CN104529954A - Method for extracting andrographolide from common andrographis herb and andrographolide finished products - Google Patents
Method for extracting andrographolide from common andrographis herb and andrographolide finished products Download PDFInfo
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- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
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Abstract
The invention relates to the technical field of andrographolide extraction, and in particular relates to a method for extracting andrographolide from common andrographis herb and andrographolide finished products obtained by using the method. The method comprises the following steps: performing enzymatic hydrolysis pretreatment on the whole herb of common andrographis herb or common andrographis herb coarse powder by using a compound enzyme of acidic cellulose and acidic xylanase, wherein the enzymatic hydrolysis pretreatment comprises spraying and heat preservation treatment processes; and performing alcohol extraction treatment on the whole herb of common andrographis herb or the common andrographis herb coarse powder subjected to pretreatment. According to an extraction method disclosed by the invention, expensive equipment does not need to be used, and the extraction cost of andrographolide can be reduced.
Description
Technical field
The present invention relates to the extractive technique field of rographolide, particularly relate to a kind of method extracting rographolide from Herba Andrographis and the rographolide finished product obtained by the method.
Background technology
Rographolide be acanthaceous plant Herba Andrographis mainly contain effective constituent, there is the effects such as antibacterial, anti-inflammatory, relieving cough and asthma, clearing heat and detoxicating, cool blood detumescence, especially there is special efficacy to bacillary with viral upper respiratory tract infection and dysentery, be described as natural antibiotics medicine.Due to rographolide complex structure, synthetic difficulty, therefore, domestic all extraction from vegetable drug obtains.
At present, about rographolide extracting method report more, specifically comprise water extraction, alcohol extracting method, potass extraction method etc., these technological operations are simple, but have that extraction efficiency is low, raw material rate of utilization is low, solvent usage quantity is large and the problem such as the difficult removal of impurity, and other extracting method, such as supercritical extraction, ultrasonic-assisted extraction, microwave radiation exaraction, resin adsorption method etc., although the higher rographolide of purity can be obtained, but required apparatus expensive, substantially increase production cost, and be difficult to be applied to industrialization scale operation.
Summary of the invention
The invention provides a kind of rographolide finished product extracting rographolide method and obtained by the method from Herba Andrographis, not increasing in extracting solution while impurity, without the need to using expensive equipment, reducing the extraction cost of rographolide.
First the embodiment of the present invention provides a kind of from Herba Andrographis, extracts rographolide method, and the method comprises:
Adopt acidic cellulase and acidic xylanase prozyme to carry out enzymolysis pre-treatment to Herba Andrographis herb or Herba Andrographis meal, described enzymolysis pre-treatment is the treatment process spraying and be incubated;
Ethanol-extracted process is carried out to pretreated Herba Andrographis herb or Herba Andrographis meal.
In technical solution of the present invention, first acidic cellulase and the cell wall substance of acidic xylanase prozyme to Herba Andrographis is utilized to degrade, change the permeability of cell walls, facilitate the stripping of rographolide, dissolution time is short, and do not increase other impurity, be beneficial to follow-up employing ethanol-extracted and process.Experiment shows that in the rographolide finished product obtained by technical scheme of the present invention, the content of Herba Andrographis is higher.In addition, enzyme digestion reaction does not need very high temperature, avoids rographolide thermo-labile, and high temperature easily decomposes the problem of loss.In addition, be not also significantly increased by the impurity of the extracting solution of the rographolide after enzymolysis pre-treatment and ethanol-extracted process, be easy to follow-up separation and purification.And technical scheme of the present invention does not need expensive equipment, decreases equipment cost, and then reduces production cost.
Preferably, the consumption of described acidic cellulase is the 300u/g-1200u/g of Herba Andrographis over dry meter, and the consumption of described acidic xylanase is the 600u/g-2400u/g of Herba Andrographis over dry meter.
Preferably, the pretreated hydrolysis temperature of described enzymolysis is 35 DEG C-50 DEG C, and enzymolysis time is 0.5-2h, and enzyme liquid concentration is 3%-10%.
