CN101864460A - Method for extracting gallic acid from bistort rhizome - Google Patents
Method for extracting gallic acid from bistort rhizome Download PDFInfo
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- CN101864460A CN101864460A CN201010182726A CN201010182726A CN101864460A CN 101864460 A CN101864460 A CN 101864460A CN 201010182726 A CN201010182726 A CN 201010182726A CN 201010182726 A CN201010182726 A CN 201010182726A CN 101864460 A CN101864460 A CN 101864460A
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- enzymolysis
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Abstract
The invention relates to a preparation method for gallic acid, which is characterized by easy operation and less equipment investment. The processing steps are as follows: dried bistort rhizome is ground and then wetted by ethanol, air blasting is carried out, the obtained ground wet material is mixed with tannase, enzymolysis is carried out for 6 to 8 hours, enzymolysis product is extracted by hot water with the temperature of 80 DEG C, extract is refined by active carbon and reducing agent, and after filtration and concentrative crystallization, acetone is used for recrystallization, so that product is obtained. When the method is adopted to prepare the gallic acid, the production process is simple, the utilization rate of material is high, the processing capacity is high, and industrialization can be easily implemented.
Description
Technical field:
The present invention relates to a kind of method of from adder-wort, extracting gallic acid, especially a kind of method for preparing gallic acid with airblasting method, enzyme process.
Background technology:
Gallic acid
3,4,5-trihydroxybenzoic acid, gallic acid
Molecular formula: C
7H
6O
5
Molecular weight: 170.12
Structural formula:
Physical properties: needle crystal (anhydrous methanol or chloroform), 235～240 ℃ of fusing points (decomposition).1g is fused to 87ml cold water, 3ml boiling water, 6ml ethanol, 100m ether, 10ml glycerine and 5ml acetone.Be dissolved in benzene, chloroform and sherwood oil hardly.
The preparation method that gallic acid is commonly used has acid-hydrolysis method, alkali hydrolysis method etc., and a small amount of Enzymatic Extraction is also arranged.The vitriol oil is used in acid hydrolysis always, and its strong oxidizing property easily causes benzene ring structure to destroy and influences yield.Chinese patent CN1104627 " doubly the basic hydrolysis of flower raw material prepares the method for gallic acid " and CN1057255 " utilize tower to draw powder production gallic acid " with neutralizing with acid with basic hydrolysis earlier, has increased the complicated operation degree again.Directly often because solvent diffusion speed is slow, the reaction conditions problem is limited in enzymolysis production, as solubilizing agent enzymolysis among the CN1083532 " technology of preparation of gallic acid by using enzyme " temperature, PH, dissolved oxygen amount is had strict requirement, difficult control.Yang Shunkai etc. " the enzymatic conversion method Chinese gallotanninic acid is produced gallic acid " also take the method for enzymolysis in the solution, and solvent diffusion is slower, and enzymolysis speed is restricted.
The airblasting method has been used in Huanghai Sea shore etc. in " the airblasting method is applied to the pre-test of Mengiferin Study on extraction process ", and has obtained good leaching yield.Airblasting method principle is similar to steam explosion, be that the great power that discharges when utilizing air in the medicinal material tissue then to reduce pressure is suddenly by compression broken through plant cell wall, tear plant tissue, make the medicinal material short texture, be beneficial to solvent and infiltrate medicinal material inside, it is long-pending to increase considerably surface in contact, is beneficial to solvent simultaneously in motion of medicinal material granule interior and conveying.
Summary of the invention:
Technical problem to be solved by this invention provides a kind of preparation method who is beneficial to big production operation, gallic acid that leaching yield is high.
For solving the problems of the technologies described above, the present invention adopts following technical proposal:
1) airblasting: get the adder-wort dried roots, pulverize the order into 40-60, add the moistening 2h of ethanol of 0.5 times of amount of raw materials quality, the burstpressures jar is closed intake valve and reducing valve, adds above-mentioned wet-milling, has filled up rubber cushion, builds and tights a bolt.Close air outlet valve and reducing valve, open intake valve and allow jar interior pressure keep 0.2-0.25MPa 20-30min at normal temperatures, pressurize is closed intake valve after finishing, and opens reducing valve, utilizes a jar internal pressure that raw material is rapidly sprayed into and holds the medicine device, gets broken wet stock;
2) enzymolysis: in above-mentioned wet stock, mix with tannase, enzymolysis, enzymolysis product extracts 0.5-1h in 80 ℃ of hot water, filter, and gets filtrate;
3) refining crystallization: filtrate adds the gac of its quality 5% and 2% reductive agent, and constant temperature 0.5-1h filters, and above-mentioned aqueous solution heating is concentrated into small volume, leaves standstill crystallization;
4) recrystallization: above-mentioned crystallization is dissolved in acetone, concentrates recrystallization 2-3 time, oven dry promptly gets product.
The said extracted method is characterized in that described 1) in moistening used alcohol concn be 40%.
