CN107011158A - A kind of method of extraction purification forulic acid in cauline leaf from Ligusticum wallichii - Google Patents
A kind of method of extraction purification forulic acid in cauline leaf from Ligusticum wallichii Download PDFInfo
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- CN107011158A CN107011158A CN201710220313.1A CN201710220313A CN107011158A CN 107011158 A CN107011158 A CN 107011158A CN 201710220313 A CN201710220313 A CN 201710220313A CN 107011158 A CN107011158 A CN 107011158A
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- ligusticum wallichii
- cauline leaf
- ethanol
- forulic acid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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Abstract
The invention discloses a kind of method of extraction purification forulic acid in cauline leaf from Ligusticum wallichii, the extraction cost for solving forulic acid in the prior art is high, the problem of resource can not be utilized effectively.The present invention comprises the following steps：Ligusticum wallichii cauline leaf is gathered in, is cut into pieces；Alkaline ethanol solution is added, is extracted, filtrate is collected in filtering；Filtrate recycling ethanol, concentration, regulation pH value to acidity, filtering, residue washing to neutrality；Filter residue adds ethanol to dissolve, centrifugation, and macroporous absorbent resin absorption will be added in supernatant, then uses water, 40%, 60%, 90% ethanol water to elute successively, collects 90% ethanol eluate；After 90% ethanol eluate concentration, add macroporous absorbent resin and carry out after second adsorption, then carry out secondary elution with water, 40%, 60%, 90% ethanol water successively, collect the 90% secondary eluent of ethanol, volatilize solvent, low temperature drying is produced.
Description
Technical field
The invention belongs to technical field of extraction of Chinese traditional medicine, and in particular to the side of extraction purification forulic acid in a kind of cauline leaf from Ligusticum wallichii
Method.
Background technology
Ligusticum wallichii is conventional Chinese medicine simply, and tradition is samphire Ligusticum wallichii Ligusticum chuanxiong with Ligusticum wallichii
Hort. dry rhizome.Summer significantly protrudes when the section disk on stem, and is excavated during purplish, removes silt, is dried after solarization,
Fibrous root is removed again.
Ligusticum wallichii is pungent, temperature；Return liver, courage, pericardium channel.With blood-activating and qi-promoting, wind-expelling pain-stopping function, for chest impediment and cardialgia, chest
Coerce shouting pain, tumbling and swelling, irregular menstruation, closed dysmenorrhea , Disorder lump in the abdomen is suffered from abdominal pain, headache, arthralgia pain due to rheumatism.
Ligusticum wallichii is mainly cultivated plant, and main product is in Sichuan Dujiang weir, and Pengzhou is equal in Yunnan, Guizhou, Guangxi and had a moderate climate
Environment in also have plantation.Modern study shows that Ligusticum wallichii contains a variety of chemical compositions with bioactivity.Such as forulic acid
(ferulic acid), forulic acid (chuanxiongzine), Ligustilide (ligustilide), Ligusticum wallichii naphthalene furan lactone
(wallichilide), protocatechuic acid (protocatechuic acid) etc..Wherein forulic acid (sodium ferulate) has anti-blood small
Plate is assembled, and suppresses platelet 5-HT release, suppresses platelet thrombus element a2 (txa2) generation, and enhancing prostaglandin is lived
Property, the effect such as vasopasm is alleviated in analgesia.It is the base that production is used to treat the disease medicine such as cardiovascular and cerebrovascular disease and Neuroleptic Leukocytopenia
This raw material.Such as Sodium Ferulate, Limai capsule, Ferulic acid, it can play vigorous and graceful and protection skin in human body simultaneously
Effect.
Conventional method obtains forulic acid from Ligusticum wallichii and extracted from Ligusticum wallichii dry rhizome.But recently as people
Health care consciousness enhancing, the favor to traditional Chinese medicine, the consumption of Chinese medicine rises violently, and the price of Ligusticum wallichii is high all the way.Planted from Ligusticum wallichii
The production cost that forulic acid is extracted in thing rhizome also remains high.On the other hand, Ligusticum wallichii only utilizes its rhizome, and other positions are discarded
Fall very unfortunate.
Therefore a kind of extracting method of forulic acid is provided, reduction production cost is low, utilizes Ligusticum wallichii resource Comprehensive, into
For those skilled in the art's urgent problem to be solved.
The content of the invention
The technical problem to be solved in the present invention is：A kind of method of extraction purification forulic acid during cauline leaf from Ligusticum wallichii is provided, solution
Certainly the extraction cost of forulic acid is high in the prior art, the problem of resource can not be utilized effectively.
