CN1830947A - Method for extracting 'Danfen' phenolic acid-A - Google Patents
Method for extracting 'Danfen' phenolic acid-A Download PDFInfo
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Abstract
A process for preparing danshinolic acid A from red sage root includes such steps as extracting in water or alcohol, concentrating, high-temp and -pressure reaction, purifying by chromatographic column, regulating pH value, extracting in organic solvent, concentrating and drying.
Description
Technical field
The present invention relates to a kind of extracting method of pharmaceutical cpd, especially a kind of extracting method that from the red sage root, extracts salvianolic acid A.
Background technology
The red sage root is the most frequently used one of the medicinal material of invigorating blood circulation, and is used for the treatment of cardiovascular and cerebrovascular diseases such as stenocardia, hypertension, coronary heart disease and apoplexy.Nearly two more than ten years, the main active ingredient pressure differential self research of the red sage root is more active.Experiment in vivo and vitro shows that pressure differential self also can be treated multiple disease except being used for the treatment of cardiovascular and cerebrovascular diseases, as tumour, hepatopathy, ephrosis, peptic ulcer etc.Most of investigator is a target with total phenolic acid or with the salvianolic acid B, and ignores the lower and active stronger salvianolic acid A of content.
Went through 20 years, " basis and the clinical study of Radix Salviae Miltiorrhizae total phenolic acids treatment cerebro-vascular diseases " project of finishing by institute of Materia Medica,Chinese Academy of Medical Sciences etc. on December 30th, 2005 by appraisal of scientific and technological achievements by sanitation Ministry tissue.
People such as Zhen Yongsu have carried out big quantity research to the activity of salvianolic acid A, find that salvianolic acid A is used for the treatment of the effect of tumour, it is characterized in that the nucleoside transporting of tumour cell is had restraining effect, and tumour cell is had lethal effect, can strengthen the curative effect of cancer therapy drug.
Chinese patent CN1384090A disclosed the extracting method of water extract-alcohol precipitation after resin in 2002, and this technology increases alcohol precipitation makes phenolic acids loss 30%.Chinese patent CN03132382. disclosed and adopts water temperature centrifugal, ultrafiltration, acid adjustment, organic solvent extraction to prepare the method for salvianolic acid A again through reversed phase column chromatography in 2002.Because salvianolic acid A content in medicinal material is very low, sometimes even do not have, so the salvianolic acid A extraction yield is very low, causes difficulty for big production, in the big production of industry certain limitation is arranged, and therefore can not fundamentally solve the industrial problems of salvianolic acid A.
Summary of the invention
The present invention be directed to the deficiency that above-mentioned prior art exists, provide a kind of salvianolic acid A extraction yield height, purity good, stable performance, the extracting method of a kind of salvianolic acid A that production cost is low.
For achieving the above object, the technique means that the present invention taked is: a kind of extracting method of salvianolic acid A may further comprise the steps:
Step 1, in the red sage root of salvia piece or pulverizing, add proper amount of solvent, after extracting, carry out solid-liquid separation as solvent;
Step 2, extracting solution is carried out high-temperature high-voltage reaction;
Step 3, with the soup that step 2 obtains, join in the chromatography column, behind the water wash-out, use the eluent wash-out, after testing, collect highly purified salvianolic acid A solution, the decompression or normal pressure be concentrated into the elutriant organic solvent-free;
Step 4, the solution that step 3 is obtained are transferred PH 2～6 with acid, through chloroform or ether class organic solvent extraction, discard organic solvent mutually after, add the acetate esters organic solvent extraction at aqueous phase, will contain the soup of acetate esters organic solvent, concentrate drying.
When the proper amount of solvent that adds in this method steps one was water, extracting temperature was 0～100 ℃, extracted and selected for use supersound extraction, refluxing extraction or dynamic countercurrent to extract, and solid-liquid separation adopts filtration, natural subsidence or centrifugal.When adopting supersound extraction, the temperature of extraction is not more than 60 ℃, and when adopting dynamic countercurrent to extract, the temperature of extraction is 50～95 ℃.
When the proper amount of solvent that adds in the step 1 is water, carry out in this method steps two also can earlier extracting solution being concentrated before the high-temperature high-voltage reaction.
