CN105481809A - Separation and purification method of salvianolic acid B and preparation method of salvianolic acid B magnesium salt - Google Patents
Separation and purification method of salvianolic acid B and preparation method of salvianolic acid B magnesium salt Download PDFInfo
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Abstract
The invention relates to a separation and purification method of salvianolic acid B and a preparation method of a salvianolic acid B magnesium salt. The separation and purification method of the salvianolic acid B comprises taking a medicinal material of danshen root or white flower danshen as a raw material, and carrying out the steps of solvent extraction, separation and purification through a magnesium salt complexing method, MCI column purification, crystallization and recrystallization. According to the methods provided by the invention, a salvianolic acid B magnesium salt complexing method is adopted, so that a chromatography process with macroporous adsorption resin or polyamide column chromatography can be saved, the purification method is simpler and more time-saving, and the cost is lower. The preparation method of the salvianolic acid B magnesium salt is simple, and is low in cost, high in yield, and high in purity which can reach 98%, so that the preparation method is more suitable for mass production.
Description
Technical field
The present invention relates to a kind of from the extraction medicinal extract of the red sage root or Salvia miltiorrhiza f. medicinal material the method for separation and purification salvianolic acid B and the preparation method of its magnesium salts.
Background technology
Salviamiltiorrhizabung has promoting blood circulation to remove blood stasis, cool blood disappears carbuncle, the effect of the relieving restlessness that clears away heart-fire.Modern pharmacological research shows, red sage root energy coronary artery dilator, increase volume of blood flow, resist myocardial ischemia, improve microcirculation, reduce myocardial consumption of oxygen, improve heart function, hypotensive, reducing blood-fat, anticoagulation, antithrombotic, anti-oxidant, many effects such as to protect the liver.
Salvianolic acid B is one of red sage root primary water-soluble composition.Pharmacological research shows, salvianolic acid B has stronger pharmacological action in scavenging free radicals, protection cardiac-cerebral ischemia reperfusion injury and protection kidney etc.
Existing salvianolic acid B separation purification method is mainly separated by macroporous adsorbent resin or high speed adverse current chromatogram is separated.The main drawback that macroporous adsorbent resin is separated is wash-out length consuming time, and workload is large, and production cost is high.Chinese patent document CN1528756A (application number: 03151476.6) disclose a kind of processing method extracting salvianolic acid B from the red sage root, several method extracting salvianolic acid B from the red sage root is carried out organic assembling, have developed the novel process of a set of applicable separation and purification salvianolic acid B.Namely first extract with water, then use flocculate with chitosan, then carry out alcohol precipitation, then extract respectively by sherwood oil and ethyl acetate, finally adopt silica gel column chromatography to obtain the salvianolic acid B of higher degree.Aforesaid method adopts silica gel column chromatography separating purification salvianolic acid B, and the purity obtained is the salvianolic acid B of 50%-96%; But process is complicated, dead absorption is comparatively large, and operating process is loaded down with trivial details, is difficult to expand production to.XiaoWang etc. are at JournalofSeparationScience2007,30,3214-3217 describes the technique adopting high speed adverse current chromatogram separation and purification salvianolic acid B, and salvianolic acid B can be purified to 94.1% by display pH gradient adverse current chromatogram, and may be applied to life in enormous quantities; But the use of high-speed counter-current chromatograph has certain restriction.
Summary of the invention
For deficiency of the prior art, the invention provides a kind of from the red sage root or Salvia miltiorrhiza f. medicinal material the method for fast separating and purifying salvianolic acid B and the preparation method of salvianolic acid B magnesium, the method simple process, efficiency is high, and product purity can reach 98%.
Technical scheme of the present invention is as follows:
A separation purification method for salvianolic acid B, to comprise with the red sage root or Salvia miltiorrhiza f. medicinal material for raw material, through solvent extraction extraction, magnesium salts complexing seperation purifying, MCI column purification, crystallization and re-crystallization step, obtains salvianolic acid B;
Described solvent extraction extraction step is: by supersound extraction, filtration under the red sage root or Salvia miltiorrhiza f. medicinal material powder 70-80wt% ethanol room temperature, filtrate reduced in volume is obtained concentrated solution, concentrated solution adds aqueous suspension, with methylene dichloride or extraction into ethyl acetate removing impurity, discard methylene dichloride or ethyl acetate layer, water layer acidic solution adjusts pH=1 ~ 2, then is extracted with ethyl acetate, acetic acid ethyl acetate extract concentrating under reduced pressure, obtains salvianolic acid B crude extract.
