CN110156764A - A method of extracting mangiferin - Google Patents
A method of extracting mangiferin Download PDFInfo
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- CN110156764A CN110156764A CN201910344794.6A CN201910344794A CN110156764A CN 110156764 A CN110156764 A CN 110156764A CN 201910344794 A CN201910344794 A CN 201910344794A CN 110156764 A CN110156764 A CN 110156764A
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- mangiferin
- mango
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- precipitating
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D407/00—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00
- C07D407/02—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00 containing two hetero rings
- C07D407/04—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00 containing two hetero rings directly linked by a ring-member-to-ring-member bond
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention discloses a kind of methods for extracting mangiferin, comprising the following steps: (1) just extracts: lime buck extracting solution is added in raw material after crushing, and stirring extracts 8~12h, filters to obtain crude extract；(2) acid solution cleans: acid solution tune pH5~6 are added in first extract, stand, before the precipitating that generates of 8h be filtered to remove, continuously add acid solution tune pH3~4, place 72~120h, worry takes precipitating；(3) refine: obtained precipitating is added its ethanol solution and carries out refluxing extraction, recycles ethyl alcohol, and mangiferin crystal is precipitated, is dried to obtain mangiferin finished product.The method of the present invention for extracting mangiferin, is extracted and is purified using lye and acid solution, does not use organic solvent, is cleaned without using resin, is belonged to environmentally friendly extracting method.This method simple process, equipment requirement is low, can be completed under normal temperature and pressure, lower production costs；Raw material sources are extensive, are advantageously implemented the higher value application of Mango Resources.
Description
Technical field
The present invention relates to medicine extractive technique field, specifically a kind of method for extracting mangiferin.
Background technique
Mangiferin (mangiferin) it is also known as mangiferin , Mango glucoside, mangiferin, it is primarily present in Anacardiaceae plant mango
(Mangifera indica L.) fruit, leaf, bark, liliaceae plant (Anemarrhena asphodeloides Bge.) rhizome, aerial part, irides blackberry lily [Belamcanda chinensis(L.) DC.] the plants such as flower, leaf
In.Its chemical structural formula are as follows:
Modern pharmacology and clinical research prove that mangiferin has various physiological activity and pharmacological action, and such as antitumor action resists
Lipid peroxidation, immunological regulation, anti-diabetic, anti-inflammatory, analgesic, antiviral, anti-radiation etc., at present both at home and abroad to mangiferin
Into many research, especially Colleges Of Traditional Chinese Medicine Of Guangxi for many years to extracting mangiferin from mango and almond and carried out a variety of medicines
The test of reason and pharmacodynamics, achieves many achievements.The pharmacological action of mangiferin is clear, and plant origin is extensive, at present clinically
It is mainly used in respiratory disease, due to its anticancer, antiviral and anti-diabetic isoreactivity, increasingly by people
Concern, with going deep into for research, mangiferin possesses good development prospect.
Mango (Mangifera indica L.) it is Anacardiaceae plant, it is one of famous tropical fruit (tree), also known as: Ma Meng,
It smears violent fruit, big fruit, hope fruit, honey hope, sweet shop sign in the form of a streamer, big fruit.In China, mango is distributed widely in Yunnan, Guangxi, Guangdong, Hainan etc.
Provinces and regions, resource very abundant.In Guangxi, mango cultivated area has just been more than 100,000 hectares, the quantity of mango leaf and myrica rubra leaf
Also very much, annual prune has up to ten million tons with leaf caused by defoliation of fruit trees.And in most cases, mango leaf is as discarded
Object is thrown aside, and the very big wasting of resources is caused, so mangiferin is extracted from mango leaf can rationally utilize resource,
Turn waste into wealth, there is good economic value and social effect.