In addition, the proper amount of solvent that adds in this method steps one is an aqueous ethanolic solution, and alcohol concn is 10～80%, and extraction can select for use supersound extraction, refluxing extraction or diacolation to extract; Solid-liquid separation adopts filtration, natural subsidence or centrifugal.
When the proper amount of solvent that adds in the step 1 is aqueous ethanolic solution, carries out also extracting solution to be carried out before the high-temperature high-voltage reaction normal pressure in this method steps two and concentrate or be evaporated to and do not have the alcohol flavor.
In the aforesaid method step 2, the high-temperature high-voltage reaction condition is the pressure of 0.01Mpa～0.25MPa, and high temperature is at 101～140 ℃, and the reaction times is 0.5～24 hour.
Filler in this method steps three in the chromatography column is macroporous resin class, ion exchange resin, ephadex-20 gel, C18 bonded-phase chromatography post or C8 bonded-phase chromatography column packing, the best filler macroporous resin of polystyrene skeleton; Eluent adopts the aqueous solution of ethanol, methyl alcohol, acetone or acetonitrile.
In this method steps four, the acid of transferring pH value to use can be various organic acids or mineral acid; The acetate esters organic solvent is ethyl acetate, propyl acetate or butylacetate; Concentrate and adopt concentrating under reduced pressure or normal pressure to concentrate; Dry employing vacuum-drying or lyophilize; The acetate esters extraction liquid can adopt single stage method drying or two-step approach drying, and single stage method adopts the concentrating under reduced pressure drying to obtain the salvianolic acid A finished product; Two-step approach is to concentrate under normal pressure or reduced pressure earlier, adopts method dryings such as vacuum-drying or lyophilize to obtain the salvianolic acid A finished product then.
The present invention has overcome defective and the deficiency in the extracting method of existing salvianolic acid A, and the amount of final extract reaches more than 3.5 ‰, and salvianolic acid A content reaches more than 80% in the extract, therefore, salvianolic acid A yield height, purity is good, and stable performance, production cost are low.
Embodiment
The extracting method of one one kinds of salvianolic acid As of embodiment:
Get DANSHEN KELI 250kg, add 60% ethanol ultrasonic extraction 3 times of 6 times of amounts, each 20 minutes, 30 ℃ of supersound extraction temperature.United extraction liquid, it is centrifugal to cross tripodia, and centrifugate adopts concentrating under reduced pressure, and temperature is controlled at 60 ℃, is concentrated to 1: 1, and concentrated solution is put in the reactor 120 ℃ of reactions 8 hours.Get above-mentioned soup and cross macroporous resin column, applied sample amount (calculating with the crude drug dry weight) and macroporous resin amount were than 1: 5, remove impurity with the water flushing of 10 times of column volumes earlier, the back is that impurity is removed in 20% ethanol water flushing with 10 times of column volume concentration, is that 40% aqueous ethanolic solution washes with concentration again, does not have salvianolic acid A to Liquid Detection, collect elutriant, 60 ℃ are evaporated to nothing alcohol flavor, with salt acid for adjusting pH value to 2 ~ 4, get supernatant liquor, with the chloroform extraction of 1 times of supernatant liquor amount volume 1 time, discard the chloroform phase, water adds 1.5 times of amount volumes of acetic acid ethyl esters extraction 3 times, combined ethyl acetate phase, concentrating under reduced pressure, make soup to the thick paste shape, lyophilize gets salvianolic acid A.
The extracting method of 21 kinds of salvianolic acid As of embodiment: basic identical with embodiment one, different is the water supersound extraction.Specific as follows:
DANSHEN KELI adds the water of 6 times of amounts, supersound extraction 3 times, each 40 minutes, 40 ℃ of ultrasonic temperature.
The extracting method of 31 kinds of salvianolic acid As of embodiment: basic identical with embodiment two, different is that ultrasonic temperature is 0 ℃, and is specific as follows:
DANSHEN KELI adds the water of 6 times of amounts, supersound extraction 3 times, each 90 minutes, 0 ℃ of ultrasonic temperature.
The extracting method of 41 kinds of salvianolic acid As of embodiment: basic identical with embodiment three, different is that ultrasonic temperature is 1 ℃.
The extracting method of embodiment kind on May Day salvianolic acid A: basic identical with embodiment two, different is that ultrasonic temperature is 60 ℃, and is specific as follows:
DANSHEN KELI adds the water of 6 times of amounts, supersound extraction 3 times, each 10 minutes, 60 ℃ of ultrasonic temperature.
