CN103463189B - Method for extracting and separating total salvianolic acids from radix salviae miltiorrhizae water extract by utilizing ionic liquid - Google Patents
Method for extracting and separating total salvianolic acids from radix salviae miltiorrhizae water extract by utilizing ionic liquid Download PDFInfo
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Abstract
The invention discloses a method for extracting and separating total salvianolic acids from a radix salviae miltiorrhizae water extract by utilizing ionic liquid. The method comprises the following steps: extracting the total salvianolic acids from the radix salviae miltiorrhizae water extract in an extraction mode by using imidazole hydrophobic ionic liquid as an extraction agent, and separating from tannin, polysaccharide, albumen and other impurities; performing back extraction on the extraction agent layer through high temperature or a basifier after the extraction is layered and separated to obtain a high-density total salvianolic acid aqueous solution or salt solution thereof which serves as a raw material for further refining, wherein the ionic liquid can be recycled as an extraction agent after the back extraction treatment. According to the method, the ionic liquid which is not volatile, inflammable or explosive is adopted to extract the total salvianolic acids, and total salvianolic acids enrichment and extraction agent regeneration can be realized by virtue of back extraction, so that the method has the advantages of simple and safe extraction process, and is easy for scale production, and an effective solution is provided to solve the production problem generated when inflammable and explosive organic solvents with strong volatilization are massively used in the process of extracting total salvianolic acids.
Description
Technical field
The present invention relates to a kind of method utilizing ionic liquid extracting and separating Radix Salviae Miltiorrhizae total phenolic acids from Salvia miltiorrhiza Bge water extract, be applicable to the medicinal ingredients extracting water-soluble phenolic acids from salviamiltiorrhizabung, belong to medical art.
Background technology
The labiate red sage root (Salvia miltiorrhiza Bge.) and root extract thereof are a kind of common Chinese medicines, and its effective constituent comprises two large classes: fat-soluble tanshinone component and water miscible salvianolic acid constituents.Salvianolic acid is the organic acid compound that a class contains phenolic hydroxyl group, mainly contains Salvianic acidA, rancinamycin IV, rosmarinic acid, coffic acid, alkannic acid, isoferulic acid, salvianolic acid A, B, C, D, E, F, G etc.
[1]soluble in water, alcohol equal solvent; there is anti-oxidant, protection cardiovascular systems, anticancer, important physiological action such as protection brain cell etc.; be generally considered the red sage root and produce one of main component of curative effect, the red sage root conventional clinically and compound injection of red sage root etc. are all based on water miscible Radix Salviae Miltiorrhizae total phenolic acids.
In order to effectively Radix Salviae Miltiorrhizae total phenolic acids can be separated from Aqueous extracts, there is the report of multiple method at present, impurity is removed as adopted water extract-alcohol precipitation, then through macroporous resin (Chinese patent CN1384090A) or polyamide column (Chinese patent CN1242364A) absorb-elute, Radix Salviae Miltiorrhizae total phenolic acids product is obtained again by methods such as decompression or lyophilizes, though this method can improve product purity, in alcohol precipitation process, product loss is larger.In order to avoid alcohol precipitation loss, Chinese patent CN1202103C obtains product by the refining mode be directly separated with macroporous resin two-stage absorb-elute through polyamide column by Aqueous extracts.Also have and extracted by percolation, and then obtain product by the mode of macroporous resin adsorption, ethanolic soln wash-out, decrease product loss (Chinese patent CN102091125B).Chinese patent CN100484929C then describes a kind of separation method, carries out the heavy removal of impurities of acid, then utilize polar organic solvent to extract Radix Salviae Miltiorrhizae total phenolic acids, obtain product by evaporation of organic solvent Radix Salviae Miltiorrhizae extract.Chinese patent CN100378088C is convection drying after removal of impurities is sunk in acid then, then carries out alcohol reflux to dried medicinal extract, obtains product by after the supernatant concentration drying of extraction.But above method all uses the organic solvent that volatility is very strong in sepn process, these solvents are inflammable and explosive, in large-scale production, therefore there is very large operation hidden danger, also need lot of energy simultaneously to the recovery of these volatile organic solvents.