The said extracted method is characterized in that described 2) in enzyme dosage be the 1-5% of wet stock quality, hydrolysis temperature is 45 ℃, enzymolysis time is 6-8h.
The said extracted method is characterized in that described 2) middle condition: the hot water consumption is 6-8 times (V/W) of enzymolysis product quality.
The said extracted method is characterized in that described 3) middle condition: refined soln is concentrated into the 1/10-1/15 crystallization of its volume.
The said extracted method is characterized in that described 4) in the acetone consumption of each recrystallization be that the 5-6 of the rapid crystalline quality of previous step doubly measures (V/W), be concentrated into the 1/5-1/8 recrystallization of original volume.
In sum, there is following advantage in the present invention: airblasting is a kind of physics assisted extraction method, and the water-soluble tannin that therefore can intact reservation extracts is just destroyed very up hill and dale by the explosion raw material mix, has increased contact area greatly; Enzymolysis process is simpler than basic hydrolysis, and also than acid hydrolysis safety, mild condition is not easy to cause the corrosion of equipment, because had handle the early stage of airblasting, need not can fully contact with material with solvent dispersion in this law; Gallic acid solubleness in acetone is very big, and evaporation is easy, so crystallization velocity is fast.
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment:
Embodiment 1
Get the about 100g of adder-wort dried roots, pulverizing is 40 orders, adds the moistening 2h of 50ml 40% ethanol, and the burstpressures jar is closed intake valve and reducing valve, adds above-mentioned wet-milling, has filled up rubber cushion, builds and tights a bolt.Close air outlet valve and reducing valve, open intake valve and allow jar interior pressure keep 0.2MPa 20min at normal temperatures, pressurize is closed intake valve after finishing, open reducing valve, utilize a jar internal pressure that raw material is rapidly sprayed into and hold the medicine device, get wet stock 136g, add the 1.4g tannase, 45 ℃ of enzymolysis 6h of constant temperature, enzymolysis product are dissolved in 80 ℃ of hot water of 900ml and extract 0.5h, add the reductive agent of 5g gac and 2g, constant temperature 0.5h, filter, be concentrated into 90ml and leave standstill crystallization, get coarse crystal 23.2g; Coarse crystal is leached, be dissolved in 5 times of amounts (V/W) acetone, heating is concentrated into the 90ml crystallization, repeats aforesaid operations recrystallization 2 times, and oven dry promptly gets product 17.3g, detects through HPLC, and purity is 98.5%.
Embodiment 2
Get the about 100g of adder-wort dried roots, pulverizing is 60 orders, adds the moistening 2h of 50ml 40% ethanol, and the burstpressures jar is closed intake valve and reducing valve, adds above-mentioned wet-milling, has filled up rubber cushion, builds and tights a bolt.Close air outlet valve and reducing valve, open intake valve and allow jar interior pressure keep 0.2MPa 25min at normal temperatures, pressurize is closed intake valve after finishing, open reducing valve, utilize a jar internal pressure that raw material is rapidly sprayed into and hold the medicine device, get wet stock 138g, add the 2g tannase, 45 ℃ of enzymolysis 7h of constant temperature, enzymolysis product are dissolved in 80 ℃ of hot water of 1000ml and extract 1h, add the reductive agent of 5g gac and 2g, constant temperature 0.5h, filter, be concentrated into 80ml and leave standstill crystallization, get coarse crystal 24.5g; Coarse crystal is leached, be dissolved in 5.5 times of amounts (V/W) acetone, heating is concentrated into the 60ml crystallization, repeats aforesaid operations recrystallization 2 times, and oven dry promptly gets product 17.5g, detects through HPLC, and purity is 98.7%.
Embodiment 3
Get the about 100g of adder-wort dried roots, pulverizing is 60 orders, adds the moistening 2h of 50ml 40% ethanol, and the burstpressures jar is closed intake valve and reducing valve, adds above-mentioned wet-milling, has filled up rubber cushion, builds and tights a bolt.Close air outlet valve and reducing valve, open intake valve and allow jar interior pressure keep 0.25MPa 30min at normal temperatures, pressurize is closed intake valve after finishing, open reducing valve, utilize a jar internal pressure that raw material is rapidly sprayed into and hold the medicine device, get wet stock 141g, add the 7g tannase, 45 ℃ of enzymolysis 8h of constant temperature, enzymolysis product are dissolved in 80 ℃ of hot water of 1100ml and extract 1h, add the reductive agent of 5g gac and 2g, constant temperature 1h, filter, be concentrated into 70ml and leave standstill crystallization, get coarse crystal 25.3g; Coarse crystal is leached, be dissolved in 6 times of amounts (V/W) acetone, heating is concentrated into the 50ml crystallization, repeats aforesaid operations recrystallization 2 times, and oven dry promptly gets product 17.9g, detects through HPLC, and purity is 99.2%.