Preferably, extract in rographolide method from Herba Andrographis of the present invention, described ethanol-extracted process specifically comprises:
Pretreated Herba Andrographis herb or Herba Andrographis meal are added the ethanol that concentration is 70%-95%, heating and refluxing extraction twice, each 1.5 hours, ethanol consumption was 8 times of Herba Andrographis dry weight for the first time, second time ethanol consumption is 6 times of Herba Andrographis dry weight, merges the phegma of twice;
Filtration leaching is carried out to described phegma, obtains extracting solution.
Preferably, extract in rographolide method from Herba Andrographis of the present invention, also comprise after ethanol-extracted process is carried out to pretreated Herba Andrographis herb or Herba Andrographis meal:
In described extracting solution, add diatomite and gac, mixing, stir 20-40 minute, suction filtration obtains filtrate, and wherein diatomaceous consumption is 0.1-0.5g/100ml filtrate, and the consumption of gac is 1-2g/100ml filtrate.
Preferably, extract in rographolide method from Herba Andrographis of the present invention, also comprise after obtained filtrate:
Be 1.20 ± 0.01g/cm by described filtrate decompression vacuum concentration to density
3, obtained rographolide medicinal extract, hold over night below 4 DEG C, suction filtration after crystal is separated out, collect crystal, by described crystal ethanol back dissolving, recrystallization obtains rographolide finished product.
The present invention also provides a kind of rographolide finished product, by above-mentioned any one from Herba Andrographis, extract rographolide method obtain, in described rographolide finished product, the content of rographolide is 95%-98%.In this rographolide finished product, the content of rographolide is higher.
Embodiment
In order to reduce the extraction cost of rographolide, embodiments provide a kind of rographolide finished product extracting rographolide method and obtained by the method from Herba Andrographis, in this technical scheme, first acidic cellulase and the cell wall substance of acidic xylanase prozyme to Herba Andrographis is utilized to degrade, change the permeability of cell walls, facilitate the stripping of rographolide, dissolution time is short, and do not increase impurity, be beneficial to follow-up employing ethanol-extracted process, in this process, without the need to using expensive equipment, under the prerequisite keeping higher extracted rate, reduce extraction cost.For making the object, technical solutions and advantages of the present invention clearly, by the following examples the present invention is described in further detail.
First the embodiment of the present invention provides a kind of from Herba Andrographis, extracts rographolide method, and the method comprises:
Adopt acidic cellulase and acidic xylanase prozyme to carry out enzymolysis pre-treatment to Herba Andrographis herb or Herba Andrographis meal, described enzymolysis pre-treatment is the treatment process spraying and be incubated;
Ethanol-extracted process is carried out to pretreated Herba Andrographis herb or Herba Andrographis meal.
Because plant cell wall is made up of Mierocrystalline cellulose, hemicellulose etc., its dense structure hinders the stripping of effective constituent in cell, make extraction efficiency lower, and in technical solution of the present invention, first utilize acidic cellulase and the cell wall substance of acidic xylanase prozyme to Herba Andrographis to degrade, change the permeability of cell walls, facilitate the stripping of rographolide, dissolution time is short, and does not increase impurity, is beneficial to follow-up employing ethanol-extracted process.Experiment shows that in the rographolide finished product obtained by technical scheme of the present invention, the content of Herba Andrographis is higher.In addition, enzyme digestion reaction does not need very high temperature, avoids rographolide thermo-labile, and high temperature easily decomposes the problem of loss.In addition, be not also significantly increased by the impurity of the extracting solution of the rographolide after enzymolysis pre-treatment and ethanol-extracted process, be easy to follow-up separation and purification.And technical scheme of the present invention does not need expensive equipment, decreases equipment cost, and then reduces production cost.
