CN107569535A - A kind of method for extracting anisetree bark active ingredient - Google Patents
A kind of method for extracting anisetree bark active ingredient Download PDFInfo
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- CN107569535A CN107569535A CN201710863160.2A CN201710863160A CN107569535A CN 107569535 A CN107569535 A CN 107569535A CN 201710863160 A CN201710863160 A CN 201710863160A CN 107569535 A CN107569535 A CN 107569535A
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- anisetree bark
- active ingredient
- anisetree
- eluent
- moving bed
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Abstract
It is to be crushed to anisetree bark the invention discloses a kind of method for extracting anisetree bark active ingredient, sieving, adds ethanol and carry out refluxing extraction, merging filtrate；After filtrate decompression concentration, anisetree bark crude extract is obtained, n-Butanol soluble is added in anisetree bark crude extract, is made into sample introduction solution；Sample introduction solution is delivered into Simulation moving bed to be isolated and purified, the chromatographic column filling molecular sieve resin of the moving bed, eluant, eluent is n-butanol and ethyl acetate mixed solvent, obtains eluent；By eluent again by being concentrated under reduced pressure, it is dried in vacuo, that is, obtains anisetree bark active ingredient.The anisetree bark crude extract of the inventive method carries out separating-purifying by Simulation moving bed, substantially increases the purity and the rate of recovery of anisetree bark active ingredient, effective approach is provided for the utilization of anisetree bark medicine.
Description
Technical field
The present invention relates to effective ingredients in plant extractive technique field, specifically a kind of side for extracting anisetree bark active ingredient
Method.
Background technology
Anisetree bark（Illicium difengpi K.I.B.et K.I.M.）For the dry of Magnoliaceae anise platymiscium anisetree bark
Dry bark, alias have bulky, short bee saage of Cortex Illicii, Cortex schizophragmatis integrifolii radicis, Chinese hydrangeavine root-bark, maple etc., its taste micro-pungent, puckery medicine, warm-natured, are removed with wind-dispelling
Wet, swelling and pain relieving effect, cures mainly arthralgia pain due to rheumatism, traumatic injury etc..Anisetree bark mainly contains steroid saponin, flavonoids, organic
The compositions such as acids, triterpene acids, Phenylpropanoid Glycosides glucoside and lignanoid's glucoside.Wherein flavone compound and steroid saponin compound
It is the material with obvious anti-inflammatory pharmacological activity.Have now been developed at present and a variety of related medicinal material is aided with by main ingredient using anisetree bark be made
Medicament, such as：FENGSHI GUANJIEYAN PIAN, osmanthus dragon ointment, chill are double from turning piece, beater wheel mill, chasing after easypro channels and collaterals blood circulation promoting slice of wind etc., can
See that anisetree bark has broad application prospects on field of medicaments.Up to now it is more rare to be related to anisetree bark extracts active ingredients
Relevant report, existing anisetree bark extracts active ingredients purification process all has that process is cumbersome, cost is high, active constituent content
Low drawback, and the technology for the flavone compound and saponins compound for obtaining high content simultaneously is not also reported, therefore,
Existing anisetree bark extracts active ingredients purification technique is difficult to industrialized production.
The content of the invention
The problem of present invention exists for existing anisetree bark extraction process of effective component, there is provided one kind utilizes Simulation moving bed
The method that technology extracts anisetree bark active ingredient.The inventive method have technique is simple, active ingredient yield is high, purity is high, into
This low, easy the advantages that realizing industrialized production.
In order to realize the above object the technical solution adopted by the present invention is as follows：
A kind of method for extracting anisetree bark active ingredient, comprises the following steps：
（1）Anisetree bark is crushed to 100-150 mesh, sieved, the ethanol for being incorporated as 5-8 times of anisetree bark medicinal material weight every time is returned
Stream extraction 2-3 times, merging filtrate；
（2）By step（1）Filtrate decompression concentration after, obtain anisetree bark crude extract, anisetree bark crude extract add n-Butanol soluble,
It is made into the sample introduction solution that mass concentration is 10-20%；
（3）Sample introduction solution is delivered into Simulation moving bed to be isolated and purified, the chromatographic column filling molecular sieve tree of the moving bed
Fat, eluant, eluent are n-butanol and ethyl acetate mixed solvent, obtain eluent；
（4）By above-mentioned eluent again by being concentrated under reduced pressure, it is dried in vacuo, that is, obtains anisetree bark active ingredient.
Further, described refluxing extraction temperature is 50-60 DEG C, each refluxing extraction 1-2h.