According to the present invention, preferably, in solvent extraction extraction step: the quality of the red sage root or Salvia miltiorrhiza f. medicinal material powder and the volume ratio of 70-80wt% ethanol are 1:(8-12) g/mL; Acetic acid ethyl acetate extract is evaporated to medicinal extract shape, without ethanol taste.
According to the present invention, preferably, magnesium salts complexing seperation purification step is: by MgCl
2be dissolved in distilled water, be mixed with the MgCl that concentration is 0.01wt% ~ 1wt%
2the aqueous solution; By MgCl
2the aqueous solution joins in the salvianolic acid B crude extract of solvent extraction extraction step gained, stirred at ambient temperature, and dripping concentration is the NaHCO of 0.1wt% ~ 1wt%
3solution, after dropwising, continues stirring 1 ~ 2 minute; Add isopyknic methylene dichloride or extraction into ethyl acetate 2 times, the aqueous solution after extraction, adjust pH=1 ~ 2 with the hydrochloric acid of 1N ~ 2.5N, then with extraction into ethyl acetate 3 times, combined ethyl acetate extraction liquid, concentrating under reduced pressure;
This concentrated solution is repeated aforesaid operations, repurity 1 time, obtain salvianolic acid B sample after purifying.
According to the present invention, preferably, in magnesium salts complexing seperation purification step: described MgCl
2mgCl contained in solution
2mole number is 1/2nd of salvianolic acid B mole number in salvianolic acid B crude extract;
Preferably, described NaHCO
3naHCO contained in solution
3mole number equal salvianolic acid B mole number in salvianolic acid B crude extract, NaHCO used
3with MgCl
2mole ratio be 2:1.
According to the present invention, preferably, MCI column purification step is: by the salvianolic acid B sample after magnesium salts complexing seperation purifying, cross MCI pillar, the removal of impurity of 10wt%-20wt% methanol solution, 30wt%-60wt% methanol solution wash-out salvianolic acid B sample, concentrated salvianolic acid B sample eluent;
Salvianolic acid B sample eluent after concentrated is repeated above-mentioned MCI column purification step, the salvianolic acid B sample after must being further purified again.
According to the present invention, preferably, in MCI column purification step: described except using mixedly the preferred 20wt% methanol aqueous solution of elutriant; The preferred 30wt% methanol solution of described wash-out salvianolic acid B sample solution used.
According to the present invention, preferably, crystallization and re-crystallization step are: by MCI column purification step gained salvianolic acid B sample dissolution in methylene dichloride: methyl alcohol volume ratio=1:9 ~ 9:1, mixing solutions in carry out crystallization and recrystallization, obtain salvianolic acid B.
According to the present invention, preferably, in crystallization and re-crystallization step, described methylene dichloride: the volume ratio of methyl alcohol preferably (2 ~ 3): (8 ~ 7).
According to the present invention, a kind of preparation method of salvianolic acid B magnesium salt complex, step is as follows:
(1) preparation of magnesium hydroxide and Magnesium hydrogen carbonate:
Get MgCl
2be dissolved in distilled water, be mixed with the MgCl that concentration is 1wt% ~ 5wt%
2the aqueous solution, then drips the NaOH aqueous solution of 1wt% ~ 5wt%, and to not regeneration white precipitate, filtering-depositing, is precipitated to neutrality with distilled water wash; Get Mg (OH)
2be added to the water, pass into CO
260 ~ 90min clarifies to solution, and ultrasonic 10 ~ 20min removes unnecessary CO in solution
2, solution is crossed and is filtered insoluble particle, obtains magnesium bicarbonate solution; Magnesium bicarbonate solution must matching while using.
(2) preparation of salvianolic acid B magnesium salt complex:
The salvianolic acid B sample of above-mentioned preparation is added in magnesium bicarbonate solution, stirs and make it dissolve; With equal-volume methylene dichloride or extraction into ethyl acetate 2 times, except oil-soluble impurities, the water layer after extraction is concentrating under reduced pressure under 40 DEG C of conditions, and residual methylene dichloride or ethyl acetate in removing water layer, aqueous solution lyophilize, obtains salvianolic acid B magnesium salt complex.
According to the preparation method of salvianolic acid B magnesium salt complex of the present invention, preferably, in magnesium bicarbonate solution, the contained mole number of Magnesium hydrogen carbonate and the mole ratio of salvianolic acid B are 2:1.It is standby that magnesium bicarbonate solution used should be brand-new, matching while using.
