CN1995027A - Separating preparation process of salvianolic acid B - Google Patents
Separating preparation process of salvianolic acid B Download PDFInfo
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- CN1995027A CN1995027A CN 200610170981 CN200610170981A CN1995027A CN 1995027 A CN1995027 A CN 1995027A CN 200610170981 CN200610170981 CN 200610170981 CN 200610170981 A CN200610170981 A CN 200610170981A CN 1995027 A CN1995027 A CN 1995027A
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Abstract
The invention discloses a separating method of salviol acid in the salvia miltiorrhizae extract, which is characterized by the following: grinding medicine materical crude slice of radix salvia miltiorrhizae; extracting through alcohol; sucking; decompressing filtrate; condensing; adding water in the condensate; adjusting pH value through alkaline to 7. 5; extracting through ether; adjusting pH value through water to 3; extracting through ether; recycling solvent; obtaining red powder-shaped rough extract of radix salvia miltiorrhizae; applying counter-current chromatographic fractionation method of pH value band to make salviol acid B.
Description
Technical field
The present invention relates to adverse current chromatogram and prepare separation method, specifically from red sage root crude extract, separate the method for preparing salvianolic acid B about using the refining counter current chromatography of pH district band.
Background technology
The red sage root is the dry root and rhizome of labiate red sage root Salvia miltiorrhiza Bge..The main active ingredient of the red sage root has water miscible pressure differential self and fat-soluble tanshinone compound.Salvianolic acid is the water soluble component that the existing caffeoyl depside of class structure has the neolignan skeleton again, modern pharmacological research shows, pressure differential self has very strong antioxygenation, can remove intravital superoxide anion and hydroxyl radical free radical, suppress peroxidatic reaction of lipid, microcirculation improvement.Salvianolic acid B is one of main representative effective constituent in the pressure differential self, account for 70% of total phenolic acid, be a kind of that content is the highest in the salvia-soluble effective constituent, activity is the strongest, the content of other salvianolic acid constituents in the red sage root and extract thereof becomes positive correlation with salvianolic acid B.Therefore the preparation of salvianolic acid has great importance for exploitation, the quality control of salvianolic acid medicine series.
At present, column chromatography is adopted in the separation of salvianolic acid constituents more, but it is very loaded down with trivial details to operate, and separation efficiency is not high; Also useful preparation type high performance liquid phase is isolating, but applied sample amount very little; High speed adverse current chromatogram is that a kind of liquid liquid distributes isolation technique, its separation principle is to utilize one-way fluid kinetic balance principle, make the unidirectional distribution in the spiral tube of high speed rotating of 2 immiscible solvent phase, the phase that fixes mutually wherein, carry the moving phase that is loaded with sample to pass stationary phase by constant flow pump, utilize the difference of sample partition ratio (K) in two-phase to realize separating.It has got rid of supporter fully to influences such as the irreversible adsorption of sample, taint, sex change, inactivations.They are different with general stratographic separate mode, make its being particularly useful for making property separation.High-speed countercurrent chromatography separation and purification red sage root water soluble ingredient salvianolic acid class material is adopted in record in " high-speed countercurrent chromatography separates the preparation salvianolic acid B " (" research and development of natural products " rolled up the 100th～104 page of the 1st phase in 2006 the 18th), preparation salvianolic acid B chemical reference substance, flash liberation can prepare the 63.4mg salvianolic acid B, and purity is 98%.
" pH district band adverse current chromatogram progress " (" analytical chemistry ", 2004,32 (4): record pH district's band adverse current chromatogram (pH-zone-refining counter-current chromatography) is that acid (alkali) dissociation constant and the hydrophobic difference of utilizing organic acids and base to be separated separated 529-533.).Compare with common adverse current chromatogram, its outstanding feature is to add to keep acid (or alkali) in the stationary phase of solvent system, adds wash-out alkali (or acid) simultaneously in moving phase, and the different substances wash-out is accompanied by the sudden change of pH value when coming out.This technology can obtain the rectangle peak of minimum overlay, impurity is concentrated in the both sides at peak simultaneously, have that the sample separation capacity is big, separation purity and separation efficiency advantages of higher, successfully be used at present the separation of multiple mixture, as amino acid derivative, peptide derivant, xanthene dyestuff, alkaloid and steric isomer etc.It has inherited advantages such as high speed adverse current chromatogram is efficient, stationary phase is pollution-free, has characteristics such as preparation amount is big and quick simultaneously, can reach more excellent effect at particular problem.