To achieve the above object, the technical solution adopted by the present invention is as follows：
The method of extraction purification forulic acid, comprises the following steps in a kind of cauline leaf from Ligusticum wallichii of the present invention：
A：Ligusticum wallichii cauline leaf is gathered in, is cut into pieces；
B：Cauline leaf after cutting is added into alkaline ethanol solution, extracted, filtrate is collected in filtering；
C：Filtrate recycling ethanol, concentration obtains concentrate, adjusts the pH value of the concentrate to acidity, filters, filter residue water
Wash to neutrality；
D：Add ethanol to dissolve the washing to neutral filter residue, centrifuge, take supernatant, it is big by being added in the supernatant
Macroporous adsorbent resin is adsorbed, then successively with water, the elution of 40%, 60%, 90% ethanol water, the ethanol elution of collection 90%
Liquid；
E：After described 90% ethanol eluate concentration, add macroporous absorbent resin and carry out after second adsorption, then successively
Secondary elution is carried out with water, 40%, 60%, 90% ethanol water, the 90% secondary eluent of ethanol is collected；
F：The secondary eluent of 90% ethanol is volatilized into solvent, low temperature drying is produced.
Further, the alkaline ethanol solution in the step B is PH8-10 50-70% ethanol solution.
Further, the alkaline ethanol solution in the step B is PH8 70% ethanol solution.
Further, the alkaline ethanol solution addition is calculated as 3-5ml with every gram of Ligusticum wallichii cauline leaf.
Further, the extraction temperature in the step B is room temperature, and extraction time is 48-96 hours.
Further, the pH value of the C regulations filtrate is less than 5.
Further, the pH value of the C regulations filtrate is 3-4.
Further, in the step D macroporous absorbent resin model D101 types, its consumption is by every gram of Ligusticum wallichii cauline leaf
Meter, is 0.05-0.1g.
Further, in the step D water, the consumption of 40%, 60%, 90% ethanol solution presses every gram of Ligusticum wallichii cauline leaf
1-2ml is calculated as, the elution speed is calculated as 0.06-0.08ml/h by every gram of Ligusticum wallichii cauline leaf.
Further, in the step E macroporous absorbent resin model D101 types, its consumption is by every gram of Ligusticum wallichii cauline leaf
Meter, is 0.005-0.01g, and the water of the secondary elution, the consumption of 40%, 60%, 90% ethanol solution are by every gram of Ligusticum wallichii stem
Leaf is calculated as 0.1-0.2ml, and the elution speed is calculated as 0.06-0.08ml/h by every gram of Ligusticum wallichii cauline leaf.
Compared with prior art, the invention has the advantages that：
(1) present invention process is simple, easy to operate, and forulic acid is extracted by raw material of Ligusticum wallichii cauline leaf, will be given up in traditional approach
The cauline leaf discarded realizes the comprehensive utilization of Ligusticum wallichii resource, has effectively dropped low production cost as raw material.
(2) invention is extracted the forulic acid in Ligusticum wallichii cauline leaf using alkaline ethanol, then extract solution is dense
It is acidified after contracting, forulic acid is precipitated out from concentrate, then the forulic acid after precipitation is dissolved in ethanol is used macropore
Resin adsorption, it is then by the way of the ethanol gradient elution of various concentrations that forulic acid is pure in other impurities progress initial gross separation
After change, adsorbing separation is carried out using macroreticular resin again, the complete extraction of forulic acid is realized and efficiently separates.
(4) present invention is not high to equipment requirement, and production cost is low, environmentally friendly, is worthy of popularization.
Embodiment
With reference to specific embodiment, the invention will be further described, and mode of the invention includes but are not limited to following
Embodiment.
Embodiment 1
The method that forulic acid is extracted from Ligusticum wallichii cauline leaf, comprises the following steps：
A：Ligusticum wallichii cauline leaf is gathered in, 1-2cm section is cut into；
B：Cauline leaf 5000g after cutting is added to PH8 70% ethanol solution 15L, normal temperature extraction time is 48 hours, mistake
Filter, collects filtrate；
C：Filtrate recycling ethanol, concentration obtains concentrate, and the pH value for adjusting the concentrate is 3-4, filtering, filter residue water
Wash to neutrality；
D：Add ethanol to dissolve the washing to neutral filter residue, centrifuge, take supernatant, will be added in the supernatant
D101 macroporous absorbent resins 250g is adsorbed, then washed successively with water, 40%, 60%, 90% ethanol water 5000-10000ml
De-, elution rate is 300-400ml/h, collects 90% ethanol eluate；
E：After described 90% ethanol eluate concentration, add D101 macroporous absorbent resins 25g and carry out after second adsorption,
Secondary elution is carried out with water, 40%, 60%, 90% ethanol water 500-1000ml successively again, elution rate is 300-
400ml/h, the secondary eluent of ethanol of collection 90%；
F：The secondary eluent of 90% ethanol is volatilized into solvent, 40 DEG C of low temperature dryings are produced.