According to the present invention, a kind of preparation method of salvianolic acid B magnesium salt complex, step is as follows:
Get MgCl
2be dissolved in distilled water, be mixed with the MgCl that concentration is 0.01wt% ~ 1wt%
2the aqueous solution; The salvianolic acid B of above-mentioned preparation is joined MgCl
2in the aqueous solution, stirring at room temperature, drips NaHCO
3the aqueous solution; After dropwising, suction filtration, lyophilize, obtains salvianolic acid B magnesium salt complex.
According to the preparation method of salvianolic acid B magnesium salt complex of the present invention, preferably, described MgCl
2mgCl contained in solution
2mole number and salvianolic acid B mole ratio are 1:2.Wherein, described NaHCO
3naHCO contained in solution
3mole number and salvianolic acid B mole ratio be 1:1.
Beneficial effect of the present invention:
The present invention adopts salvianolic acid B magnesium complexometry, can save the chromatography process of macroporous adsorbent resin or polyamide column chromatography, and purification process is simpler and save time, and cost is lower.The preparation method of salvianolic acid B magnesium is simple, and cost is low, and yield is high, and purity is high, and purity can reach 98%, is more suitable for large production.
Accompanying drawing explanation
Fig. 1 is the HPLC figure of the salvianolic acid B crude extract that the embodiment of the present invention 1 step (1) obtains.
Fig. 2 is the HPLC figure of the salvianolic acid B sample obtained after the embodiment of the present invention 1 step (2) magnesium salts complexometry purifying.
Fig. 3 is the HPLC figure of salvianolic acid B sample after the embodiment of the present invention 1 step (3) MCI purifying.
Fig. 4 is the HPLC figure of the salvianolic acid B obtained after the embodiment of the present invention 1 step (4) recrystallization.
Fig. 5 is the HPLC figure of the salvianolic acid B magnesium that the embodiment of the present invention 2 obtains.
Fig. 6 is the salvianolic acid B magnesium that obtains of the embodiment of the present invention 3
1h-NMR collection of illustrative plates.
Fig. 7 is the salvianolic acid B magnesium that obtains of the embodiment of the present invention 3
13c-NMR collection of illustrative plates.
Embodiment
Below by specific embodiment, also the invention will be further described by reference to the accompanying drawings, but be not limited thereto.
Embodiment 1: the preparation of high-purity danshinolic acid A
(1) extraction of salvianolic acid B: get red rooted salvia powder and be about 500g, add 75wt% ethanol, the quality of red rooted salvia powder and the volume ratio of ethanol are 1:12g/mL; Supersound extraction 2 times, each 30 minutes, filter, merging filtrate, concentrating under reduced pressure, concentrated solution adds suitable quantity of water, the removal of impurities of equal-volume dichloromethane extraction, water layer 2.5N hydrochloric acid adjusts pH=2, then with isopyknic extraction into ethyl acetate 2 times, acetic acid ethyl acetate extract concentrating under reduced pressure under 45 DEG C of conditions, obtains salvianolic acid B crude extract.
(2) magnesium salts complexometry purifying: by NaHCO
3with MgCl
2mol ratio is that the solution of 2:1 joins during salvianolic acid B slightly extracts, and makes it dissolve, 2 removal of impurities of isopyknic extraction into ethyl acetate, discard ethyl acetate layer, water layer acidic solution adjusts pH=2, then with equal-volume extraction into ethyl acetate 3 times, combined ethyl acetate extraction liquid, concentrating under reduced pressure, obtains concentrated solution;
Concentrated solution is repeated aforesaid operations, obtains the salvianolic acid B sample of purifying.
(3) MCI purifying: the salvianolic acid B sample of purifying in (2) is carried out the separation of MCI post, first with the removal of impurities of 20wt% methanol solution wash-out, then 30wt% methanol solution wash-out salvianolic acid B.
The salvianolic acid B elutriant eluted repeats a MCI post again and is separated, and obtains the salvianolic acid B sample that purity reaches 91%.
(4) recrystallization: by salvianolic acid B sample dissolution in step (3) in methyl alcohol: dissolve in the hot solution of methylene dichloride=3:8 (volume ratio), places crystallization.Leach crystallization, then carry out secondary crystal, obtain content of danshinolic acid B and reach 98%.