The extracting method of 61 kinds of salvianolic acid As of embodiment: basic identical with embodiment one, different is that the aqueous ethanolic solution diacolation extracts.Specific as follows:
Red sage root meal, the diacolation bucket of packing into was soaked in the 60% aqueous ethanolic solution sealing that adds 1.5 times of amounts 6 hours, dress is real, and 60% aqueous ethanolic solution is not stopped to add in the upper end, opens valve below and collects percolate, when collecting 6 ~ 7 times of amount medicinal material volumes, do not have salvianolic acid A, judge that diacolation stops to Liquid Detection.
The extracting method of embodiment kind July 1st salvianolic acid A: basic identical with embodiment one, different is the aqueous ethanolic solution refluxing extraction.
Salvia piece adds the aqueous ethanolic solution of 8 times of amounts, refluxing extraction 3 times, each 1.5 hours.
The extracting method of embodiment Aug. 1st kind salvianolic acid A: basic identical with embodiment one, different is the water refluxing extraction.
Salvia piece adds the water of 10 times of amounts, refluxing extraction 3 times, each 1 hour.
The extracting method of 91 kinds of salvianolic acid As of embodiment: basic identical with embodiment one, different is hydrodynamic(al) attitude countercurrent extraction.
Salvia piece, 80 ℃ of Heating temperatures, flow velocity is jar/40min.
The extracting method of 11 kinds of salvianolic acid As of embodiment: basic identical with embodiment nine, different is that Heating temperature is 50 ℃.
The extracting method of 11 kinds of salvianolic acid As of embodiment: basic identical with embodiment nine, different is that Heating temperature is 95 ℃.
The extracting method of 12 kinds of salvianolic acid As of embodiment: basic identical with embodiment two, different is that extracting solution does not concentrate and directly carries out high-temperature high-voltage reaction.
The extracting method of 13 kinds of salvianolic acid As of embodiment: basic identical with embodiment eight, different is that extracting solution does not concentrate and directly carries out high-temperature high-voltage reaction.
The extracting method of 14 kinds of salvianolic acid As of embodiment: basic identical with embodiment nine, different is that extracting solution does not concentrate and directly carries out high-temperature high-voltage reaction.
The extracting method of embodiment kind salvianolic acid A on ten May Day: basic identical with embodiment one, different is that column purification adopts the C18 bonding as chromatographic column filler.
The extracting method of 16 kinds of salvianolic acid As of embodiment: basic identical with embodiment one, different is that column purification adopts the C8 bonding as chromatographic column filler.
The extracting method of embodiment kind salvianolic acid A ten July 1st: basic identical with embodiment one, different is column purification, eluting solvent methanol aqueous solution.
The extracting method of 18 kinds of salvianolic acid As of embodiment: basic identical with embodiment one, different is column purification, eluting solvent aqueous acetone solution.
The extracting method of 19 kinds of salvianolic acid As of embodiment: basic identical with embodiment one, different is column purification, eluting solvent acetonitrile solution.
The extracting method of 21 kinds of salvianolic acid As of embodiment: basic identical with embodiment one, different is that the pH value is regulated and adopted sulfuric acid.
The extracting method of 21 kinds of salvianolic acid As of embodiment: basic identical with example one, different is to transfer pH value to 2-3 during the adjust pH organic solvent extraction.
The extracting method of 22 kinds of salvianolic acid As of embodiment: basic identical with example one, different is, adopts ether when regulating the pH organic solvent extraction earlier, after use ethyl acetate extraction.
The extracting method of 23 kinds of salvianolic acid As of embodiment: basic identical with example one, different is, adopts chloroform when regulating the pH organic solvent extraction earlier, after use n-butyl acetate extraction.
Claims (10)
1, a kind of extracting method of salvianolic acid A is characterized in that this method may further comprise the steps:
Step 1, in the red sage root of salvia piece or pulverizing, add proper amount of solvent, after extracting, carry out solid-liquid separation as solvent;
Step 2, extracting solution is carried out high-temperature high-voltage reaction;
Step 3, with the soup that step 2 obtains, join in the chromatography column, behind the water wash-out, use the eluent wash-out, after testing, collect highly purified salvianolic acid A solution, the decompression or normal pressure be concentrated into the elutriant organic solvent-free;
Step 4, the solution that step 3 is obtained are transferred PH2～6 with acid, through chloroform or ether class organic solvent extraction, discard organic solvent mutually after, add the acetate esters organic solvent extraction at aqueous phase, will contain the soup of acetate esters organic solvent, concentrate drying.