Summary of the invention
The present invention is directed to deficiency of the prior art proposed a kind of from Radix Salviae Miltiorrhizae extract the method for fast separating and purifying salvianolic acid B, this method technology is easy, the efficient height, preparation amount is big, product purity is greater than 95%.
This programme is realized by following technical measures: with the filtrate decompression behind salvia piece pulverizing, alcohol extracting, the suction filtration concentrate concentrated solution; Concentrated solution adds water, with basic solution adjust pH to 7.5, uses extracted with diethyl ether; Water is used extracted with diethyl ether with acidic solution adjust pH to 3, reclaims solvent, gets red powder shape red sage root crude extract;
To be disposed at by the solvent systems that ethers and water are formed and leave standstill behind the shake well in the separating funnel 12 hours, layering, last addition 1-30mmol/L acid is stationary phase, and following addition 1-30mmol/L buck is a moving phase, and it is identical wherein to add acid base concentration;
The GS10A2 type half preparation type counter current chromatograph that adopts Beijing new technology application research to be produced, counter current chromatograph is by ram pump, sampling valve, Ultraviolet Detector, registering instrument and the chromatography column (spiral tube that is formed by the polyfluortetraethylene pipe multiple wraps, capacity is 230mL) etc. composition, its order of connection is: ram pump → sampling valve → chromatography column → Ultraviolet Detector → registering instrument.At first make sampling valve be in the sample introduction state, stationary phase is filled the chromatography column of half preparation type counter current chromatograph with certain flow rate with pump, the opening speed controller, the chromatography column of half preparation type counter current chromatograph is just changeed, during turn up 800r/min, take by weighing a certain amount of red sage root crude extract and put into the stationary phase dissolving, inject the liquid storage tube of counter current chromatograph sampling valve with syringe, the rotation sampling valve makes sample enter chromatography column for connecing the column attitude.It is 2.0mL/min that flow rate of mobile phase is set, beginning pump moving phase;
According to the detector ultraviolet spectrogram, isolating each peak is all collected, obtain salvianolic acid B.
The beneficial effect of this programme can be learnt according to the narration to such scheme, owing to adopt pH district band adverse current chromatogram to separate the preparation salvianolic acid B, preparation amount is 8 times of common adverse current chromatogram preparation amount, purity has fractional dose and reaches characteristics such as gram magnitude, disengaging time weak point, sample free of losses, rate of recovery height, isolating environment mitigation, saving solvent more than 95%.Therefore the present invention has compared with prior art realized technical purpose.
The concrete characteristics of this programme also have, and the consumption volume ratio of ethers and water is 0.1～1: 1 in the described solvent systems.Described ether compound can be one of t-butyl methyl ether, ether, sherwood oil.Acid in the described stationary phase is trifluoroacetic acid, and the alkali in the described moving phase is ammoniacal liquor.Described alcohol extracting is for using 70-95% alcohol reflux 4 times, each 1 hour.It is one of the hydrochloric acid of 1mol/L, sulfuric acid of 1mol/L that described aqueous phase is used to transfer the acidic solution of pH value.The basic solution of described accent pH value is one of sodium hydrogen carbonate solution, 1mol/L sodium hydroxide solution.
Description of drawings
The present invention is described in further detail below in conjunction with accompanying drawing.
The isolating color atlas A of pH district band adverse current chromatogram of Fig. 1 embodiment 1 Radix Salviae Miltiorrhizae extract: salvianolic acid B; Solvent systems: t-butyl methyl ether: water=1: 1; Acid base concentration 10mmol/L; Applied sample amount 2.0g; A is a salvianolic acid B, purity 95.8%
The isolating color atlas A of pH district band adverse current chromatogram of Fig. 2 embodiment 2 Radix Salviae Miltiorrhizae extracts: salvianolic acid B; Solvent systems: t-butyl methyl ether: water=1: 1; Acid base concentration 20mmol/L; Applied sample amount 2.0g; A is a salvianolic acid B, purity 95.5%
The isolating color atlas A of pH district band adverse current chromatogram of Fig. 3 embodiment 3 Radix Salviae Miltiorrhizae extracts: salvianolic acid B; Solvent systems: ether: water=1: 1; Acid base concentration 10mmol/L; Applied sample amount 0.5g; A is a salvianolic acid B, purity 96.6%
Embodiment
Embodiment 1: gets salvia piece 2200g and pulverizes the back with 95% alcohol reflux 4 times (each 1h), and suction filtration, filtrate decompression concentrates, and gets concentrated solution.The concentrated solution water gaging that doubles is transferred pH to 7.5, extracted with diethyl ether with sodium hydrogen carbonate solution.Water is used extracted with diethyl ether with the hydrochloric acid adjust pH to 3 of 1mol/L, reclaims ether, gets red powder shape red sage root crude extract 57.19g.This crude extract separates the preparation salvianolic acid B with method of the present invention.