Claims (6)
1. method of extracting gallic acid from adder-wort is characterized in that comprising following steps:
1) airblasting: get the adder-wort dried roots, pulverize the order into 40-60, add the moistening 2h of ethanol of 0.5 times of amount of raw materials quality, the burstpressures jar is closed intake valve and reducing valve, adds above-mentioned wet-milling, has filled up rubber cushion, builds and tights a bolt.Close air outlet valve and reducing valve, open intake valve and allow jar interior pressure keep 0.2-0.25MPa 20-30min at normal temperatures, pressurize is closed intake valve after finishing, and opens reducing valve, utilizes a jar internal pressure that raw material is rapidly sprayed into and holds the medicine device, gets broken wet stock;
2) enzymolysis: in above-mentioned wet stock, mix with tannase, enzymolysis, enzymolysis product extracts 0.5-1h in 80 ℃ of hot water, filter, and gets filtrate;
3) refining crystallization: filtrate adds the gac of its quality 5% and 2% reductive agent, and constant temperature 0.5-1h filters, and above-mentioned aqueous solution heating is concentrated into small volume, leaves standstill crystallization;
4) recrystallization: above-mentioned crystallization is dissolved in acetone, filters, concentrate, recrystallization 2-3 time, oven dry promptly gets product.
2. according to the described extracting method of claim 1, it is characterized in that described 1) in moistening used alcohol concn be 40%.
3. according to the described extracting method of claim 1, it is characterized in that described 2) in enzyme dosage be the 1-5% of wet stock quality, hydrolysis temperature is 45 ℃, enzymolysis time is 6-8h.
4. according to the described extracting method of claim 1, it is characterized in that described 2) middle condition: the hot water consumption is 6-8 times (V/W) of enzymolysis product quality.
5. according to the described extracting method of claim 1, it is characterized in that described 3) middle condition: refined soln is concentrated into the 1/10-1/15 crystallization of its volume.
6. according to the described extracting method of claim 1, it is characterized in that described 4) in the acetone consumption of each recrystallization be that the 5-6 of the rapid crystalline quality of previous step doubly measures (V/W), be concentrated into the 1/5-1/8 recrystallization of original volume.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010182726A CN101864460A (en) | 2010-05-26 | 2010-05-26 | Method for extracting gallic acid from bistort rhizome |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201010182726A CN101864460A (en) | 2010-05-26 | 2010-05-26 | Method for extracting gallic acid from bistort rhizome |
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| CN101864460A true CN101864460A (en) | 2010-10-20 |
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| CN201010182726A Pending CN101864460A (en) | 2010-05-26 | 2010-05-26 | Method for extracting gallic acid from bistort rhizome |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102603919A (en) * | 2012-04-13 | 2012-07-25 | 赵岩 | Method for preparing alginic acid and sodium alginate through air steam explosion coupling biological compound enzyme technology |
| CN111521710A (en) * | 2020-05-12 | 2020-08-11 | 劲牌持正堂药业有限公司 | Determination method for improving gallic acid content and stability in bistort rhizome |
| CN112877373A (en) * | 2021-01-26 | 2021-06-01 | 桂林莱茵生物科技股份有限公司 | Preparation method for obtaining gallic acid with content of more than 99% |
| CN114426478A (en) * | 2022-01-28 | 2022-05-03 | 广西壮族自治区中国科学院广西植物研究所 | High-content gallic acid and preparation method thereof |
| WO2023051745A1 (en) * | 2021-09-30 | 2023-04-06 | 上海百斯杰生物工程有限公司 | Method for producing gallic acid |
-
2010
- 2010-05-26 CN CN201010182726A patent/CN101864460A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102603919A (en) * | 2012-04-13 | 2012-07-25 | 赵岩 | Method for preparing alginic acid and sodium alginate through air steam explosion coupling biological compound enzyme technology |
| CN111521710A (en) * | 2020-05-12 | 2020-08-11 | 劲牌持正堂药业有限公司 | Determination method for improving gallic acid content and stability in bistort rhizome |
| CN112877373A (en) * | 2021-01-26 | 2021-06-01 | 桂林莱茵生物科技股份有限公司 | Preparation method for obtaining gallic acid with content of more than 99% |
| CN112877373B (en) * | 2021-01-26 | 2023-03-21 | 桂林莱茵生物科技股份有限公司 | Preparation method for obtaining gallic acid with content of more than 99% |
| WO2023051745A1 (en) * | 2021-09-30 | 2023-04-06 | 上海百斯杰生物工程有限公司 | Method for producing gallic acid |
| CN114426478A (en) * | 2022-01-28 | 2022-05-03 | 广西壮族自治区中国科学院广西植物研究所 | High-content gallic acid and preparation method thereof |
| CN114426478B (en) * | 2022-01-28 | 2023-10-31 | 广西壮族自治区中国科学院广西植物研究所 | High-content gallic acid and preparation method thereof |
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Application publication date: 20101020 |