Forulic acid 0.458g obtained by the present embodiment, purity is 94%.
Embodiment 2
The method that forulic acid is extracted from Ligusticum wallichii cauline leaf, comprises the following steps：
A：Ligusticum wallichii cauline leaf is gathered in, 1-2cm section is cut into；
B：Cauline leaf 5000g after cutting is added to PH10 70% ethanol solution 25L, normal temperature extraction time is 96 hours,
Filtering, collects filtrate；
C：Filtrate recycling ethanol, concentration obtains concentrate, and the pH value for adjusting the concentrate is 3, and filtering, filter residue is washed with water
Wash to neutrality；
D：Add ethanol to dissolve the washing to neutral filter residue, centrifuge, take supernatant, will be added in the supernatant
D101 macroporous absorbent resins 500g is adsorbed, then is washed successively with water, 40%, 60%, 90% ethanol water 10000ml elutions
De- speed is 400ml/h, collects 90% ethanol eluate；
E：After described 90% ethanol eluate concentration, add D101 macroporous absorbent resins 50g and carry out after second adsorption,
Secondary elution is carried out with water, 40%, 60%, 90% ethanol water 500-1000ml successively again, elution rate is 300-
400ml/h, the secondary eluent of ethanol of collection 90%；
F：The secondary eluent of 90% ethanol is volatilized into solvent, 50 DEG C of low temperature dryings are produced.
Forulic acid 0.464g obtained by the present embodiment, purity is 96%.
Embodiment 3
The method that forulic acid is extracted from Ligusticum wallichii cauline leaf, comprises the following steps：
A：Ligusticum wallichii cauline leaf is gathered in, 1-2cm section is cut into；
B：Cauline leaf 5000g after cutting is added to PH8 70% ethanol solution 20L, normal temperature extraction time is 60 hours, mistake
Filter, collects filtrate；
C：Filtrate recycling ethanol, concentration obtains concentrate, and the pH value for adjusting the concentrate is 4.5, filtering, filter residue water
Wash to neutrality；
D：Add ethanol to dissolve the washing to neutral filter residue, centrifuge, take supernatant, will be added in the supernatant
D101 macroporous absorbent resins 400g is adsorbed, then successively with water, 40%, 60%, 90% ethanol water 800ml elutions, elution
Speed is 350ml/h, collects 90% ethanol eluate；
E：After described 90% ethanol eluate concentration, add D101 macroporous absorbent resins 40g and carry out after second adsorption,
Secondary elution is carried out with water, 40%, 60%, 90% ethanol water 600ml successively again, elution rate is 300ml/h, collected
The 90% secondary eluent of ethanol；
F：The secondary eluent of 90% ethanol is volatilized into solvent, 40 DEG C of low temperature dryings are produced.
Forulic acid 0.429g obtained by the present embodiment, purity is 92%.
Embodiment 4
The method that forulic acid is extracted from Ligusticum wallichii cauline leaf, comprises the following steps：
A：Ligusticum wallichii cauline leaf is gathered in, is cut into pieces；
B：Cauline leaf 5000g after cutting is added to PH9 60% ethanol solution 19L, normal temperature extraction time is 72 hours, mistake
Filter, collects filtrate；
C：Filtrate recycling ethanol, concentration obtains concentrate, and the pH value for adjusting the concentrate is 3.5, filtering, filter residue water
Wash to neutrality；
D：Add ethanol to dissolve the washing to neutral filter residue, centrifuge, take supernatant, will be added in the supernatant
D101 macroporous absorbent resins 500g is adsorbed, then successively with water, 40%, 60%, 90% ethanol water 9000ml elutions, elution
Speed is 350ml/h, collects 90% ethanol eluate；
E：After described 90% ethanol eluate concentration, add D101 macroporous absorbent resins 50g and carry out after second adsorption,
Secondary elution is carried out with water, 40%, 60%, 90% ethanol water 8000ml successively again, elution rate is 350ml/h, received
The secondary eluent of ethanol of collection 90%；
F：The secondary eluent of 90% ethanol is volatilized into solvent, 40 DEG C of low temperature dryings are produced.
Forulic acid 0.422g obtained by the present embodiment, purity is 98%.
