solvent is purified.When the inventive method solves the type macroporous absorbent resins of nonpolar D 101 and isolates and purifies jujuboside, the adsorption-desorption rate of resin is low, the problem for causing jujuboside purity low, and, up to more than 45%, desorption efficiency is up to more than 85% for jujuboside purity.
Description
Technical field
The invention belongs to the separating and purifying technology field of natural extracts, it is related to a kind of using macroporous absorbent resin pair
The method that the thick saponin(e of spina date seed of extraction is further isolated and purified.
Background technology
Spina date seed be Rhamnaceae jujube wild jujube (Ziziphus jujubeVar. spinosa) drying and ripening kind
Benevolence, be《Chinese Pharmacopoeia》Record Chinese medicine.
Jujuboside have tranquilizing soporific, be depressured, resist myocardial ischemia, reducing blood lipid, atherosclerosis, shield brain and
The pharmacological actions such as anti peroxidation of lipid.Jujuboside belongs to tetracyclic triterpene saponins, and it mainly includes Saponin A, acid
Jujube kernel saponin(e B, Spine Date Seed jujubosideB 1, jujuboside E, jujuboside D, jujuboside H etc. ten is several.
The thick saponin extraction method of the most frequently used spina date seed is solvent extraction method.To improve the recovery rate of extractant, typically
Need to introduce semi-bionic extraction method, multiplex-enzyme extraction, microwave radiation exaraction, ultrasonic wave added in the extraction process of the thick saponin(e of spina date seed
The auxiliary extraction technology means such as extraction or ultra high pressure extraction.But, the thick saponin(e of spina date seed extracted using above-mentioned various methods
Purity is also only capable of reaching 5.3~18.3%.
The purity of jujuboside is very big for its application influence limitation.Therefore, the extraction purification skill of jujuboside
Art is just able to safety, the key of wide popularization and application as it.
At present, scholars have carried out extensive work with regard to improving the DNA purity and recovery rate of jujuboside.More into
The ripe jujuboside method that isolates and purifies mainly has n-butanol extraction, ultrafiltration, preparative high performance liquid chromatography and big
Macroporous adsorbent resin method etc..Wherein, macroporous absorbent resin has physical chemistry steady due to its internal three dimensions solid pore structure
Qualitative high, specific surface area is big, aperture and the features such as big pore volume, and the adsorption capacity of resin is big, selectivity is good, adsorption rate is fast, solution
Mild condition is inhaled, is widely used in isolating and purifying for jujuboside.Commonly use and there is preferably separation to jujuboside
The macroreticular resin of purification effect has D-101, SP700, HPD-100, AB-8 and ADS-7 etc..
The factor that influence macroporous absorbent resin isolates and purifies jujuboside effect is a lot.Lot of documents report, resin
Polarity is one of key influence factor.
Nonpolar D-101 types macroporous absorbent resin is in the isolating and purifying of jujuboside using more.
(purification with macroreticular resin spina date seed total saposins technical study [J] the China Dispensaries, 2006,17 such as Lee fruit
(15):Wet D-101 types purification with macroreticular resin spina date seed total saposins 1191-1193.) are used, with washing for spina date seed total saposins
De- rate and refined degree etc. are index, show that optimum process condition and parameter are distillation from the composition and wash-out precedence of eluent
Water, 30% ethanol, each 3BV of 70% ethanol, are eluted successively with the speed of 1BV/h, collect 70% alcohol elution, the total soap in this position
The refined degree of glycosides has reached 208.4%.
It is different from, Cui Ying etc. (purification with macroreticular resin wild jujube kernel alcohol extractive technical study [J] Chinese patent drugs,
2009, 31(7):1035-1037.) the D-101 type purification with macroreticular resin jujubosides to do, while limiting wild jujube
Saponin concentrations in benevolence crude extract, with orthogonal test, (investigating factor includes resin demand, adsorption flow rate, eluate concentration, wash-out
Liquid consumption) show that the optimum process condition for purifying jujuboside is：The dried resin of 1 times of amount crude drug adsorbs the liquid of 0.2g/mL,
Rate of adsorption 2.2mL/min (i.e. 100mL liquid 2.5h), 50% ethanol elution of 4BV collects eluent.Now solid content purity
Highest, purity (41.43%) is not 3.85 times of purity (10.77%) before purification after purification.