Here it should be noted that, in view of rographolide is stablized in acid condition, and it is unstable in neutral and alkaline conditions, therefore the present invention adopts acidic cellulase and acidic xylanase prozyme to carry out enzymolysis pre-treatment to Herba Andrographis herb or Herba Andrographis meal, prevent the destruction of rographolide, be also conducive to improving extraction efficiency.PH value during this enzymolysis pre-treatment is 3.0-6.2, and preferable ph is 4.0-5.5.This enzymolysis pretreatment technology is the treatment process spraying and be incubated, and the enzyme liquid namely adopting acidic cellulase and acidic xylanase prozyme to be formed sprays Herba Andrographis meal or Herba Andrographis herb, under hydrolysis temperature, be then incubated the duration of setting.
In addition, first enzymolysis pre-treatment is adopted to carry out ethanol-extracted process again, such sequence of steps relative to the advantage of first carrying out ethanol-extracted process and carry out enzyme extraction process is: first ethanol-extracted again enzymolysis processing and ethanol-extracted and enzymolysis processing is carried out this two schemes simultaneously and all be have employed ethanol, enzyme denaturation inactivation can be caused like this, normal catalysis can not be played, and first enzymolysis processing carries out ethanol-extracted again, ethanol can not impact the catalyzed reaction of enzyme.
Preferably, the consumption of described acidic cellulase is the 300u/g-1200u/g of Herba Andrographis over dry meter, and the consumption of described acidic xylanase is the 600u/g-2400u/g of Herba Andrographis over dry meter.
When the consumption of acidic cellulase is lower than the 300u/g of Herba Andrographis over dry meter, because enzyme concn is lower, catalyzed degradation Herba Andrographis cell wall cellulose DeGrain, little on the impact of rographolide extraction yield, when the consumption of acidic cellulase is higher than the 1200u/g of Herba Andrographis over dry meter, the catalytic efficiency of enzyme reaches stationary value, then increases enzyme dosage and can cause unnecessary waste; When the consumption of acidic xylanase is lower than the 600u/g of Herba Andrographis over dry meter, then do not have synergy with acidic cellulase, the stripping of rographolide can not be promoted, when the consumption of acidic xylanase is higher than the 2400u/g of Herba Andrographis over dry meter, rographolide extraction rate reached, to stable, can not increase again.In addition, acid cellulose enzyme dosage is preferably 600u/g-1200u/g, and the consumption of acidic xylanase is preferably 900u/g-2400u/g.
Preferably, the pretreated hydrolysis temperature of described enzymolysis is 35 DEG C-50 DEG C, and enzymolysis time is 0.5-2 hour (h), and enzyme liquid concentration is 3%-10%.
At this, enzyme liquid concentration is the mass ratio of the quality of acidic cellulase and acidic xylanase prozyme and the aqueous solution of this prozyme.
Preferably, extract in rographolide method from Herba Andrographis of the present invention, described ethanol-extracted process specifically comprises:
Pretreated Herba Andrographis herb or Herba Andrographis meal are added the ethanol that concentration is 70%-95%, heating and refluxing extraction twice, each 1.5 hours, ethanol consumption was 8 times of Herba Andrographis dry weight for the first time, second time ethanol consumption is 6 times of Herba Andrographis dry weight, merges the phegma of twice;
Filtration leaching is carried out to described phegma, obtains extracting solution.
Preferably, extract in rographolide method from Herba Andrographis of the present invention, also comprise after ethanol-extracted process is carried out to pretreated Herba Andrographis herb or Herba Andrographis meal:
In described extracting solution, add diatomite and gac, mixing, stir 20-40 minute, suction filtration obtains filtrate, and wherein diatomaceous consumption is 0.1-0.5g/100ml filtrate, and the consumption of gac is 1-2g/100ml filtrate.Use diatomite and gac to carry out Impurity removal to extracting solution, only need to adopt suction filtration, avoid and use sherwood oil, acetone and other organic solvent pollution on the environment, also reduce the cost using the expensive device such as resin.