Ionic liquid (Ionic Liquids) is the organic compound that a class is composed entirely of ions, can stably exist in liquid form under room temperature or similar temperature, be otherwise known as ionic liquid at room temperature (Room Temperature Ionic Liquids, RTILs), material due to ionic state has extremely low, nonflammable, the heat stable feature of volatility, therefore there is the great potential of alternative organic solvent as separating medium, since entering 21 century, become the study hotspot in separation engineering.The hydrophobic ionic liquid of bibliographical information has good extraction ability to aldehydes matter, and (Lee is not busy, Deng, process engineering journal, 2005,, but hydrophobic ionic liquid is applied to extracting and separating Radix Salviae Miltiorrhizae total phenolic acids not yet has disclosed bibliographical information 5 (2): 148-151.).
Therefore a kind of extracting method of new Radix Salviae Miltiorrhizae total phenolic acids is developed; avoid or reduce using inflammable and explosive volatile organic solvent, will be conducive to improving production security, and reduce operation easier; be easy to industrialization amplify, the green large-scale production of red sage root water extraction effective constituent can be realized.
Technical scheme
Technical problem to be solved by this invention is to provide a kind of method utilizing ionic liquid extracting and separating Radix Salviae Miltiorrhizae total phenolic acids from Salvia miltiorrhiza Bge water extract.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
Utilize a method for ionic liquid extracting and separating Radix Salviae Miltiorrhizae total phenolic acids from Salvia miltiorrhiza Bge water extract, the method comprises the steps:
(1) extract: with imidazoles hydrophobicity ionic liquid at room temperature for extraction agent, liquid-liquid extraction is carried out to pretreated Salvia miltiorrhiza Bge water extract, the volume ratio of Salvia miltiorrhiza Bge water extract and extraction agent is 1:(0.2 ~ 1), extraction temperature is 10 ~ 30 DEG C, after abundant mixing, after system layering, separate aqueous layer and extraction oxidant layer, collect extraction oxidant layer;
(2) reextraction and extractant regeneration:
Hot water is utilized to carry out hot back extraction the extraction oxidant layer of getting of step (1), the volume ratio of extraction oxidant layer and hot water is 1:(0.3 ~ 1), back extraction temperature is 60 ~ 90 DEG C, after abundant mixing, separate aqueous layer and extraction oxidant layer after system layering, water intaking layer obtains the aqueous solution containing Radix Salviae Miltiorrhizae total phenolic acids, and the extraction oxidant layer after back extraction is reused for the extracting and separating of step (1);
Or,
Alkaline solution is utilized to carry out alkali back extraction the extraction oxidant layer of getting of step (1), the volume ratio of extraction oxidant layer and alkaline solution is 1:(0.2 ~ 1), back extraction temperature is 30 ~ 60 DEG C, after abundant mixing, separate aqueous layer and extraction oxidant layer after system layering, water intaking layer obtains the salt brine solution containing Radix Salviae Miltiorrhizae total phenolic acids, and the extraction oxidant layer after back extraction is reused for the extracting and separating of step (1) after washing process.
In step (1), described imidazoles hydrophobicity ionic liquid at room temperature is: 1-hexyl-3-Methylimidazole hexafluorophosphate ([Hmim] PF
6), 1-butyl-3-Methylimidazole bromine salt ([Bmim] Br), 1-base-3-Methylimidazole four fluorophosphate ([Hmim] BF
4), 1-octyl group-3-Methylimidazole bromine salt ([Omim] Br) or 1-butyl-3-Methylimidazole bis trifluoromethyl sulfimide salt ([Bmim] NTf2).
In step (1), described pretreated Salvia miltiorrhiza Bge water extract is usually prepared as follows and obtains: red rooted salvia is crushed to 30 ~ 100 orders, according to solid-to-liquid ratio 5 ~ 10%(mass ratio) be placed in 85 DEG C at reflux 1.5h, repeat twice, filter, after merging, obtain crude extract.And then the clarification Salvia miltiorrhiza Bge water extract that flocculation filtration or centrifugation or micro-filtration uf processing obtain is carried out to it, wherein, the concentration of Radix Salviae Miltiorrhizae total phenolic acids is 0.15 ~ 1.5mg/mL, pH2.0 ~ 8.0.