2, the extracting method of a kind of salvianolic acid A according to claim 1, it is characterized in that the proper amount of solvent that adds in this method steps one is a water, extracting temperature is 0～100 ℃, extraction selects for use supersound extraction, refluxing extraction or dynamic countercurrent to extract, and solid-liquid separation adopts filtration, natural subsidence or centrifugal.
3, the extracting method of a kind of salvianolic acid A according to claim 2 is characterized in that: the temperature of supersound extraction is not more than 60 ℃ in this method steps one; The temperature that dynamic countercurrent extracts is 50～95 ℃.
4, the extracting method of a kind of salvianolic acid A according to claim 2 is characterized in that: carry out in this method steps two before the high-temperature high-voltage reaction extracting solution being concentrated.
5, the extracting method of a kind of salvianolic acid A according to claim 1 is characterized in that the proper amount of solvent that adds in this method steps one is an aqueous ethanolic solution, and alcohol concn is 10～80%, and extraction can select for use supersound extraction, refluxing extraction or diacolation to extract; Solid-liquid separation adopts filtration, natural subsidence or centrifugal.
6, the extracting method of a kind of salvianolic acid A according to claim 5 is characterized in that carrying out in this method steps two also extracting solution to be carried out before the high-temperature high-voltage reaction normal pressure and concentrates or be evaporated to and do not have the alcohol flavor.
7, according to the extracting method of claim 1 or 4 or 6 each described a kind of salvianolic acid As, it is characterized in that in this method steps two, the high-temperature high-voltage reaction condition is the pressure of 0.01Mpa～0.25MPa, and high temperature is at 101～140 ℃, and the reaction times is 0.5～24 hour.
8, the extracting method of a kind of salvianolic acid A according to claim 1, it is characterized in that the filler in the chromatography column is macroporous resin class, ion exchange resin, Sephadex-20 gel, C18 bonded-phase chromatography post or C8 bonded-phase chromatography column packing in this method steps three, eluent adopts the aqueous solution of ethanol, methyl alcohol, acetone or acetonitrile.
9, the extracting method of a kind of salvianolic acid A according to claim 8 is characterized in that the filler in the chromatography column is the macroporous resin of polystyrene skeleton in this method steps three.
10, the extracting method of a kind of salvianolic acid A according to claim 1 is characterized in that in this method steps four, and the acid of transferring pH value to use can be various organic acids or mineral acid; The acetate esters organic solvent is ethyl acetate, propyl acetate or butylacetate; Concentrate and adopt concentrating under reduced pressure or normal pressure to concentrate; Dry employing vacuum-drying or lyophilize.
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| CN100462072C (en) * | 2007-01-23 | 2009-02-18 | 北京本草天源药物研究院 | Medicine composition used for injection and its preparing method |
| CN101019878B (en) * | 2007-03-27 | 2010-04-14 | 北京本草天源药物研究院 | Injection medicine composite containing salvianolic acid A and its preparation |
| CN101230003B (en) * | 2007-01-23 | 2010-04-21 | 北京本草天源药物研究院 | Preparation method of salvia miltiorrhiza tanshinoate A |
| CN101006984B (en) * | 2007-02-01 | 2010-05-19 | 北京本草天源药物研究院 | An injection preparation containing salvianolic acid A and extract of panax natoginseng, and its preparation method and application |
| CN101006975B (en) * | 2007-02-01 | 2010-05-19 | 北京本草天源药物研究院 | An oral medicine preparation containing salvianolic acid A and extract of panax natoginseng, and its preparation method and application |