Preferably, extract in rographolide method from Herba Andrographis of the present invention, also comprise after obtained filtrate:
Be 1.20 ± 0.01g/cm by described filtrate decompression vacuum concentration to density
3, obtained rographolide medicinal extract, hold over night below 4 DEG C, suction filtration after crystal is separated out, collect crystal, by described crystal ethanol back dissolving, recrystallization obtains rographolide finished product.
The present invention also provides a kind of rographolide finished product, by above-mentioned any one from Herba Andrographis, extract rographolide method obtain, in described rographolide finished product, the content of rographolide is 95%-98%.In this rographolide finished product, the content of rographolide is higher.
Below by way of specific embodiment, the rographolide finished product that the present invention extracts rographolide method and obtained by the method from Herba Andrographis is described.
Embodiment 1
Prepare the enzyme liquid of acidic cellulase and acidic xylanase prozyme, get acidic cellulase 300u/g (Herba Andrographis over dry meter), acidic xylanase 600u/g (Herba Andrographis over dry meter), add water stirring and dissolving, is configured to the complex enzyme liquid that concentration is 3%.Get Herba Andrographis herb 10kg and be sliced into 1-2cm, complex enzyme liquid is evenly sprayed in Herba Andrographis section, mixes, enzymolysis processing 0.4h, 0.5h, 1h, 2h, 2.5h is incubated at 35 DEG C, after reaction terminates, add the alcohol reflux twice that concentration is 85%, each 1.5 hours, ethanol consumption is 8 times of Herba Andrographis dry weight for the first time, second time ethanol consumption is 6 times of Herba Andrographis dry weight, merges the phegma of twice, carries out filtration leaching to phegma, obtain extracting solution, stand-by.Remaining Herba Andrographis residue (abbreviation residue) with clear water washing, dry, utilize Determination of Andrographolide in high effective liquid chromatography for measuring residue, measurement result in table 1, i.e. residue lactone content in table 1.
Diatomite and 2% (g/ml) gac of 0.5% (g/ml) is added in extracting solution, mixing, stir 30min, suction filtration obtains filtrate, utilize Determination of Andrographolide in high effective liquid chromatography for measuring filtrate, calculate the extraction yield of rographolide, wherein, rographolide in extraction yield=filtrate/Herba Andrographis dry weight × 100%, in filtrate the content of rographolide and the rographolide of calculating extraction yield the results are shown in Table 1, be namely respectively the filtrate lactone content in table 1 and lactone extraction yield.
By filtrate decompression vacuum concentration to density 1.20 ± 0.01g/cm
3obtained rographolide medicinal extract, hold over night below 4 DEG C, suction filtration after crystal is separated out, collects crystal, by the crystal ethanol back dissolving of collecting, recrystallization obtains rographolide finished product, utilize Determination of Andrographolide in high effective liquid chromatography for measuring rographolide finished product, the results are shown in Table 1, the finished product lactone content namely in table 1.
Wherein, the test condition of high performance liquid chromatography measures according to Chinese Pharmacopoeia (2010 editions) high performance liquid chromatography (annex VI D), also adopts this test condition in following examples.
Table 1 enzymolysis processing duration is on the impact of Determination of Andrographolide and extraction yield
As shown in Table 1, when enzymolysis duration is 2h, in Herba Andrographis finished product, the content of rographolide reaches 96%.And along with the further increase of time, in Herba Andrographis finished product, the content of rographolide does not effectively increase.When enzymolysis duration is lower than 0.5h, because the reaction times is shorter, catalytic effect is not obvious.