The extraction of mangiferin is all extracted using organic solvent mostly in the prior art, or is carried out with organic resin
Absorption purification, or extracted using enzymatic isolation method, production cost is higher, and the use of organic solvent and resin can cause environment
Certain influence, while also will affect the quality of mango glycoside product.Such as following patent: 1, Chinese patent: extracting awns with mango leaf
The method of fruit glycosides；Application number: 201710570143.X；Applicant: Hunan Yuan Cao Bioisystech Co., Ltd；Abstract: Yi Zhongcong
The method that mangiferin is extracted in mango leaf, makes first pulverize by mango leaf, improves sporoderm-broken rate, then with edible ethanol
Mangiferin crude extract is extracted from mango leaf, and the mangiferin coarse extraction is combined D296 resin anion (R.A.) with D101 macroreticular resin
Isolate and purify with the big mangiferin of moral, can not only industrialized production safely and effectively different purity specification mango glucoside extract, and
And really realize the higher value application of safe and simple, reasonable, economic Mango Resources and the industrial metaplasia of series of products
It produces, fully demonstrates the theory of Green Chemistry production and the strategy of circular economy.2, a kind of Chinese patent: preparation side of mangiferin
Method；Application number: 201010292465.0；Applicant: Kunming Medicine Group Stock Co., Ltd；Abstract: the present invention relates to drugs
Chemical field discloses a kind of preparation method of mangiferin.The preparation method of mangiferin of the present invention be with mango fruit,
Mango leaf, mango bark and Asphodeloides Bge Rhizome are that the mixed solution of raw material alcohol and water extracts, filtering, filtrate concentration, gained concentration
Liquid is extracted with organic solvent, then aqueous phase extracted is taken to crystallize, and is recrystallized with the mixed solution of acetone and water to get mangiferin.This
The preparation method of the mangiferin is invented without using macroporous resin purification, resin pre-treatment, absorption and elution process is avoided, contracts
The short production cycle, the rate of transform is improved, and reduce the usage amount of organic solvent, saved production cost, reduced pair
The pollution of environment.The mangiferin prepared using the preparation method of mangiferin of the present invention is with high purity, not containing benezene organic solvent,
It is highly-safe.
Therefore, studying the low extraction process of a kind of environmental sound, simple process, production cost has good meaning.
Summary of the invention
The object of the present invention is to provide a kind of methods for extracting mangiferin, are extracted and are purified using lye and acid solution,
Without using organic solvent, cleans without using resin, belong to environmentally friendly extracting method.This method simple process, equipment are wanted
It asks low, can be completed under normal temperature and pressure, lower production costs；Raw material sources are extensive, are advantageously implemented the high-valued of Mango Resources
It utilizes.
The invention is realized by the following technical scheme:
A method of extracting mangiferin, comprising the following steps:
(1) it just extracts: taking fresh mango leaf, spray or immature mango, after being crushed with high speed disintegrator, it is heavy that its is added
The lime buck extracting solution of 2~5 times of amount, stirring extract 8~12h, are filtered to remove sediment, taking filtrate is first extract；
Fresh mango leaf, spray mangiferin rich in, it is in all parts of the country it is annual prune and defoliation of fruit trees caused by leaf
Son has up to ten million tons；Mango can also fall many small mango naturally before and after bearing fruit, most of these resources, which not can be carried out, fills
The utilization divided, causes great waste, and the present invention is used to extract the higher value application that mangiferin is advantageously implemented Mango Resources.
(2) acid solution cleans: acid solution tune pH5~6 are added in the first extract that step (1) obtains, stands and generates precipitating, before
The precipitating that 8h is generated is filtered to remove, and continuously adds acid solution tune pH3~4, places 72~120h, generates precipitating completely, it is heavy that worry takes
It forms sediment；
The sediment and liquid discarded in step (1) and step (2) can carry out waste utilization, be used to prepare mango special fertilizer material,
Not only waste pollution environment can be prevented, but also raw material can be made full use of, turns waste into wealth, economizes on resources, reduces production
Cost.
(3) refine: the ethyl alcohol that the volume fraction of 5~10 times of its weight is 45~65% is added in the precipitating that step (2) is obtained
Solution, refluxing extraction 1~2 time, 60~90min, recycles ethyl alcohol every time, and mangiferin crystal is precipitated, is dried to obtain mangiferin finished product.
The present invention carries out refluxing extraction using 45~65% ethanol solution, and the ethanol solution in this concentration range is to awns
Fruit glycosides has good dissolubility, can dissolve mangiferin to greatest extent, and remove the impurity of some non-prolamines.
Specifically, the immature mango refers to that mango core is the mango before forming stone, and growth duration does not surpass
Cross 2 months mango；It is enucleated before use.Mangiferin rich in immature mango pericarp, and mango is growing
The phenomenon that often having physiological fruit drop in the process, mango will fall off or extra as extract mangiferin raw material it
One, it both can be salvaged, economized on resources, and the raw material sources of mangiferin can be increased, and improved the recovery rate of mangiferin.