Above-described embodiment is only one of the preferred embodiment of the present invention, should not be taken to limit the protection model of the present invention
Enclose, as long as the present invention body design thought and mentally make have no the change of essential meaning or polishing, it is solved
Technical problem it is still consistent with the present invention, should be included in protection scope of the present invention within.
Claims (10)
1. a kind of method of extraction purification forulic acid in cauline leaf from Ligusticum wallichii, it is characterised in that：Comprise the following steps：
A：Ligusticum wallichii cauline leaf is gathered in, is cut into pieces；
B：Cauline leaf after cutting is added into alkaline ethanol solution, extracted, filtrate is collected in filtering；
C：Filtrate recycling ethanol, concentration obtains concentrate, adjusts the pH value of the concentrate to acidity, filtering, filter residue is washed with water
To neutrality；
D：Add ethanol to dissolve the washing to neutral filter residue, centrifuge, take supernatant, inhaled macropore is added in the supernatant
Attached resin adsorption, then successively with water, the elution of 40%, 60%, 90% ethanol water, the ethanol eluate of collection 90%；
E：By described 90% ethanol eluate concentration after, add macroporous absorbent resin carry out second adsorption after, then successively with water,
40%th, 60%, 90% ethanol water carries out secondary elution, collects the 90% secondary eluent of ethanol；
F：The secondary eluent of 90% ethanol is volatilized into solvent, low temperature drying is produced.
2. the method for extraction purification forulic acid in a kind of cauline leaf from Ligusticum wallichii according to claim 1, it is characterised in that：It is described
50-70% ethanol solution that alkaline ethanol solution in step B is PH8-10.
3. the method for extraction purification forulic acid in a kind of cauline leaf from Ligusticum wallichii according to claim 2, it is characterised in that：It is described
70% ethanol solution that alkaline ethanol solution in step B is PH8.
4. the method for extraction purification forulic acid in a kind of cauline leaf from Ligusticum wallichii according to claim 3, it is characterised in that：It is described
Alkaline ethanol solution addition is calculated as 3-5ml with every gram of Ligusticum wallichii cauline leaf.
5. the method for extraction purification forulic acid in a kind of cauline leaf from Ligusticum wallichii according to claim 4, it is characterised in that：It is described
Extraction temperature in step B is room temperature, and extraction time is 48-96 hours.
6. the method for extraction purification forulic acid in a kind of cauline leaf from Ligusticum wallichii according to claim 5, it is characterised in that：It is described
The pH value of C regulation filtrates is less than 5.
7. the method for extraction purification forulic acid in a kind of cauline leaf from Ligusticum wallichii according to claim 6, it is characterised in that：It is described
The pH value of C regulation filtrates is 3-4.
8. the method for extraction purification forulic acid in a kind of cauline leaf from Ligusticum wallichii according to claim 7, it is characterised in that：It is described
The model D101 types of macroporous absorbent resin in step D, its consumption is 0.05-0.1g based on every gram of Ligusticum wallichii cauline leaf.
9. the method for extraction purification forulic acid in a kind of cauline leaf from Ligusticum wallichii according to claim 8, it is characterised in that：It is described
The consumption of water, 40%, 60%, 90% ethanol solution in step D is calculated as 1-2ml, the elution speed by every gram of Ligusticum wallichii cauline leaf
Degree is calculated as 0.06-0.08ml/h by every gram of Ligusticum wallichii cauline leaf.
10. the method for extraction purification forulic acid in a kind of cauline leaf from Ligusticum wallichii according to claim 9, it is characterised in that：Institute
The model D101 types of macroporous absorbent resin in step E are stated, its consumption is 0.005-0.01g based on every gram of Ligusticum wallichii cauline leaf, institute
State the water of secondary elution, the consumption of 40%, 60%, 90% ethanol solution and be calculated as 0.1-0.2ml by every gram of Ligusticum wallichii cauline leaf, institute
State elution speed and be calculated as 0.06-0.08ml/h by every gram of Ligusticum wallichii cauline leaf.
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Cited By (2)
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| CN109422806A (en) * | 2017-09-04 | 2019-03-05 | 四川协力制药有限公司 | A kind of preparation method of corticotropin(ACTH) |
| CN114989006A (en) * | 2022-06-23 | 2022-09-02 | 安徽雷允上药业有限公司 | Method for separating ferulic acid from volatile oil of ligusticum wallichii and angelica sinensis |
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| CN109422806A (en) * | 2017-09-04 | 2019-03-05 | 四川协力制药有限公司 | A kind of preparation method of corticotropin(ACTH) |
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| CN114989006A (en) * | 2022-06-23 | 2022-09-02 | 安徽雷允上药业有限公司 | Method for separating ferulic acid from volatile oil of ligusticum wallichii and angelica sinensis |
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