Further, the vacuum being concentrated under reduced pressure be -0.06 ~ -0.08Mpa, temperature be 55-65 DEG C.
Further, the volume ratio of n-butanol and ethyl acetate is 2-4 in the eluant, eluent:1.
Further, it is described vacuum drying be vacuum be -0.06 ~ -0.08Mpa, temperature be at 50-60 DEG C drying.
Further, it is described to utilize Simulation moving bed to control elution flow rate pump 50-100mL/min, pressure when isolating and purifying
6-8MPa, sample introduction flow rate pump 10-20mL/min, pressure 6-8MPa, 40-50 DEG C of operating temperature.
Further, total saponin content is 25-32%, general flavone content 30-40% in the anisetree bark active ingredient.
Compared with prior art, advantages of the present invention and have the beneficial effect that：
1st, the inventive method anisetree bark crude extract by Simulation moving bed carry out separating-purifying, substantially increase anisetree bark effectively into
The purity and the rate of recovery divided, total saponin content is 25-32%, general flavone content 30-40% wherein in extract, is anisetree bark medicine
The utilization of thing provide effective approach.
2nd, the present invention is continous way production using Simulation moving bed, overcomes the defects of intermittent production of column chromatography is present,
Simulation moving bed has production automation degree height, operating efficiency is high, cost is relatively low, production environment safety and environmental protection, easily realizes
Industrialized production.
3rd, the present invention, can be preferably real using molecular sieve as stationary phase using n-butanol and ethyl acetate as mobile phase
The separation of existing anisetree bark active ingredient and other impurities, improve the purity of active ingredient total saposins and general flavone.
4th, the inventive method has the advantages that technique is simple, consume energy low, safety and environmental protection, cost are cheap, easily realizes industry
Metaplasia is produced, and effective approach is provided for the utilization of anisetree bark medicinal material.
Embodiment
The present invention program is further described below in conjunction with specific embodiment, but is not limited to the protection model of the present invention
Enclose.
Embodiment 1
A kind of method for extracting anisetree bark active ingredient, comprises the following steps：
（1）Anisetree bark 10kg is crushed to 100 mesh, sieved, the ethanol for being incorporated as 6 times of anisetree bark medicinal material weight every time is flowed back
Extraction 3 times, refluxing extraction temperature are 60 DEG C, first time refluxing extraction 2h, second of refluxing extraction 1.5h, third time refluxing extraction
1h, merging filtrate；
（2）By step（1）Filtrate vacuum be -0.06 Mpa, temperature be 60 DEG C and be concentrated under reduced pressure into paste, obtain anisetree bark
Crude extract, n-Butanol soluble is added in anisetree bark crude extract, be made into the sample introduction solution that mass concentration is 15%；
（3）Sample introduction solution is delivered into Simulation moving bed to be isolated and purified, the chromatographic column filling molecular sieve tree of the moving bed
Fat, eluant, eluent are that volume is 3:1 n-butanol and ethyl acetate mixed solvent, obtains eluent；It is described to utilize Simulation moving bed point
Control elution flow rate pump 50mL/min, pressure 6MPa, sample introduction flow rate pump 15mL/min, pressure 6MPa during from purifying, work temperature
45 DEG C of degree.
（4）By above-mentioned eluent vacuum be -0.06 Mpa, temperature be 60 DEG C and be concentrated under reduced pressure into paste, in vacuum
It is to be dried in vacuo at 50 DEG C to spend for -0.06 Mpa, temperature, that is, obtains anisetree bark active ingredient.
Anisetree bark active ingredient obtained by the present embodiment detects by HPLC, and wherein total saponin content is 28.41%, total yellow
Ketone content is 37.29%.
Embodiment 2
A kind of method for extracting anisetree bark active ingredient, comprises the following steps：
（1）Anisetree bark 5kg is crushed to 100 mesh, sieved, the ethanol for being incorporated as 5 times of anisetree bark medicinal material weight every time is flowed back
Extraction 2 times, refluxing extraction temperature are 55 DEG C, first time refluxing extraction 2h, second of refluxing extraction 1h, third time refluxing extraction
1h, merging filtrate；
（2）By step（1）Filtrate vacuum be -0.06 Mpa, temperature be 65 DEG C and be concentrated under reduced pressure into paste, obtain anisetree bark
Crude extract, n-Butanol soluble is added in anisetree bark crude extract, be made into the sample introduction solution that mass concentration is 20%；
（3）Sample introduction solution is delivered into Simulation moving bed to be isolated and purified, the chromatographic column filling molecular sieve tree of the moving bed
Fat, eluant, eluent are that volume is 4:1 n-butanol and ethyl acetate mixed solvent, obtains eluent；It is described to utilize Simulation moving bed point
Control elution flow rate pump 100mL/min, pressure 8MPa, sample introduction flow rate pump 20mL/min, pressure 8MPa during from purifying, work temperature