Embodiment 2
Prepare the enzyme liquid of acidic cellulase and acidic xylanase prozyme, get acidic cellulase 1200u/g (Herba Andrographis over dry meter), acidic xylanase 900u/g (Herba Andrographis over dry meter), add water stirring and dissolving, is configured to the complex enzyme liquid that concentration is respectively 1%, 3%, 5%, 10%, 15%.Get Herba Andrographis meal 10kg, spray by complex enzyme liquid and mix, at 45 DEG C, be incubated enzymolysis processing 2h, after reaction terminates, adding concentration is 85% alcohol reflux twice, each 1.5 hours, ethanol consumption was 8 times of Herba Andrographis dry weight for the first time, and second time ethanol consumption is 6 times of Herba Andrographis dry weight, merge the phegma of twice, filtration leaching is carried out to phegma, obtains extracting solution, stand-by.Remaining Herba Andrographis residue (abbreviation residue) with clear water washing, dry, utilize Determination of Andrographolide in high effective liquid chromatography for measuring residue, measurement result in table 2, i.e. residue lactone content in table 2.
Diatomite and 1.5% (g/ml) gac of 0.2% (g/ml) is added in extracting solution, mixing, stir 40min, suction filtration obtains filtrate, Determination of Andrographolide in high effective liquid chromatography for measuring clear liquor, calculate the extraction yield of rographolide, the extraction yield of Determination of Andrographolide and calculating in filtrate the results are shown in Table 2, be namely respectively the filtrate lactone content in table 2 and lactone extraction yield.
By filtrate decompression vacuum concentration to density 1.20 ± 0.01g/cm
3obtained rographolide medicinal extract, hold over night below 4 DEG C, suction filtration after crystal is separated out, collects crystal, by the crystal ethanol back dissolving of collecting, recrystallization obtains rographolide finished product, utilize Determination of Andrographolide in high effective liquid chromatography for measuring rographolide finished product, the results are shown in Table 2, the finished product lactone content namely in table 2.
Table 2 enzyme liquid concentration is on the impact of Determination of Andrographolide and extraction yield
As shown in Table 2, when enzyme liquid concentration is 5%, in Herba Andrographis finished product, the content of rographolide reaches 98%.When enzyme liquid concentration lower than 3% time, enzyme liquid concentration is lower, and catalysis shell-broken effect is not obvious, when enzyme liquid concentration is higher than 10%, because enzyme liquid measure is less, be unfavorable for spray mixing, fully react.
Embodiment 3
Prepare acidic cellulase and acidic xylanase prozyme, get acidic cellulase 900u/g (Herba Andrographis over dry meter), acidic xylanase 2400u/g (Herba Andrographis over dry meter), add water stirring and dissolving, is configured to the complex enzyme liquid that concentration is 5%.Get Herba Andrographis meal 10kg, spray by complex enzyme liquid and mix, at 30 DEG C, 35 DEG C, 45 DEG C, 50 DEG C, 55 DEG C, be incubated enzymolysis processing 2h, after reaction terminates, adding concentration is 90% alcohol reflux twice, each 1.5 hours, ethanol consumption was 8 times of Herba Andrographis dry weight for the first time, and second time ethanol consumption is 6 times of Herba Andrographis dry weight, merge the phegma of twice, filtration leaching is carried out to phegma, obtains extracting solution, stand-by.Remaining Herba Andrographis residue (abbreviation residue) with clear water washing, dry, utilize Determination of Andrographolide in high effective liquid chromatography for measuring residue, measurement result in table 3, i.e. residue lactone content in table 3.
Extracting solution adds diatomite and 1.5% (g/ml) gac of 0.5% (g/ml), mixing, stir 40min, suction filtration obtains filtrate, utilize Determination of Andrographolide in high effective liquid chromatography for measuring clear liquor, calculate the extraction yield of rographolide.The extraction yield of Determination of Andrographolide and calculating in filtrate the results are shown in Table 3, be namely respectively the filtrate lactone content in table 3 and lactone extraction yield.
By filtrate decompression vacuum concentration to density 1.20 ± 0.01g/cm
3obtained rographolide medicinal extract, hold over night below 4 DEG C, suction filtration after crystal is separated out, collects crystal, by the crystal ethanol back dissolving of collecting, recrystallization obtains rographolide finished product, utilize Determination of Andrographolide in high effective liquid chromatography for measuring rographolide finished product, the results are shown in Table 3, the finished product lactone content namely in table 3.