Adopt half preparation type counter current chromatograph, solvent selects for use t-butyl methyl ether and aqueous systems to separate the preparation salvianolic acid B from red sage root crude extract.At first above-mentioned solvent system is disposed in the separating funnel, shakes up the back standing demix with 1: 1 volume ratio, ready to balance after for some time up and down two-phase separately get and be stationary phase mutually, to wherein adding the 10mmol/L trifluoroacetic acid; Be moving phase mutually down, add 10mmol/L ammoniacal liquor.The GS10A2 type half preparation type counter current chromatograph that adopts Beijing new technology application research to be produced, it is by ram pump, sampling valve, Ultraviolet Detector, registering instrument and the chromatography column (spiral tube that forms by the polyfluortetraethylene pipe multiple wraps, capacity is 230mL) etc. composition, at first make sampling valve be in the sample introduction state, stationary phase is filled chromatography column with pump with certain flow rate, the opening speed controller, the chromatography column of half preparation type counter current chromatograph is just changeed, during turn up 800r/min, taking by weighing the 2g Radix Salviae Miltiorrhizae extract is dissolved in the 25mL stationary phase, inject the liquid storage tube of counter current chromatograph sampling valve with syringe, the rotation sampling valve makes sample enter chromatography column for connecing the column attitude.It is 2.0mL/min that flow rate of mobile phase is set, beginning pump moving phase; Receive salvianolic acid B according to detector ultraviolet spectrogram (Fig. 1) then, weight is 524.2mg, and product purity is 96.8%.
Utilize HPLC analytical separation thing.The HPLC condition: Tianjin, island Shim pack VP-ODS post (4.6mm * 250mm), 25 ℃ of column temperatures, flow velocity: 1.0ml/min, sample size: 5 μ L, moving phase: methyl alcohol: 5% acetate=35: 65, detect wavelength 281nm.
Embodiment 2: gets salvia piece 1000g and pulverizes the back with 80% alcohol reflux 4 times (each 1h), and suction filtration, filtrate decompression concentrates, and gets concentrated solution.The concentrated solution water gaging that doubles is transferred pH to 7.5, extracted with diethyl ether with the sodium hydroxide solution of 1mol/L.Water is used extracted with diethyl ether with the dilute sulfuric acid solution adjust pH to 3 of 1mol/L, reclaims ether, gets red powder shape red sage root crude extract 25.52g.This crude extract separates the preparation salvianolic acid B with method of the present invention.Adopt half preparation type counter current chromatograph, solvent selects for use t-butyl methyl ether and aqueous systems to separate the preparation salvianolic acid B from red sage root crude extract.At first above-mentioned solvent system is disposed in the separating funnel, shakes up the back standing demix with 1: 1 volume ratio, ready to balance after for some time up and down two-phase separately get and be stationary phase mutually, to wherein adding the 20mmol/L trifluoroacetic acid; Be moving phase mutually down, add 20mmol/L ammoniacal liquor.The GS10A2 type half preparation type counter current chromatograph that adopts Beijing new technology application research to be produced, it is by ram pump, sampling valve, Ultraviolet Detector, registering instrument and the chromatography column (spiral tube that forms by the polyfluortetraethylene pipe multiple wraps, capacity is 230mL) etc. composition, at first make sampling valve be in the sample introduction state, stationary phase is filled chromatography column with pump with certain flow rate, the opening speed controller, the chromatography column of half preparation type counter current chromatograph is just changeed, during turn up 800r/min, taking by weighing the 2g Radix Salviae Miltiorrhizae extract is dissolved in the 30mL stationary phase, inject the liquid storage tube of counter current chromatograph sampling valve with syringe, the rotation sampling valve makes sample enter chromatography column for connecing the column attitude.It is 2.0mL/min that flow rate of mobile phase is set, beginning pump moving phase; Receive salvianolic acid B according to detector ultraviolet spectrogram (Fig. 2) then, weight is 516mg,, to measure through HPLC, product purity is 96.5%.