| CN101186572B (en) * | 2007-12-19 | 2010-05-19 | 天津大学 | Method for one-step separation and purification of salvianolic acid from water extract of salvia miltiorrhiza |
| CN101851162A (en) * | 2009-03-30 | 2010-10-06 | 天津天士力制药股份有限公司 | Novel salvianolic acid compound L and preparation method and application thereof |
| CN102212001A (en) * | 2010-04-06 | 2011-10-12 | 山东靶点药物研究有限公司 | Compound salvianolic acid F methyl ester and preparation method thereof |
| CN102212003A (en) * | 2010-04-06 | 2011-10-12 | 山东靶点药物研究有限公司 | Method for purifying salvianolic acid A by using reversed-phase chromatography |
| CN101696166B (en) * | 2007-01-23 | 2012-05-09 | 北京本草天源药物研究院 | Preparation method of salvianolic acid A from salvia miltiorrhiza |
| CN102531901A (en) * | 2010-12-25 | 2012-07-04 | 上海绿谷制药有限公司 | Preparation method for salvianolic acid A |
| CN103242161A (en) * | 2013-05-17 | 2013-08-14 | 成都科源生物技术有限公司 | Method for preparing salvianolic acid A |
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| CN1305866C (en) * | 2003-08-19 | 2007-03-21 | 江苏扬子江药业集团有限公司 | Method of extracting phenolic components from chinese medicine red sage root and its freeze dried powder injection agent |
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| CN101696166B (en) * | 2007-01-23 | 2012-05-09 | 北京本草天源药物研究院 | Preparation method of salvianolic acid A from salvia miltiorrhiza |
| CN101230003B (en) * | 2007-01-23 | 2010-04-21 | 北京本草天源药物研究院 | Preparation method of salvia miltiorrhiza tanshinoate A |
| CN100462072C (en) * | 2007-01-23 | 2009-02-18 | 北京本草天源药物研究院 | Medicine composition used for injection and its preparing method |
| CN101006984B (en) * | 2007-02-01 | 2010-05-19 | 北京本草天源药物研究院 | An injection preparation containing salvianolic acid A and extract of panax natoginseng, and its preparation method and application |
| CN101006975B (en) * | 2007-02-01 | 2010-05-19 | 北京本草天源药物研究院 | An oral medicine preparation containing salvianolic acid A and extract of panax natoginseng, and its preparation method and application |
| CN101019878B (en) * | 2007-03-27 | 2010-04-14 | 北京本草天源药物研究院 | Injection medicine composite containing salvianolic acid A and its preparation |
| CN101186572B (en) * | 2007-12-19 | 2010-05-19 | 天津大学 | Method for one-step separation and purification of salvianolic acid from water extract of salvia miltiorrhiza |
| CN101851162A (en) * | 2009-03-30 | 2010-10-06 | 天津天士力制药股份有限公司 | Novel salvianolic acid compound L and preparation method and application thereof |
| CN101851162B (en) * | 2009-03-30 | 2014-09-17 | 天士力制药集团股份有限公司 | Novel salvianolic acid compound L and preparation method and application thereof |
| CN102212003A (en) * | 2010-04-06 | 2011-10-12 | 山东靶点药物研究有限公司 | Method for purifying salvianolic acid A by using reversed-phase chromatography |
| CN102212001B (en) * | 2010-04-06 | 2013-11-06 | 山东靶点药物研究有限公司 | Compound salvianolic acid F methyl ester and preparation method thereof |
| CN102212001A (en) * | 2010-04-06 | 2011-10-12 | 山东靶点药物研究有限公司 | Compound salvianolic acid F methyl ester and preparation method thereof |
| CN102531901A (en) * | 2010-12-25 | 2012-07-04 | 上海绿谷制药有限公司 | Preparation method for salvianolic acid A |
| CN102531901B (en) * | 2010-12-25 | 2015-04-08 | 苏州雷纳药物研发有限公司 | Preparation method for salvianolic acid A |
| CN103242161A (en) * | 2013-05-17 | 2013-08-14 | 成都科源生物技术有限公司 | Method for preparing salvianolic acid A |
| CN103570548A (en) * | 2013-10-17 | 2014-02-12 | 浙江永宁药业股份有限公司 | Preparation method of salvinaolic acid A |
| CN103570548B (en) * | 2013-10-17 | 2015-07-08 | 浙江永宁药业股份有限公司 | Preparation method of salvinaolic acid A |
| CN108872440A (en) * | 2018-08-11 | 2018-11-23 | 中山市永恒化工新材料研究院有限公司 | Method for measuring content of phenol in water |
| CN108872440B (en) * | 2018-08-11 | 2021-06-29 | 中山市永恒化工新材料研究院有限公司 | A kind of measuring method of phenol content in water |
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