In step (1), described liquid-liquid extraction is single-stage or multi-stage solvent extraction.
In step (1), separate aqueous layer and extraction oxidant layer after system layering, if when remaining the Radix Salviae Miltiorrhizae total phenolic acids of more than 0.05mg/mL in water layer, can the operation of repeating step (1), merge extraction oxidant layer.
In step (2), described alkaline solution is the aqueous sodium hydroxide solution of 0.1 ~ 1.0mol/L.
In step (2), after system layering, separate aqueous layer and extraction oxidant layer, will extract oxidant layer repeating step (2) and again strip, until total back extraction ratio of Radix Salviae Miltiorrhizae total phenolic acids reaches more than 93%.
In step (2), extraction oxidant layer after alkali back extraction is carried out washing be treated to: deionized water and extraction oxidant layer volume ratio 3:1, multi_layer extraction water-yielding stratum after fully mixing under normal temperature, detect the pH of water layer, if pH value is more than 7.5, then continue with new deionized water wash extraction agent, until the pH value isolating water layer is less than 7.5.
Beneficial effect: the present invention compared with prior art has following advantage:
1. adopt relevant ions liquid as extraction agent, compared with the alcoholic solvent reported with current domestic and foreign literature, almost non-volatility, without combustion explosion, good operation safety;
2. adopt relevant ions liquid as extraction agent, good to the extraction selectivity of Radix Salviae Miltiorrhizae total phenolic acids, can avoid adopting polymeric adsorbent, decrease discharge of wastewater;
3., by hot water back extraction or alkali back extraction, realize recovery and the enrichment of Radix Salviae Miltiorrhizae total phenolic acids while regenerating extracting agent, decrease energy expenditure and product loss.
Embodiment
According to following embodiment, the present invention may be better understood.But those skilled in the art will readily understand, concrete material proportion, processing condition and result thereof described by embodiment only for illustration of the present invention, and should can not limit the present invention described in detail in claims yet.
Embodiment 1:
In the present embodiment, get the Radix Salviae Miltiorrhizae total phenolic acids of pretreated Salvia miltiorrhiza Bge water extract concentration be 0.78mg/mL, pH regulator is 2.0, and extraction agent is [Hmim] PF
6, at 10 DEG C, carry out secondary liquid-liquid extraction, the Aqueous extracts of every grade and extraction agent volume ratio are 1:1, and every grade of extraction time is 35min.After extraction phase-splitting, detect and show that total percentage extraction of its Radix Salviae Miltiorrhizae total phenolic acids is 95.5%.Employing temperature is that the hot water of 80 DEG C carries out hot water back extraction process to the extraction oxidant layer obtained, back extraction temperature maintains 80 DEG C, and the volume ratio of extraction oxidant layer and hot water is 1:1, and each Stripping times is 30min, twice back extraction, obtains the aqueous solution containing Radix Salviae Miltiorrhizae total phenolic acids after phase-splitting.Total back extraction ratio of Radix Salviae Miltiorrhizae total phenolic acids is 93.4%.The ionic liquid obtained after back extraction is used for again the Salvia miltiorrhiza Bge water extract secondary extraction under the same terms, total percentage extraction of its Radix Salviae Miltiorrhizae total phenolic acids is respectively 93.6%, and the regeneration rate of ionic liquid is 98.01%.The Radix Salviae Miltiorrhizae total phenolic acids aqueous solution that back extraction obtains is concentrated final vacuum through underpressure distillation and is dried to solid extract, wherein the average content of Radix Salviae Miltiorrhizae total phenolic acids is 86.3%.