Embodiment 3: gets salvia piece 1000g and pulverizes the back with 70% alcohol reflux 4 times (each 1h), and suction filtration, filtrate decompression concentrates, and gets concentrated solution.The concentrated solution water gaging that doubles is transferred pH to 7.5, extracted with diethyl ether with sodium hydrogen carbonate solution.Water is used extracted with diethyl ether with the hydrochloric acid adjust pH to 3 of 1mol/L, reclaims ether, gets red powder shape red sage root crude extract 23.13g.Adopt half preparation type counter current chromatograph, solvent selects for use ether and aqueous systems to separate the preparation salvianolic acid B from red sage root crude extract.At first above-mentioned solvent system is disposed in the separating funnel, shakes up the back standing demix with 1: 2 volume ratio, ready to balance after for some time up and down two-phase separately get and be stationary phase mutually, to wherein adding the 5mmol/L trifluoroacetic acid; Be moving phase mutually down, add 5mmol/L ammoniacal liquor.The GS10A2 type half preparation type counter current chromatograph that adopts Beijing new technology application research to be produced, it is by ram pump, sampling valve, Ultraviolet Detector, registering instrument and the chromatography column (spiral tube that forms by the polyfluortetraethylene pipe multiple wraps, capacity is 230mL) etc. composition, at first make sampling valve be in the sample introduction state, stationary phase is filled chromatography column with pump with certain flow rate, the opening speed controller, the chromatography column of half preparation type counter current chromatograph is just changeed, during turn up 800r/min, taking by weighing the 0.5g Radix Salviae Miltiorrhizae extract is dissolved in the 10mL stationary phase, inject the liquid storage tube of counter current chromatograph sampling valve with syringe, the rotation sampling valve makes sample enter chromatography column for connecing the column attitude.It is 2.0mL/min that flow rate of mobile phase is set, beginning pump moving phase; Receive salvianolic acid B according to detector ultraviolet spectrogram (Fig. 3) then, weight is 130mg, measures through HPLC, and product purity is 95.6%.
Though the present invention is described also full disclosure by embodiment and the accompanying drawing of selecting for use thereof, for a person skilled in the art, under the situation that does not exceed essence of the present invention, any change and variation all belong to scope of the present invention.
Claims (7)
1, a kind of method for separating and preparing of salvianolic acid B, it is characterized in that with the filtrate decompression behind salvia piece pulverizing, alcohol extracting, the suction filtration concentrate concentrated solution;
Concentrated solution adds water, with basic solution adjust pH to 7.5, uses extracted with diethyl ether; Water is used extracted with diethyl ether with acidic solution adjust pH to 3, reclaims solvent, gets red powder shape red sage root crude extract;
To be disposed at by the solvent systems that ethers and water are formed and leave standstill behind the shake well in the separating funnel 12 hours, layering, last addition 1-30mmol/L acid is stationary phase, and following addition 1-30mmol/L buck is a moving phase, and it is identical wherein to add acid base concentration;
At first make sampling valve be in the sample introduction state, stationary phase is filled the chromatography column of half preparation type counter current chromatograph with certain flow rate with pump, the opening speed controller, the chromatography column of half preparation type counter current chromatograph is just changeed, during turn up 800r/min, take by weighing a certain amount of red sage root crude extract and put into the stationary phase dissolving, inject the liquid storage tube of counter current chromatograph sampling valve with syringe, the rotation sampling valve is for connecing the column attitude, make sample enter chromatography column, it is 2.0mL/min that flow rate of mobile phase is set, beginning pump moving phase;
According to the detector ultraviolet spectrogram, isolating each peak is all collected, obtain salvianolic acid B.
2, the method for separating and preparing of salvianolic acid B according to claim 1 is characterized in that the consumption volume ratio of ethers and water is 0.1～1: 1 in the described solvent systems.
3, the method for separating and preparing of salvianolic acid B according to claim 2 is characterized in that described ether compound can be one of t-butyl methyl ether, ether, sherwood oil.
4, according to the method for separating and preparing of claim 1 or 2 or 3 described salvianolic acid Bs, it is characterized in that the acid in the described stationary phase is trifluoroacetic acid, the alkali in the described moving phase is ammoniacal liquor.