50 DEG C of degree.
（4）By above-mentioned eluent vacuum be -0.06 Mpa, temperature be 65 DEG C and be concentrated under reduced pressure into paste, in vacuum
It is to be dried in vacuo at 60 DEG C to spend for -0.06 Mpa, temperature, that is, obtains anisetree bark active ingredient.
Anisetree bark active ingredient obtained by the present embodiment detects by HPLC, and wherein total saponin content is 26.07%, total yellow
Ketone content is 34.87%.
Embodiment 3
A kind of method for extracting anisetree bark active ingredient, comprises the following steps：
（1）Anisetree bark 5kg is crushed to 120 mesh, sieved, the ethanol for being incorporated as 8 times of anisetree bark medicinal material weight every time is flowed back
Extraction 2 times, refluxing extraction temperature are 60 DEG C, first time refluxing extraction 2h, second of refluxing extraction 1.5h, merging filtrate；
（2）By step（1）Filtrate vacuum be -0.08Mpa, temperature be 55 DEG C and be concentrated under reduced pressure into paste, obtain anisetree bark
Crude extract, n-Butanol soluble is added in anisetree bark crude extract, be made into the sample introduction solution that mass concentration is 12%；
（3）Sample introduction solution is delivered into Simulation moving bed to be isolated and purified, the chromatographic column filling molecular sieve tree of the moving bed
Fat, eluant, eluent are that volume is 2:1 n-butanol and ethyl acetate mixed solvent, obtains eluent；It is described to utilize Simulation moving bed point
Control elution flow rate pump 80mL/min, pressure 7MPa, sample introduction flow rate pump 15mL/min, pressure 7MPa during from purifying, work temperature
40 DEG C of degree.
（4）By above-mentioned eluent vacuum be -0.068Mpa, temperature be 55 DEG C and be concentrated under reduced pressure into paste, in vacuum
It is to be dried in vacuo at 55 DEG C to spend for -0.08 Mpa, temperature, that is, obtains anisetree bark active ingredient.
Anisetree bark active ingredient obtained by the present embodiment detects by HPLC, and wherein total saponin content is 29.74%, total yellow
Ketone content is 32.15%.
Embodiment 4
A kind of method for extracting anisetree bark active ingredient, comprises the following steps：
（1）Anisetree bark 10kg is crushed to 150 mesh, sieved, the ethanol for being incorporated as 7 times of anisetree bark medicinal material weight every time is flowed back
Extraction 3 times, refluxing extraction temperature are 50 DEG C, first time refluxing extraction 1.5h, second of refluxing extraction 1h, third time refluxing extraction
1h, merging filtrate；
（2）By step（1）Filtrate vacuum be -0.06 Mpa, temperature be 60 DEG C and be concentrated under reduced pressure into paste, obtain anisetree bark
Crude extract, n-Butanol soluble is added in anisetree bark crude extract, be made into the sample introduction solution that mass concentration is 15%；
（3）Sample introduction solution is delivered into Simulation moving bed to be isolated and purified, the chromatographic column filling molecular sieve tree of the moving bed
Fat, eluant, eluent are that volume is 3:1 n-butanol and ethyl acetate mixed solvent, obtains eluent；It is described to utilize Simulation moving bed point
Control elution flow rate pump 60mL/min, pressure 6MPa, sample introduction flow rate pump 15mL/min, pressure 6MPa during from purifying, work temperature
45 DEG C of degree.
（4）By above-mentioned eluent vacuum be -0.06 Mpa, temperature be 60 DEG C and be concentrated under reduced pressure into paste, in vacuum
It is to be dried in vacuo at 55 DEG C to spend for -0.06 Mpa, temperature, that is, obtains anisetree bark active ingredient.
Anisetree bark active ingredient obtained by the present embodiment detects by HPLC, and wherein total saponin content is 31.72%, total yellow
Ketone content is 35.19%.