Further to improve the purity of jujuboside, CN 101401855A increased the preprocessing process to resin, i.e.,
In 100g D-101 type macroporous absorbent resins plus 1000mL 95% ethanol, 24h is soaked, with 95% ethanol elution to 1 part of efflux
Plus untill 5 parts of water occur without muddiness, then be eluted to without alcohol taste with distilled water, flow velocity is 2ml/min.With the purifying resin for pre-processing
Wild jujube kernel alcohol extractive, jujuboside content 2.47% in solid content.
In sum, for nonpolar D-101 types macroporous absorbent resin, what the eluent in purifying jujuboside was used
All it is the aqueous solution of ethanol, but recovery rate and purity are all unsatisfactory.
Other nonpolar macroporous adsorption resins also have certain application in the isolating and purifying of jujuboside.
Fourth Ke etc. (research [J] the ion exchanges of total triterpene saponins and absorption in SP700 macroporous resin purification spina date seeds,
2011, 27(1):33-42.) filtered out from the different macroreticular resin of 7 kinds of polarity a kind of has to spina date seed total triterpene saponins
The nonpolar SP700 resins of good adsorption and desorption performance.Jujuboside is adsorbed after reaching balance on resin, uses volume integral
The ethanol solution that number is respectively 50% and 90% carries out stepwise elution, and wash-out yield highest can reach 95.1%, purified rear saponin(e
Content improves 4 times.
Li Jiaying etc. (purification with macroreticular resin jujuboside technical study [J], contemporary Chinese medicinal application,
2013, 11, 7(22):237.) nonpolar HPD-100 purification with macroreticular resin spina date seed total saposins are selected, it is enriched in
70% ethanol eluate position, eluting rate is 91.77%, and it is 298.75% to refine degree, and the refined degree of Saponin A is
266.53%, the rate of recovery 91.77%.
(extraction and purification process of jujuboside studies [J] Chinese medicines, 2005,28 to Wu Yulan etc. in Semen Ziziphi Spinosae (parched)
(3):HPD-100 type macroporous absorbent resins 219-223.) are also using in jujuboside extraction and purification process, is drawn
Optimal purifying process condition is：Impurity is first washed away successively with 150mL 10.5%NaOH solution and 150mL ethanol, then uses 50mL
70% ethanol elution, up to 17.9%, eluting rate reaches 72.8% to Saponin A purity.
As can be seen here, nonpolar macroporous adsorption resin is applied to jujuboside and isolating and purifying, but all exists and to be difficult to
Wash-out and the low problem of purity.
And for the macroporous absorbent resin of low pole, also have during the isolating and purifying of jujuboside it is certain should
With.
CN 101322758A disclose the side that a kind of low pole AB-8 type macroporous absorbent resins isolate and purify jujuboside
Method, be by concentration for 4.5mg/mL spina date seed extract solution with the flow velocity of 2mL/min in AB-8 macroporous absorbent resins (chromatographic column footpath
Height is than being 1: after 10) adsorbing, first washes polysaccharide impurity with water, then with 30~70% ethanol solution gradient elutions, collect wash-out
Liquid, 60~65 DEG C of rotary evaporation concentrations, vacuum drying obtains the extract of spina date seed total saposins >=40%.
And (purification with macroreticular resin technique [J] China reality of the preferred jujuboside of orthogonal design such as Yang Junxuan
Test pharmacology of traditional Chinese medical formulae magazine, 2012,18 (12):63-66.) then select polarity ADS-7 type purification with macroreticular resin spina date seed soaps
Glycosides, show that optimum process condition and parameter are post blade diameter length ratio 3: 1, quality of liquid medicine concentration 1.0g/mL, absorption speed by orthogonal test
Rate 1.0BV/h, resin crude drug adsorbance 0.4g/g, elute the ethanol of solvent 70%, elution rate 2BV/h.