Embodiment 2:
In the present embodiment, get the Radix Salviae Miltiorrhizae total phenolic acids of Salvia miltiorrhiza Bge water extract concentration be 0.15mg/mL, pH regulator is 6.0, and extraction agent is [Bmim] NTf
2, at 20 DEG C, carry out single-stage liquid-liquid extraction, Aqueous extracts and extraction agent volume ratio are 1:1, and extraction time is 40min.After extraction phase-splitting, detect and show that total percentage extraction of its Radix Salviae Miltiorrhizae total phenolic acids is 94.7%.Employing temperature is that the hot water of 90 DEG C carries out hot water back extraction process to the extraction oxidant layer obtained, back extraction temperature maintains 90 DEG C, and the volume ratio of extraction oxidant layer and hot water is 1:1, and each Stripping times is 30min, back extraction twice, obtains the aqueous solution containing Radix Salviae Miltiorrhizae total phenolic acids after phase-splitting.Total back extraction ratio of Radix Salviae Miltiorrhizae total phenolic acids is 94.5%, and the ionic liquid obtained after back extraction is used for again the Salvia miltiorrhiza Bge water extract secondary extraction under the same terms, total percentage extraction of its Radix Salviae Miltiorrhizae total phenolic acids is respectively 93.5%, and the regeneration rate of ionic liquid is respectively 98.73%.Therefore hot water back extraction volume ratio is preferably 1:1 ~ 1:0.5.The Radix Salviae Miltiorrhizae total phenolic acids aqueous solution that back extraction obtains is concentrated postlyophilization to solid extract through underpressure distillation, and wherein the average content of Radix Salviae Miltiorrhizae total phenolic acids is 90.3%.Embodiment 3:
In the present embodiment, get the Radix Salviae Miltiorrhizae total phenolic acids of Salvia miltiorrhiza Bge water extract concentration be 0.84mg/mL, pH regulator is 3.0, and extraction agent is [Hmim] PF
6, at 20 DEG C, carry out three grades of liquid-liquid extraction, the Aqueous extracts of every grade and extraction agent volume ratio are 1:0.5, and every grade of extraction time is 40min.After extraction phase-splitting, detect and show that total percentage extraction of its Radix Salviae Miltiorrhizae total phenolic acids is 93.5%.Employing concentration is that the sodium hydroxide solution of 0.8mol/L carries out alkali back extraction process to the extraction oxidant layer obtained, and the volume ratio of extraction oxidant layer and alkali lye is 1:0.3, back extraction 30min at 60 DEG C, a back extraction, obtains the aqueous solution containing Radix Salviae Miltiorrhizae total phenolic acids after phase-splitting.The back extraction ratio of Radix Salviae Miltiorrhizae total phenolic acids is 93.7%.The Radix Salviae Miltiorrhizae total phenolic acids aqueous solution that back extraction obtains is concentrated final vacuum through underpressure distillation and is dried to solid extract, wherein the average content of Radix Salviae Miltiorrhizae total phenolic acids is 87.6%.The extraction oxidant layer be separated after back extraction is washed, deionized water and extraction oxidant layer volume ratio 3:1,15min is uniformly mixed under normal temperature, isolate water layer, detecting water layer pH is 8.0, then continue by new deionized water wash extraction oxidant layer, again isolate water layer, detecting water layer pH is 6.8, and reach washing requirement, extraction agent can reuse.
Embodiment 4:
In the present embodiment, get the Radix Salviae Miltiorrhizae total phenolic acids of Salvia miltiorrhiza Bge water extract concentration be 1.45mg/mL, pH regulator is 2.5, extraction agent is [Omim] Br, at 30 DEG C, carry out three grades of liquid-liquid extraction, the Aqueous extracts of every grade and extraction agent volume ratio are 1:1, and every grade of extraction time is 25min.After extraction phase-splitting, detect and show that total percentage extraction of its Radix Salviae Miltiorrhizae total phenolic acids is 93.5%.Employing concentration is that the sodium hydroxide solution of 1.0mol/L carries out alkali back extraction process to the extraction oxidant layer obtained, and the volume ratio of extraction oxidant layer and alkali lye is 1:0.2, back extraction 30min at 70 DEG C, a back extraction, obtains the aqueous solution containing Radix Salviae Miltiorrhizae total phenolic acids after phase-splitting.After testing, the back extraction ratio of corresponding Radix Salviae Miltiorrhizae total phenolic acids is: 95.4%.The Radix Salviae Miltiorrhizae total phenolic acids aqueous solution that back extraction obtains is concentrated postlyophilization to solid extract through underpressure distillation, and wherein the average content of Radix Salviae Miltiorrhizae total phenolic acids is 85.2%.The extraction oxidant layer be separated after back extraction is washed, deionized water and extraction oxidant layer volume ratio 3:1, be uniformly mixed 10min under normal temperature, isolate water layer, detecting water layer pH is 8.5, then continue by new deionized water wash extraction oxidant layer, so repeatedly twice, isolate water layer, final to detect water layer pH be 7.3, reach washing requirement, extraction agent can reuse.