Table 3 hydrolysis temperature is on the impact of Determination of Andrographolide and extraction yield
As shown in Table 3, when hydrolysis temperature is 45 DEG C, the extraction rate reached of rographolide to maximum, and now in finished product the content of rographolide also up to 98%.When hydrolysis temperature is lower than 35 DEG C, do not reach the optimal reactive temperature of prozyme, catalytic efficiency is low.When temperature is higher than 45 DEG C, the change of rographolide extraction efficiency is little, when temperature is higher, just can cause enzyme deactivation.
Embodiment 4
Adopt acidic cellulase in this embodiment, acidic xylanase processes Herba Andrographis herb separately, and acidic cellulase and acidic xylanase by a certain percentage compound Herba Andrographis herb is processed, enzyme A is the acidic cellulase of 600u/g (Herba Andrographis over dry meter) consumption, enzyme B is the acidic xylanase of 1200u/g (Herba Andrographis over dry meter) consumption, enzyme C is the prozyme of the acidic cellulase of 600u/g (Herba Andrographis over dry meter) consumption and the acidic xylanase of 1200u/g (Herba Andrographis over dry meter) consumption, add water stirring and dissolving respectively, be configured to the complex enzyme liquid that concentration is 5%.Get Herba Andrographis herb 10kg and be sliced into 1-2cm, complex enzyme liquid is evenly sprayed in Herba Andrographis section, mixes, enzymolysis processing 2h is incubated at 45 DEG C, after reaction terminates, add the alcohol reflux twice that concentration is 85%, each 1.5 hours, ethanol consumption is 8 times of Herba Andrographis dry weight for the first time, second time ethanol consumption is 6 times of Herba Andrographis dry weight, merges the phegma of twice, carries out filtration leaching to phegma, obtain extracting solution, stand-by.Remaining Herba Andrographis residue (abbreviation residue) with clear water washing, dry, utilize Determination of Andrographolide in high effective liquid chromatography for measuring residue, measurement result in table 4, i.e. residue lactone content in table 4.
In extracting solution, add diatomite and 2% (g/ml) gac of 0.5% (g/ml), mixing, stir 30min, suction filtration obtains filtrate.Utilize Determination of Andrographolide in high effective liquid chromatography for measuring clear liquor, calculate the extraction yield of rographolide.The extraction yield of Determination of Andrographolide and calculating in filtrate the results are shown in Table 4, be namely respectively the filtrate lactone content in table 4 and lactone extraction yield.
By filtrate decompression vacuum concentration to density 1.20 ± 0.01g/cm
3obtained rographolide medicinal extract, hold over night below 4 DEG C, suction filtration after crystal is separated out, collects crystal, by the crystal ethanol back dissolving of collecting, recrystallization obtains rographolide finished product, utilize Determination of Andrographolide in high effective liquid chromatography for measuring rographolide finished product, the results are shown in Table 4, the finished product lactone content namely in table 4.
The different enzyme of table 4 is on the impact of Determination of Andrographolide and extraction yield
As shown in Table 4, when adopting separately acidic cellulase or acidic xylanase, rographolide extraction efficiency is lower, when acidic cellulase and acidic xylanase by a certain percentage compound use time, under the synergy of acidic xylanase, accelerate the stripping of rographolide, extraction efficiency obviously increases.
Below, the advantage of the present invention relative to prior art is summed up:
Adopt enzymolysis pre-treatment, because enzymatic hydrolysis condition is gentle, avoid the pyrolytic decomposition of rographolide, and enzymolysis pre-treatment is consuming time short, and efficiency is high.Adopt extracting method of the present invention, known by above-described embodiment 1 to 4, in extracting solution, the content of rographolide is substantially more than 80%, even up to 85%, and in residue the content of rographolide substantially lower than 1%, even minimumly be only 0.2%, and extraction yield is substantially more than 80%, even up to 92%;
In addition, impurity in extracting solution is not significantly increased, be easy to follow-up separation and purification, utilize diatomite and remove impurity with active carbon, can obtain content up to 98% rographolide, avoid and use sherwood oil, acetone and other organic solvent pollution on the environment, decrease the cost using the expensive device such as resin;
In addition, extracting method technique of the present invention is simple, easy handling, and without the need to adding any equipment, application is convenient, is beneficial to large-scale production.