From above-mentioned prior art literature, scholars' high spot reviews resin polarity, sample concentration, blade diameter length ratio, wash-out
Influence of the factors such as liquid to jujuboside purification degrees, and based on experiment, optimization isolates and purifies the resin of jujuboside
The correlation optimum process condition such as polarity and eluent.After purifying resin, the purity of jujuboside is only capable of reaching 17.9~
41.4%。
It is well known, however, that macroporous absorbent resin is that organic substance is selectively adsorbed from solution by physical absorption,
So as to reach the purpose of separating-purifying.This absorption property is the result of Van der Waals force or generation hydrogen bond.Simultaneously as macropore
The loose structure of polymeric adsorbent, makes its material different to molecular size be acted on screening.It is former according to above-mentioned absorption and screening
Reason, size and resin according to organic compound molecule amount and polarity are passed through to the difference of its absorption affinity on macroporous absorbent resin
Certain solvent wash-out, you can the purpose different to reach separation, purifying, removal of impurities, concentration etc..
It follows that the adsorption of macroporous absorbent resin and target molecule, the size of target molecule, and macropore are inhaled
The aperture of attached resin just turns into the key factor for influenceing it to isolate and purify effect.And the work between macroporous absorbent resin and target molecule
Or actually firmly Van der Waals force generation hydrogen bond, and macroporous absorbent resin the physical parameter such as aperture, can be by right
Resin carries out relevant characterization and obtains.After specify that the chemical structural formula of target molecule simultaneously, it becomes possible to probe into macroporous absorption tree
Fat isolates and purifies the process nature of jujuboside, so that the related property by changing macroporous absorbent resin, improves it to acid
The purification degrees and absorption-desorption rate of jujube kernel saponin(e.
On macroporous absorbent resin in the method using preceding being pre-processed, only mentioned first in CN 101401855A,
Its preprocessing process is also only simple solvent soaking with washing.However, macroporous absorbent resin is before and after solvent soaking washing, with
And before and after being adsorbed to jujuboside, whether the requirement of exchange of solvent is really achieved in its aperture, or pore size is
No to change, the purification degrees for improving jujuboside have very important influence, but related content has no document
Report.
Therefore, existing macroporous absorbent resin isolates and purifies the method for jujuboside and remains that DNA purity is low, carries
The defect such as pure efficiency is low, the rate of recovery is low, solvent load is big.
The content of the invention
It is an object of the invention to provide a kind of method for efficiently separating purifying jujuboside, to solve using nonpolar D-
When 101 type macroporous absorbent resins isolate and purify jujuboside, the absorption-desorption rate of macroporous absorbent resin is low, causes spina date seed
The low problem of saponin(e purity.
The method for efficiently separating purifying jujuboside of the present invention is by nonpolar D-101 types macroporous absorption tree
The method that fat is pre-processed, improves the absorption property of nonpolar D-101 types macroporous absorbent resin, by improving macroporous absorption tree
Utilization rate of the fat during jujuboside is isolated and purified, improves adsorbance of the jujuboside on resin, desorption efficiency and
Jujuboside purity also significantly improves, to realize efficiently separating the purpose of purifying jujuboside.
Specifically, the present invention is to efficiently separate purifying using what following methods realized jujuboside：By nonpolar D-101
Type macroporous absorbent resin is placed in deionized water and impregnates to complete swelling, ultrasonically treated 30min, and 70~90 DEG C are dried under vacuum to contain
10~30wt% of water, then be placed in methyl alcohol and impregnate to complete swelling, wet method preparative chromatography post adds the first of the thick saponin(e of spina date seed
Alcohol extract is fully adsorbed, with methyl alcohol as eluent, be eluted to eluent it is colourless after, collect eluent, evaporation solvent methyl alcohol obtains
To the jujuboside of purifying.