Embodiment 5:
In the present embodiment, get the Radix Salviae Miltiorrhizae total phenolic acids of Salvia miltiorrhiza Bge water extract concentration be 0.75mg/mL, pH regulator is 4.5, and extraction agent is [Hmim] BF
4, at 25 DEG C, carry out secondary liquid-liquid extraction, the Aqueous extracts of every grade and extraction agent volume ratio are 1:1, and every grade of extraction time is 40min.After extraction phase-splitting, employing temperature is that the hot water of 80 DEG C carries out hot water back extraction process to the extraction oxidant layer obtained, back extraction temperature maintains 80 DEG C, the volume ratio of extraction oxidant layer and hot water is respectively 1:0.5, each Stripping times is 30min, back extraction twice, obtains the aqueous solution containing Radix Salviae Miltiorrhizae total phenolic acids after phase-splitting, and the Salvia miltiorrhiza Bge water extract secondary extraction ionic liquid obtained after back extraction is used for again under the same terms, 5 times so repeatedly.The median extraction yield of Radix Salviae Miltiorrhizae total phenolic acids is 93.6% after testing, and average back extraction ratio is 95.9%, and the Radix Salviae Miltiorrhizae total phenolic acids aqueous solution that back extraction obtains concentrates postlyophilization to solid extract through underpressure distillation, and wherein the average content of Radix Salviae Miltiorrhizae total phenolic acids is 88.7%.
Embodiment 6:
In the present embodiment, get the Radix Salviae Miltiorrhizae total phenolic acids of Salvia miltiorrhiza Bge water extract concentration be 0.88mg/mL, pH regulator is 3.0, extraction agent is [Bmim] Br, at 20 DEG C, carry out secondary liquid-liquid extraction, the Aqueous extracts of every grade and extraction agent volume ratio are 1:1, and every grade of extraction time is 40min.After extraction phase-splitting, employing concentration is that the sodium hydroxide solution of 1.0mol/L carries out alkali back extraction process to the extraction oxidant layer obtained, and the volume ratio of extraction oxidant layer and alkali lye is 1:0.25, back extraction 40min at 60 DEG C, obtains the aqueous solution containing Radix Salviae Miltiorrhizae total phenolic acids after phase-splitting.The extraction oxidant layer be separated after back extraction is washed, deionized water and extraction oxidant layer volume ratio 3:1, be uniformly mixed 10min under normal temperature, isolate water layer, detect water layer pH, pH, all more than 8.0, continues, by new deionized water wash extraction oxidant layer, to isolate water layer, so 2 times repeatedly, final detection water layer pH is all lower than 7.5, and reach washing requirement, extraction agent can Reusability.The ionic liquid obtained after back extraction is used for again the Salvia miltiorrhiza Bge water extract secondary extraction under the same terms, 5 times so repeatedly.The median extraction yield of Radix Salviae Miltiorrhizae total phenolic acids is 94.4% after testing, and average back extraction ratio is 91.6%, and the Radix Salviae Miltiorrhizae total phenolic acids aqueous solution that back extraction obtains concentrates postlyophilization to solid extract through underpressure distillation, and wherein the average content of Radix Salviae Miltiorrhizae total phenolic acids is 84.0%.