Obviously, those skilled in the art can carry out various change and modification to the present invention and not depart from the spirit and scope of the present invention.Like this, if these amendments of the present invention and modification belong within the scope of the claims in the present invention and equivalent technologies thereof, then the present invention is also intended to comprise these change and modification.
Claims (7)
1. from Herba Andrographis, extract a method for rographolide, it is characterized in that, comprising:
Adopt acidic cellulase and acidic xylanase prozyme to carry out enzymolysis pre-treatment to Herba Andrographis herb or Herba Andrographis meal, described enzymolysis pre-treatment is the treatment process spraying and be incubated;
Ethanol-extracted process is carried out to pretreated Herba Andrographis herb or Herba Andrographis meal.
2. the method for claim 1, is characterized in that, the consumption of described acidic cellulase is the 300u/g-1200u/g of Herba Andrographis over dry meter, and the consumption of described acidic xylanase is the 600u/g-2400u/g of Herba Andrographis over dry meter.
3. the method for claim 1, is characterized in that, the pretreated hydrolysis temperature of described enzymolysis is 35 DEG C-50 DEG C, and enzymolysis time is 0.5-2h, and enzyme liquid concentration is 3%-10%.
4. the method as described in any one in claim 1-3, is characterized in that, described ethanol-extracted process specifically comprises:
Pretreated Herba Andrographis herb or Herba Andrographis meal are added the ethanol that concentration is 70%-95%, heating and refluxing extraction twice, each 1.5 hours, ethanol consumption was 8 times of Herba Andrographis dry weight for the first time, second time ethanol consumption is 6 times of Herba Andrographis dry weight, merges the phegma of twice;
Filtration leaching is carried out to described phegma, obtains extracting solution.
5. method as claimed in claim 4, is characterized in that, also comprise after carrying out ethanol-extracted process to pretreated Herba Andrographis herb or Herba Andrographis meal:
In described extracting solution, add diatomite and gac, mixing, stir 20-40 minute, suction filtration obtains filtrate, and wherein diatomaceous consumption is 0.1-0.5g/100ml filtrate, and the consumption of gac is 1-2g/100ml filtrate.
6. method as claimed in claim 5, is characterized in that, also comprise after obtained filtrate:
Be 1.20 ± 0.01g/cm by described filtrate decompression vacuum concentration to density
3, obtained rographolide medicinal extract, hold over night below 4 DEG C, suction filtration after crystal is separated out, collect crystal, by described crystal ethanol back dissolving, recrystallization obtains rographolide finished product.
7. a rographolide finished product, is characterized in that, described rographolide finished product is obtained by the method described in any one of claim 1 ~ 6, and in described rographolide finished product, the content of rographolide is 95%-98%.
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| CN107746395A (en) * | 2017-10-23 | 2018-03-02 | 吉林大学珠海学院 | A kind of method of andrographolide in extraction chuanxinlian tablet |
| CN114015732A (en) * | 2021-11-29 | 2022-02-08 | 陕西嘉禾生物科技股份有限公司 | Industrial preparation method of andrographolide and dehydroandrographolide |
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| CN103145660A (en) * | 2013-03-25 | 2013-06-12 | 成都天台山制药有限公司 | Andrographolide and preparation method thereof |
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| CN114015732A (en) * | 2021-11-29 | 2022-02-08 | 陕西嘉禾生物科技股份有限公司 | Industrial preparation method of andrographolide and dehydroandrographolide |
| CN114015732B (en) * | 2021-11-29 | 2024-03-01 | 陕西嘉禾生物科技股份有限公司 | Industrial preparation method of andrographolide and dehydroandrographolide |
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