Embodiment 5
A kind of method for extracting anisetree bark active ingredient, comprises the following steps：
（1）Anisetree bark 5kg is crushed to 150 mesh, sieved, the ethanol for being incorporated as 8 times of anisetree bark medicinal material weight every time is flowed back
Extraction 2 times, refluxing extraction temperature are 60 DEG C, first time refluxing extraction 2.0h, second of refluxing extraction 1.5h, merging filtrate；
（2）By step（1）Filtrate vacuum be -0.08Mpa, temperature be 55 DEG C and be concentrated under reduced pressure into paste, obtain anisetree bark
Crude extract, n-Butanol soluble is added in anisetree bark crude extract, be made into the sample introduction solution that mass concentration is 12%；
（3）Sample introduction solution is delivered into Simulation moving bed to be isolated and purified, the chromatographic column filling molecular sieve tree of the moving bed
Fat, eluant, eluent are that volume is 3:1 n-butanol and ethyl acetate mixed solvent, obtains eluent；It is described to utilize Simulation moving bed point
Control elution flow rate pump 80mL/min, pressure 6MPa, sample introduction flow rate pump 10mL/min, pressure 6MPa during from purifying, work temperature
40 DEG C of degree.
（4）By above-mentioned eluent vacuum be -0.08Mpa, temperature be 60 DEG C and be concentrated under reduced pressure into paste, in vacuum
It is to be dried in vacuo at 60 DEG C for -0.06 Mpa, temperature, that is, obtains anisetree bark active ingredient.
Anisetree bark active ingredient obtained by the present embodiment detects by HPLC, and wherein total saponin content is 26.75%, total yellow
Ketone content is 39.41%.
Claims (6)
- A kind of 1. method for extracting anisetree bark active ingredient, it is characterised in that：Comprise the following steps：（1）Anisetree bark is crushed to 100-150 mesh, sieved, the ethanol for being incorporated as 5-8 times of anisetree bark medicinal material weight every time is returned Stream extraction 2-3 times, merging filtrate；（2）By step（1）Filtrate decompression concentration after, obtain anisetree bark crude extract, anisetree bark crude extract add n-Butanol soluble, It is made into the sample introduction solution that mass concentration is 10-20%；（3）Sample introduction solution is delivered into Simulation moving bed to be isolated and purified, the chromatographic column filling molecular sieve tree of the moving bed Fat, eluant, eluent are n-butanol and ethyl acetate mixed solvent, obtain eluent；（4）By above-mentioned eluent again by being concentrated under reduced pressure, it is dried in vacuo, that is, obtains anisetree bark active ingredient.
- 2. the method for anisetree bark active ingredient is extracted according to claim 1, it is characterised in that：Described refluxing extraction temperature For 50-60 DEG C, each refluxing extraction 1-2h.
- 3. the method for anisetree bark active ingredient is extracted according to claim 1, it is characterised in that：The vacuum being concentrated under reduced pressure It is 55-65 DEG C to spend for -0.06 ~ -0.08Mpa, temperature.
- 4. the method for anisetree bark active ingredient is extracted according to claim 1, it is characterised in that：N-butanol in the eluant, eluent Volume ratio with ethyl acetate is 2-4:1.
- 5. the method for anisetree bark active ingredient is extracted according to claim 1, it is characterised in that：The vacuum drying is vacuum It is to be dried at 50-60 DEG C to spend for -0.06 ~ -0.08Mpa, temperature.
- 6. the method for anisetree bark active ingredient is extracted according to claim 1, it is characterised in that：It is described to utilize Simulation moving bed Control elution flow rate pump 50-100mL/min, pressure 6-8MPa, sample introduction flow rate pump 10-20mL/min, pressure 6- when isolating and purifying 8MPa, 40-50 DEG C of operating temperature.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114047283A (en) * | 2022-01-11 | 2022-02-15 | 赛灵药业科技集团股份有限公司北京分公司 | TLC identification and HPLC detection method for schizophragma integrifolia in Henggu fracture healing agent |
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- 2017-09-22 CN CN201710863160.2A patent/CN107569535A/en active Pending
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| CN102002029A (en) * | 2010-11-06 | 2011-04-06 | 黑龙江八一农垦大学 | Method for separating and extracting isoflavone by simulated moving bed adsorption |
| CN104193793A (en) * | 2014-08-07 | 2014-12-10 | 中国农业科学院特产研究所 | Method for preparing ginsenoside Rb3 in American ginseng fruit by adopting simulated moving bed |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114047283A (en) * | 2022-01-11 | 2022-02-15 | 赛灵药业科技集团股份有限公司北京分公司 | TLC identification and HPLC detection method for schizophragma integrifolia in Henggu fracture healing agent |
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Application publication date: 20180112 |