Embodiment 2: prepared by salvianolic acid B magnesium
Get MgCl
2be dissolved in distilled water, be mixed with the MgCl that concentration is 1wt%
2the aqueous solution, then drips the NaOH aqueous solution of 1wt%, and to not regeneration white precipitate, filtering-depositing, is precipitated to neutrality with distilled water wash; Get Mg (OH)
2be added to the water, pass into CO
260 ~ 90min clarifies to solution, and ultrasonic 10min removes unnecessary CO in solution
2, solution is crossed and is filtered insoluble particle, obtains magnesium bicarbonate solution; Magnesium bicarbonate solution must matching while using.
Join in freshly prepd magnesium bicarbonate solution by the salvianolic acid B sample 20mg of obtained for embodiment 1 98%, concussion makes it dissolve.With equal-volume extraction into ethyl acetate, combining extraction liquid, concentrating under reduced pressure evaporate to dryness, obtains high-purity danshinolic acid B magnesium salts.1H-NMR(600MHz,D
2O)δ:6.74(dd,J=29.3,13.8Hz,3H),6.67(t,J=9.4Hz,1H),6.62(dd,J=18.9,9.3Hz,2H),6.54(t,J=8.7Hz,2H),6.49(d,J=8.1Hz,1H),6.21(dd,J=31.4,8.0Hz,1H),6.07(s,1H),5.89(d,J=8.1Hz,1H),5.63(t,J=12.6Hz,1H),5.60–5.52(m,1H),4.78(dd,J=9.6,3.3Hz,1H),4.73–4.67(m,1H),3.91(d,J=4.5Hz,1H),2.89(dt,J=13.5,6.9Hz,1H),2.83–2.66(m,2H),2.38(dd,J=14.1,11.6Hz,1H).13C-NMR(151MHz,D
2O)δ:177.4,176.5,172.5,168.3,147.8,146.1,144.0,143.0,142.7,142.1,141.7,130.2,129.3,124.1,122.7,121.7,121.3,120.1,117.93,117.4,116.7,116.4,116.2,116.1,115.8,113.9,112.9,86.1,77.5,76.3,56.6,36.7,36.1.
Embodiment 3: prepared by salvianolic acid B magnesium
Get MgCl
2be dissolved in distilled water, be mixed with the MgCl that concentration is 0.05wt%
2the aqueous solution; 98% salvianolic acid B sample 20mg embodiment 1 prepared joins MgCl
2in the aqueous solution, stirring at room temperature, drips NaHCO
3the aqueous solution; After dropwising, suction filtration, lyophilize, obtains salvianolic acid B magnesium salt complex.
Described MgCl
2mgCl contained in solution
2mole number and salvianolic acid B mole ratio are 1:2.Wherein, described NaHCO
3naHCO contained in solution
3mole number and salvianolic acid B mole ratio be 1:1.
Claims (10)
1. a separation purification method for salvianolic acid B, to comprise with the red sage root or Salvia miltiorrhiza f. medicinal material for raw material, through solvent extraction extraction, magnesium salts complexing seperation purifying, MCI column purification, crystallization and re-crystallization step, obtains salvianolic acid B;
Described solvent extraction extraction step is: by supersound extraction, filtration under the red sage root or Salvia miltiorrhiza f. medicinal material powder 70-80wt% ethanol room temperature, filtrate reduced in volume is obtained concentrated solution, concentrated solution adds aqueous suspension, with methylene dichloride or extraction into ethyl acetate removing impurity, discard methylene dichloride or ethyl acetate layer, water layer acidic solution adjusts pH=1 ~ 2, then is extracted with ethyl acetate, acetic acid ethyl acetate extract concentrating under reduced pressure, obtains salvianolic acid B crude extract.
2. the separation purification method of salvianolic acid B according to claim 1, is characterized in that, in solvent extraction extraction step: the quality of the red sage root or Salvia miltiorrhiza f. medicinal material powder and the volume ratio of 70-80wt% ethanol are 1:(8-12) g/mL.
3. the separation purification method of salvianolic acid B according to claim 1, is characterized in that, magnesium salts complexing seperation purification step is: by MgCl
2be dissolved in distilled water, be mixed with the MgCl that concentration is 0.01wt% ~ 1wt%
2the aqueous solution; By MgCl
2the aqueous solution joins in the salvianolic acid B crude extract of solvent extraction extraction step gained, stirred at ambient temperature, and dripping concentration is the NaHCO of 0.1wt% ~ 1wt%
3solution, after dropwising, continues stirring 1 ~ 2 minute; Add isopyknic methylene dichloride or extraction into ethyl acetate 2 times, the aqueous solution after extraction, adjust pH=1 ~ 2 with the hydrochloric acid of 1N ~ 2.5N, then with extraction into ethyl acetate 3 times, combined ethyl acetate extraction liquid, concentrating under reduced pressure;
This concentrated solution is repeated aforesaid operations, repurity 1 time, obtain salvianolic acid B sample after purifying.