Claims (5)
1. utilize a method for ionic liquid extracting and separating Radix Salviae Miltiorrhizae total phenolic acids from Salvia miltiorrhiza Bge water extract, it is characterized in that, the method comprises the steps:
(1) extract: with imidazoles hydrophobicity ionic liquid at room temperature for extraction agent, liquid-liquid extraction is carried out to pretreated Salvia miltiorrhiza Bge water extract, the volume ratio of Salvia miltiorrhiza Bge water extract and extraction agent is 1:(0.2 ~ 1), extraction temperature is 10 ~ 30 DEG C, after abundant mixing, after system layering, separate aqueous layer and extraction oxidant layer, collect extraction oxidant layer;
(2) reextraction and extractant regeneration:
Hot water is utilized to carry out hot back extraction the extraction oxidant layer of getting of step (1), the volume ratio of extraction oxidant layer and hot water is 1:(0.3 ~ 1), back extraction temperature is 60 ~ 90 DEG C, after abundant mixing, separate aqueous layer and extraction oxidant layer after system layering, water intaking layer obtains the aqueous solution containing Radix Salviae Miltiorrhizae total phenolic acids, and the extraction oxidant layer after back extraction is reused for the extracting and separating of step (1);
Or,
Alkaline solution is utilized to carry out alkali back extraction the extraction oxidant layer of getting of step (1), the volume ratio of extraction oxidant layer and alkaline solution is 1:(0.2 ~ 1), back extraction temperature is 30 ~ 60 DEG C, after abundant mixing, separate aqueous layer and extraction oxidant layer after system layering, water intaking layer obtains the salt brine solution containing Radix Salviae Miltiorrhizae total phenolic acids, and the extraction oxidant layer after back extraction is reused for the extracting and separating of step (1) after washing process;
In step (1), described imidazoles hydrophobicity ionic liquid at room temperature is: 1-hexyl-3-Methylimidazole hexafluorophosphate, 1-butyl-3-Methylimidazole bromine salt, 1-be base-3-Methylimidazole four fluorophosphate, 1-octyl group-3-Methylimidazole bromine salt or 1-butyl-3-Methylimidazole bis trifluoromethyl sulfimide salt;
In step (1), described pretreated Salvia miltiorrhiza Bge water extract is: the clarification Salvia miltiorrhiza Bge water extract obtained through flocculation filtration or centrifugation or micro-filtration uf processing, and wherein, the concentration of Radix Salviae Miltiorrhizae total phenolic acids is 0.15 ~ 1.5mg/mL, pH2.0 ~ 8.0;
In step (2), described alkaline solution is the aqueous sodium hydroxide solution of 0.1 ~ 1.0mol/L.
2. the method utilizing ionic liquid extracting and separating Radix Salviae Miltiorrhizae total phenolic acids from Salvia miltiorrhiza Bge water extract according to claim 1, is characterized in that, in step (1), described liquid-liquid extraction is single-stage or multi-stage solvent extraction.
3. the method utilizing ionic liquid extracting and separating Radix Salviae Miltiorrhizae total phenolic acids from Salvia miltiorrhiza Bge water extract according to claim 1, it is characterized in that, in step (1), separate aqueous layer and extraction oxidant layer after system layering, if when remaining the Radix Salviae Miltiorrhizae total phenolic acids of more than 0.05mg/mL in water layer, can the operation of repeating step (1), merge extraction oxidant layer.
4. the method utilizing ionic liquid extracting and separating Radix Salviae Miltiorrhizae total phenolic acids from Salvia miltiorrhiza Bge water extract according to claim 1, it is characterized in that, in step (2), separate aqueous layer and extraction oxidant layer after system layering, oxidant layer repeating step (2) will be extracted again strip, until total back extraction ratio of Radix Salviae Miltiorrhizae total phenolic acids reaches more than 93%.
5. the method utilizing ionic liquid extracting and separating Radix Salviae Miltiorrhizae total phenolic acids from Salvia miltiorrhiza Bge water extract according to claim 1, it is characterized in that, in step (2), extraction oxidant layer after alkali back extraction is carried out washing be treated to: deionized water and extraction oxidant layer volume ratio 3:1, multi_layer extraction water-yielding stratum after fully mixing under normal temperature, detects the pH of water layer, if pH value is more than 7.5, then continue with new deionized water wash extraction agent, until the pH value isolating water layer is less than 7.5.
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| 离子液体在中药提取、分离与分析中的应用;张丹丹等;《中国药科大学学报》;20130815;第44卷(第4期);380-384 * |
| 离子液体微波辅助提取葛根总黄酮;李倩等;《武汉工程大学学报》;20111130;第33卷(第11期);31-34,42 * |
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