Wherein, the nonpolar D-101 types macroporous absorbent resin that the present invention is used is the opaque spherical particle of milky, particle diameter
0.5~1.25mm, 60~75wt% of resin initial water content.
Usually, the nonpolar D-101 types macroporous absorbent resin that the water content is 60~75wt% is placed in deionized water
24~36h of middle dipping, you can ensure resin complete swelling.
The present invention carries out ultrasonically treated to the macroporous absorbent resin after complete swelling, it is therefore an objective to make hydrone as much as possible
Into in resin duct, while increasing the aperture of resin and pore volume, in its preparation process in removal resin surface and duct
In residual substance.The ultrasonically treated ultrasonic wave for preferably using 100~250W of power is processed.
Then, described ultrasonically treated and dried nonpolar D-101 types macroporous absorbent resin is soaked in methyl alcohol
The time of stain is also 24~36h, can equally make resin complete swelling.
Preferably, in the methanol extract liquid of the thick saponin(e of spina date seed for being used in the present invention, the concentration of jujuboside is 1.0
~5.0mg/mL.
The methanol extract liquid of the thick saponin(e of above-mentioned spina date seed is added the upper prop volume of chromatographic column to be preferably chromatographic column by the present invention
0.05~0.25 times of the macroporous absorbent resin volume of interior filling.
And then, after the macroporous absorbent resin is packed into chromatographic column by the present invention, the blade diameter length ratio of the resin column of formation is preferred
It is 1: 10~1: 1.
After the methanol extract liquid of the thick saponin(e of the spina date seed is added into chromatographic column, fully adsorbed with macroporous absorbent resin and contacted
After 12~48h, you can jujuboside is fully adsorbed on macroporous absorbent resin, it is possible to use eluant methanol is to spina date seed
Saponin(e is eluted.
During jujuboside is eluted, the elution flow rate of the eluent is preferably 0.3~0.8BV/ to the present invention
h.Under above-mentioned condition, as long as using the eluent of 3~5BV, you can the jujuboside that will be adsorbed on chromatographic column is all under wash-out
Come.
In elution process, due to showing obvious yellow containing other impurities in the eluent of preceding 0.5~1BV.Therefore originally
After invention discards this elution fractions, remaining eluent is collected.The above-mentioned eluent being collected into is colourless, ensure that wild jujube
The purity of benevolence saponin(e.
Saponin content in the jujuboside for preparing is determined using HPLC methods, calculating its product purity can reach
More than 45%, desorption efficiency can reach more than 85%.
What the present invention was provided efficiently separates the method for purifying jujuboside first using the nonpolar D-101 of ultrasonication
Type macroporous absorbent resin, the nonpolar D-101 types macroporous absorbent resin in water is impregnated in using intensified by ultrasonic wave, uses up hydrone
In entrance resin duct more than possible, the aperture of resin and pore volume are increased, be effectively improved resin adsorption performance, make spina date seed soap
Glycosides molecule enters resin duct and adsorbs on resin.
Secondly, be vacuum dried for the resin of ultrasonically treated mistake by the present invention, controls its water content for 10~30wt%, is made
Resin duct is contained within a small amount of hydrone, and hydroxyl (associated water) content on surface is moderate, then after methyl alcohol dipping, the water in resin
The bigger hydrogen bond system of spatial volume is formed between molecule and methanol molecules, is increased and hydrogen bond is formed between solvent and jujuboside
Specific surface, enhances absorption affinity (association hydrone and methanol molecules hydroxyl and the spina date seed soap of jujuboside molecule and resin
With Hydrogenbond between glycosides molecules hydroxyl groups), further improve absorption property of the resin to jujuboside molecule.Meanwhile, this hair
It is bright to be also modified by eluent, effectively improve desorption effect of the eluent to jujuboside molecule.