4. the separation purification method of salvianolic acid B according to claim 3, is characterized in that, in magnesium salts complexing seperation purification step: described MgCl
2mgCl contained in solution
2mole number is 1/2nd of salvianolic acid B mole number in salvianolic acid B crude extract;
Preferably, described NaHCO
3naHCO contained in solution
3mole number equal salvianolic acid B mole number in salvianolic acid B crude extract, NaHCO used
3with MgCl
2mole ratio be 2:1.
5. the separation purification method of salvianolic acid B according to claim 1, it is characterized in that, MCI column purification step is: by the salvianolic acid B sample after magnesium salts complexing seperation purifying, cross MCI pillar, the removal of impurity of 10wt%-20wt% methanol solution, 30wt%-60wt% methanol solution wash-out salvianolic acid B sample, concentrated salvianolic acid B sample eluent;
Salvianolic acid B sample eluent after concentrated is repeated above-mentioned MCI column purification step, the salvianolic acid B sample after must being further purified again.
6. the separation purification method of salvianolic acid B according to claim 5, is characterized in that, in MCI column purification step: described is 20wt% methanol aqueous solution except using mixedly elutriant; Described wash-out salvianolic acid B sample solution used is 30wt% methanol solution.
7. the separation purification method of salvianolic acid B according to claim 1, it is characterized in that, crystallization and re-crystallization step are: by MCI column purification step gained salvianolic acid B sample dissolution in methylene dichloride: carry out crystallization and recrystallization in the mixing solutions of methyl alcohol volume ratio=1:9 ~ 9:1, obtain salvianolic acid B.
8. the separation purification method of salvianolic acid B according to claim 7, is characterized in that, in crystallization and re-crystallization step, and described methylene dichloride: the volume ratio of methyl alcohol is (2 ~ 3): (8 ~ 7).
9. a preparation method for salvianolic acid B magnesium salt complex, step is as follows:
(1) preparation of magnesium hydroxide and Magnesium hydrogen carbonate:
Get MgCl
2be dissolved in distilled water, be mixed with the MgCl that concentration is 1wt% ~ 5wt%
2the aqueous solution, then drips the NaOH aqueous solution of 1wt% ~ 5wt%, and to not regeneration white precipitate, filtering-depositing, is precipitated to neutrality with distilled water wash; Get Mg (OH)
2be added to the water, pass into CO
260 ~ 90min clarifies to solution, and ultrasonic 10 ~ 20min removes unnecessary CO in solution
2, solution is crossed and is filtered insoluble particle, obtains magnesium bicarbonate solution; Magnesium bicarbonate solution must matching while using.
(2) preparation of salvianolic acid B magnesium salt complex:
Salvianolic acid B sample any one of claim 1-8 prepared adds in magnesium bicarbonate solution, stirs and makes it dissolve; With equal-volume methylene dichloride or extraction into ethyl acetate 2 times, except oil-soluble impurities, the water layer after extraction is concentrating under reduced pressure under 40 DEG C of conditions, and residual methylene dichloride or ethyl acetate in removing water layer, aqueous solution lyophilize, obtains salvianolic acid B magnesium salt complex.
10. a preparation method for salvianolic acid B magnesium salt complex, step is as follows:
Get MgCl
2be dissolved in distilled water, be mixed with the MgCl that concentration is 0.01wt% ~ 1wt%
2the aqueous solution; Salvianolic acid B prepared by any one of claim 1-8 is joined MgCl
2in the aqueous solution, stirring at room temperature, drips NaHCO
3the aqueous solution; After dropwising, suction filtration, lyophilize, obtains salvianolic acid B magnesium salt complex.
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Cited By (2)
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CN117756890A (en) * | 2024-01-03 | 2024-03-26 | 山东康耐斯生物科技有限公司 | Preparation for repairing coliform by umbilical cord mesenchymal stem cells, preparation method thereof and application of preparation in weight losing |
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CN117756890A (en) * | 2024-01-03 | 2024-03-26 | 山东康耐斯生物科技有限公司 | Preparation for repairing coliform by umbilical cord mesenchymal stem cells, preparation method thereof and application of preparation in weight losing |
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