The lime buck extracting solution the preparation method comprises the following steps: take suitable water, quick lime and sodium hydrate solid is added,
The weight ratio of quick lime and sodium hydrate solid is 10:0.8~1.2, stirs to dissolve to saturation state, is then diluted with water
10~20 times, obtain lime buck extracting solution.Lime buck extracting solution prepared by the present invention belongs to compound lye, at room temperature
Its alkalinity is stronger, can dissolve the mangiferin and some impurity of the overwhelming majority, for just extract to raw material.Limewash can be with
Inhibit the dissolution such as colloid, albumen in mango leaf, but not strong to mangiferin solvability, and sodium hydroxide to mangiferin, colloid,
Albumen etc. all has very strong solvability, and the two cooperation is suitable for extracting mangiferin out.
The phosphoric acid that the acid solution is the sulfuric acid solution that mass fraction is 5~20% or mass fraction is 10~15% is molten
Liquid or two kinds of acid solutions are compounded in accordance with the appropriate ratio.Acid solution is added in the present invention to clean, predominantly removes wherein
Calcium ion, sulfate radical or phosphate radical in calcium ion and acid solution generate and precipitate, and the time of fully reacting is usually no more than 8
Hour, so the liquid of front 8h discards, it can substantially all removing calcium ion.Through inventor's the study found that 5~20%
Sulfuric acid solution or mass fraction be 10~15% phosphoric acid solution it is best for the effect for removing calcium ion, and not will cause
The residual of excessive sulfate radical or phosphate radical.
Mangiferin (mangiferin), Chinese nickname: mangiferin , Mango glucoside, mangiferin, molecular formula: C16H12O4；CAS
Number: 4773-96-0.Property: 267~272 DEG C of fusing point (decomposition).+ 43.3 ° of optical activity (c=0.9, pyridine), is slightly soluble in methanol, second
Alcohol, water dissolve in hot dilute methanol, hot Diluted Alcohol, do not dissolve in nonpolar solvent.There is preferable treatment for treating chronic bronchitis
Effect is the principle active component of Swertia mussotii treatment hepatitis, is active constituent antiviral in Asphodeloides Bge Rhizome.Mangiferin, which has, to be inhibited
Central nervous system, anti-inflammatory, antibacterial, anti-herpes simplex virus HSV-2, cholagogue and immunization, caused by alleviating HSV-2 virus
Sacrum nerve root disease: buttocks or thigh pain or cacesthesia, the retention of urine are shown as, there are also rectitis, urethritis with disease for it
Syndrome etc..The risk that cervical carcinoma occurs for HSV-2 virus women is 5~10 times bigger than general female.It is acute to simulated high altitude low
Oxygen hepatic injury has protective effect.
The method that the present invention extracts mangiferin, being counted its yield is 0.5~1.0%, and the purity of mangiferin is through height in finished product
Effect liquid phase chromatogram method is measured as 92~95%.Wherein, yield is that final product quality accounts for the percentage of fresh feed weight, purity be at
Mass percent shared by mangiferin in product mangiferin.
Beneficial effects of the present invention:
1, the method for the present invention for extracting mangiferin, is extracted and is purified using lye and acid solution, without using organic molten
Agent cleans without using resin, belongs to environmentally friendly extracting method.
2, the method for the present invention for extracting mangiferin, raw material sources are extensive, and simple process, equipment requirement is low, room temperature
It can be completed under normal pressure, liquid waste produced during the preparation process and sediment can be used for preparing mango special fertilizer material, both can be with
Waste pollution environment is prevented, and raw material can be made full use of, turns waste into wealth, economizes on resources, reduces production cost.
3, the method for the present invention for extracting mangiferin is made with mango leaf, spray or the immature mango fallen
It extracts for raw material, both can be salvaged, economize on resources, and the raw material sources of mangiferin can be increased, improve mangiferin
Recovery rate, be advantageously implemented the higher value application of Mango Resources, may advantageously facilitate the development of Guangxi mango industry.
Specific embodiment
In order to keep technical solution of the present invention and advantage clearer, below with reference to the embodiment of the present invention, to the present invention
Technical solution be clearly and completely described.
Embodiment 1
(1) it just extracts: taking fresh mango leaf, spray or immature mango, after being crushed with high speed disintegrator, it is heavy that its is added
The lime buck extracting solution of 3 times of amount, stirring extract 10h, are filtered to remove sediment, taking filtrate is first extract；
The lime buck extracting solution the preparation method comprises the following steps: take suitable water, quick lime and sodium hydrate solid, raw stone is added
The weight ratio of ash and sodium hydrate solid is 10:1, stirs to dissolve to saturation state, is then diluted with water 10 times, obtains stone
Grey buck extracting solution.
The immature mango refers to that mango core is the mango before forming stone, and growth duration is no more than 2 months
Mango；It is enucleated before use.