The inventive method is making full use of ultrasonic wave to strengthen resin, improves nonpolar D-101 types macroporous absorption tree
While the aperture of fat and pore volume, the association water content in nonpolar D-101 types macroporous absorbent resin duct and presence are improved
Form, and jujuboside is extracted as eluent with the methanol solution being modified, the method for foundation has solid-liquid separation efficiency high, molten
Agent consumption is few, low cost, the jujuboside purity for extracting advantage high.
Specific embodiment
Specific embodiment of the invention is further described with reference to embodiment.Following examples are only used for more
Technical scheme is clearly demonstrated, rather than limiting the scope of the invention.Those of ordinary skill in the art are not
In the case of departing from the principle of the invention and objective, various change, modification, replacement and the modification carried out for these embodiments,
Should be included within protection scope of the present invention.
Embodiment 1.
0.5~1.25mm of particle diameter, the nonpolar D-101 types macroporous absorbent resin 20g of initial water content 60% are taken, is placed in
24h is impregnated in 100mL deionized waters, after making its complete swelling, with the ultrasonically treated 30min of the ultrasonoscope of power 100W.Will place
Resin after reason is vacuum dried 3h in 80 DEG C, to water content 20%, takes 10g and is placed in 150mL methyl alcohol and impregnate 24h, makes it completely molten
It is swollen.
Internal diameter 2cm, the chromatographic column of 24cm high are taken, the above-mentioned macroporous absorbent resin handled well is filled into post in a wet process, methyl alcohol is washed
To efflux without muddiness.
The thick saponin(e methanol solution 5mL of spina date seed of concentration 2.0mg/mL is taken, is added in chromatographic column, make solution abundant with resin
After contact 24h, with the methanol solution of 3BV as eluent, with the elution flow rate drip washing chromatographic column of 0.3BV/h.Discard preceding 40mL
Eluent, collects colourless solution part thereafter, and evaporation solvent methyl alcohol obtains jujuboside 3mg.
Product, the purity 51.3% of jujuboside, desorption efficiency 91% are determined with HPLC methods.
Embodiment 2.
0.5~1.25mm of particle diameter, the nonpolar D-101 types macroporous absorbent resin 20g of initial water content 75% are taken, is placed in
36h is impregnated in 150mL deionized waters, after making its complete swelling, with the ultrasonically treated 30min of the ultrasonoscope of power 200W.Will place
Resin after reason is vacuum dried 2h in 70 DEG C, to water content 30%, takes 15g and is placed in 150mL methyl alcohol and impregnate 36h, makes it completely molten
It is swollen.
Internal diameter 3cm, the chromatographic column of 24cm high are taken, the above-mentioned macroporous absorbent resin handled well is filled into post in a wet process, methyl alcohol is washed
To efflux without muddiness.
The thick saponin(e methanol solution 10mL of spina date seed of concentration 5.0mg/mL is taken, is added in chromatographic column, solution is filled with resin
After tap touches 36h, with the methanol solution of 4BV as eluent, with the elution flow rate drip washing chromatographic column of 0.8BV/h.Before discarding
80mL eluents, collect colourless solution part thereafter, and evaporation solvent methyl alcohol obtains jujuboside 19mg.
Product, the purity 45.7% of jujuboside, desorption efficiency 86% are determined with HPLC methods.
Embodiment 3.
0.5~1.25mm of particle diameter, the nonpolar D-101 types macroporous absorbent resin 20g of initial water content 70% are taken, is placed in
36h is impregnated in 120mL deionized waters, after making its complete swelling, with the ultrasonically treated 30min of the ultrasonoscope of power 150W.Will place
Resin after reason is vacuum dried 2h in 90 DEG C, to water content 20%, takes 10g and is placed in 100mL methyl alcohol and impregnate 36h, makes it completely molten
It is swollen.
Internal diameter 1.5cm, the chromatographic column of 24cm high are taken, the above-mentioned macroporous absorbent resin handled well is filled into post, methyl alcohol in a wet process
Untill efflux is washed till without muddiness.