5, the method for separating and preparing of salvianolic acid B according to claim 1 is characterized in that described alcohol extracting is for using 70-95% alcohol reflux 4 times, each 1 hour.
6, the method for separating and preparing of salvianolic acid B according to claim 1 is characterized in that it is one of the hydrochloric acid of 1mol/L, sulfuric acid of 1mol/L that described aqueous phase is used to transfer the acidic solution of pH value.
7, the method for separating and preparing of salvianolic acid B according to claim 1, the basic solution that it is characterized in that described accent pH value are one of sodium hydrogen carbonate solution, 1mol/L sodium hydroxide solution.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101168539B (en) * | 2007-12-04 | 2011-01-19 | 哈药集团中药二厂 | Method for extracting salvianolic acid B |
| CN103735619A (en) * | 2013-12-31 | 2014-04-23 | 正大青春宝药业有限公司 | Method for preparing salviae miltiorrhizae extractum with high-content danshinolic acid B from salviae miltiorrhizae medicinal material |
| CN105541601A (en) * | 2015-12-14 | 2016-05-04 | 山东省分析测试中心 | Separation and preparation method of organic acid monomers in Chinese usnea and application thereof |
| CN106431915A (en) * | 2016-09-07 | 2017-02-22 | 山东省分析测试中心 | Method for preparing salvianolic acid A |
| CN109053417A (en) * | 2018-07-27 | 2018-12-21 | 山东省分析测试中心 | A kind of preparation method of high-purity ginkgoic acid |
| CN110194758A (en) * | 2019-04-29 | 2019-09-03 | 山东省分析测试中心 | A method of the fast separating and purifying Aristolochic Acid compound from caulis aristologhiae manshuriensis |
| CN113185406A (en) * | 2021-04-16 | 2021-07-30 | 山东省分析测试中心 | Efficient preparation method of phenolic acid active ingredients in salvia yunnanensis |
| CN113402489A (en) * | 2021-04-16 | 2021-09-17 | 宁波大学 | Method for efficiently preparing salvianolic acid B and lithospermic acid |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1164582C (en) * | 2002-12-31 | 2004-09-01 | 南京虹桥医药技术研究所 | Process for preparing danshen salviandic acid |
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2006
- 2006-12-30 CN CNB200610170981XA patent/CN100420682C/en active Active
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101168539B (en) * | 2007-12-04 | 2011-01-19 | 哈药集团中药二厂 | Method for extracting salvianolic acid B |
| CN103735619A (en) * | 2013-12-31 | 2014-04-23 | 正大青春宝药业有限公司 | Method for preparing salviae miltiorrhizae extractum with high-content danshinolic acid B from salviae miltiorrhizae medicinal material |
| CN103735619B (en) * | 2013-12-31 | 2017-01-11 | 正大青春宝药业有限公司 | Method for preparing salviae miltiorrhizae extractum with high-content danshinolic acid B from salviae miltiorrhizae medicinal material |
| CN105541601A (en) * | 2015-12-14 | 2016-05-04 | 山东省分析测试中心 | Separation and preparation method of organic acid monomers in Chinese usnea and application thereof |
| CN105541601B (en) * | 2015-12-14 | 2017-07-04 | 山东省分析测试中心 | The method for separating and preparing of organic acid monomer and application in a kind of sunglo |
| CN106431915A (en) * | 2016-09-07 | 2017-02-22 | 山东省分析测试中心 | Method for preparing salvianolic acid A |
| CN106431915B (en) * | 2016-09-07 | 2019-04-23 | 山东省分析测试中心 | A kind of preparation method of salviandic acid A |
| CN109053417A (en) * | 2018-07-27 | 2018-12-21 | 山东省分析测试中心 | A kind of preparation method of high-purity ginkgoic acid |
| CN109053417B (en) * | 2018-07-27 | 2021-03-05 | 山东省分析测试中心 | Preparation method of high-purity ginkgolic acid |
| CN110194758A (en) * | 2019-04-29 | 2019-09-03 | 山东省分析测试中心 | A method of the fast separating and purifying Aristolochic Acid compound from caulis aristologhiae manshuriensis |
| CN113185406A (en) * | 2021-04-16 | 2021-07-30 | 山东省分析测试中心 | Efficient preparation method of phenolic acid active ingredients in salvia yunnanensis |
| CN113402489A (en) * | 2021-04-16 | 2021-09-17 | 宁波大学 | Method for efficiently preparing salvianolic acid B and lithospermic acid |
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