The thick saponin(e methanol solution 7mL of spina date seed of concentration 1.0mg/mL is taken, is added in chromatographic column, make solution abundant with resin
After contact 24h, with the methanol solution of 3BV as eluent, with the elution flow rate drip washing chromatographic column of 0.3BV/h.Discard preceding 20mL
Eluent, collects colourless solution part thereafter, and evaporation solvent methyl alcohol obtains jujuboside 2mg.
Product, the purity 49.3% of jujuboside, desorption efficiency 90% are determined with HPLC methods.
Comparative example 1.
0.5~1.25mm of particle diameter, the nonpolar D-101 types macroporous absorbent resin 20g of initial water content 60% are taken, 90 DEG C true
Sky is dried to moisture-free, is taken 10g and is placed in 150mL methyl alcohol and impregnates 24h, makes its complete swelling.
Internal diameter 2cm, the chromatographic column of 24cm high are taken, the above-mentioned macroporous absorbent resin handled well is filled into post in a wet process, methyl alcohol is washed
To efflux without muddiness.
The thick saponin(e methanol solution 5mL of spina date seed of concentration 2.0mg/mL is taken, is added in chromatographic column, make solution abundant with resin
After contact 24h, with the methanol solution of 3BV as eluent, with the elution flow rate drip washing chromatographic column of 0.3BV/h.Discard preceding 40mL
Eluent, collects colourless solution part thereafter, and evaporation solvent methyl alcohol obtains jujuboside 2.6mg.
Product, the purity 17.6% of jujuboside, desorption efficiency 53% are determined with HPLC methods.
It is computed understanding, adsorbance of the jujuboside on resin after the treatment of comparative example 1 is only to be set after embodiment 1 is processed
0.5 times of fat.
Claims (10)
1. it is a kind of efficiently separate purifying jujuboside method, be by nonpolar D-101 types macroporous absorbent resin be placed in from
Impregnated to complete swelling in sub- water, ultrasonically treated 30min, 70~90 DEG C are dried under vacuum to 10~30wt% of water content, then are placed in first
Impregnated in alcohol to complete swelling, wet method preparative chromatography post adds the methanol extract liquid of the thick saponin(e of spina date seed fully to adsorb, with methyl alcohol
Be eluent, be eluted to eluent it is colourless after, collect eluent, evaporation solvent methyl alcohol, the jujuboside for being purified.
2. method according to claim 1, it is characterized in that by the nonpolar D-101 types macroporous absorbent resin in deionization
24~36h is impregnated in water.
3. method according to claim 1, it is characterized in that the ultrasonication power is 100~250W.
4. method according to claim 1, it is characterized in that by the nonpolar D-101 types macroporous absorbent resin in methyl alcohol
24~36h of dipping.
5. method according to claim 1, it is characterized in that the spina date seed soap in the thick saponin(e methanol extract liquid of the spina date seed
Glycosides concentration is 1.0~5.0mg/mL.
6. method according to claim 1, it is characterized in that the upper prop volume of the thick saponin(e methanol extract liquid of the spina date seed is
0.05~0.25 times of macroporous absorbent resin volume.
7. method according to claim 1, it is characterized in that the blade diameter length ratio of the resin column formed in the chromatographic column is 1: 10
~1: 1.
8. method according to claim 1, it is characterized in that the methanol extract liquid of the thick saponin(e of the spina date seed is added into chromatography
12~48h of contact is fully adsorbed in post with macroporous absorbent resin.
9. method according to claim 1, it is characterized in that the elution flow rate of eluent is 0.3~0.8BV/h.
10. method according to claim 1, it is characterized in that being eluted using the eluent of 3~5BV, and discards preceding 0.5
The eluent of~1BV.
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| CN107412371A (en) * | 2017-09-01 | 2017-12-01 | 安徽省芬格欣生物药业有限公司 | It is a kind of that there is mental-tranquilization, the jujuboside extracting method of tranquilizing soporific function |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107412371A (en) * | 2017-09-01 | 2017-12-01 | 安徽省芬格欣生物药业有限公司 | It is a kind of that there is mental-tranquilization, the jujuboside extracting method of tranquilizing soporific function |
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