(2) acid solution clean: in the first extract that step (1) obtains be added acid solution tune pH5, stand generate precipitating, before 8h
The precipitating of generation is filtered to remove, and continuously adds acid solution tune pH3.4, places 80h, generates precipitating completely, worry takes precipitating；
The phosphoric acid solution that the acid solution is the sulfuric acid solution that mass fraction is 5% and person's mass fraction is 10% is according to volume ratio 2:
1 is compounded.
(3) refine: the ethanol solution that the volume fraction of 8 times of its weight is 65% is added in the precipitating that step (2) is obtained, and returns
Stream extracts 2 times, each 60min, recycles ethyl alcohol, and mangiferin crystal is precipitated, is dried to obtain mangiferin finished product.
Embodiment 2
(1) it just extracts: taking fresh mango leaf and spray, after being crushed with high speed disintegrator, the lime alkali of 2 times of its weight is added
Aqueous extract, stirring extract 12h, are filtered to remove sediment, taking filtrate is first extract；
The lime buck extracting solution the preparation method comprises the following steps: take suitable water, quick lime and sodium hydrate solid, raw stone is added
The weight ratio of ash and sodium hydrate solid is 10:1.2, stirs to dissolve to saturation state, is then diluted with water 20 times, obtains
To lime buck extracting solution.
The immature mango refers to that mango core is the mango before forming stone, and growth duration is no more than 2 months
Mango；It is enucleated before use.
(2) acid solution clean: in the first extract that step (1) obtains be added acid solution tune pH6, stand generate precipitating, before 8h
The precipitating of generation is filtered to remove, and continuously adds acid solution tune pH4, places 120h, generates precipitating completely, worry takes precipitating；
The acid solution is the phosphoric acid solution that mass fraction is 15%.
(3) refine: the ethanol solution that the volume fraction of 10 times of its weight is 45% is added in the precipitating that step (2) is obtained, and returns
Stream extracts 2 times, each 90min, recycles ethyl alcohol, and mangiferin crystal is precipitated, is dried to obtain mangiferin finished product.
Embodiment 3
(1) it just extracts: taking fresh mango leaf, spray or immature mango, after being crushed with high speed disintegrator, it is heavy that its is added
The lime buck extracting solution of 5 times of amount, stirring extract 8h, are filtered to remove sediment, taking filtrate is first extract；
The lime buck extracting solution the preparation method comprises the following steps: take suitable water, quick lime and sodium hydrate solid, raw stone is added
The weight ratio of ash and sodium hydrate solid is 10:0.8, stirs to dissolve to saturation state, is then diluted with water 15 times, obtains
Lime buck extracting solution.
The immature mango refers to that mango core is the mango before forming stone, and growth duration is no more than 2 months
Mango；It is enucleated before use.
(2) acid solution cleans: acid solution tune pH5.5 is added in the first extract that step (1) obtains, stands and generates precipitating, before
The precipitating that 8h is generated is filtered to remove, and continuously adds acid solution tune pH3, places 72h, generates precipitating completely, worry takes precipitating；
The acid solution is the sulfuric acid solution that mass fraction is 20%.
(3) it refines: the soak that step (2) obtains is filtered, take filter residue, 5 times of filter residue weight of volume point is added
The ethanol solution that number is 65% refluxing extraction 1 time, time 90min, recycles ethyl alcohol, mangiferin crystal is precipitated, is dried to obtain awns
Fruit glycosides finished product.
Embodiment 4
(1) it just extracts: taking fresh mango leaf, spray or immature mango, after being crushed with high speed disintegrator, it is heavy that its is added
The lime buck extracting solution of 5 times of amount, stirring extract 12h, are filtered to remove sediment, taking filtrate is first extract；
The lime buck extracting solution the preparation method comprises the following steps: take suitable water, quick lime and sodium hydrate solid, raw stone is added
The weight ratio of ash and sodium hydrate solid is 10:1, stirs to dissolve to saturation state, is then diluted with water 10 times, obtains stone
Grey buck extracting solution.
The immature mango refers to that mango core is the mango before forming stone, and growth duration is no more than 2 months
Mango；It is enucleated before use.
(2) acid solution cleans: acid solution tune pH5.4 is added in the first extract that step (1) obtains, stands and generates precipitating, before
The precipitating that 8h is generated is filtered to remove, and continuously adds acid solution tune pH3.6, places 100h, generates precipitating completely, worry takes precipitating；
The phosphoric acid solution that the acid solution is the sulfuric acid solution that mass fraction is 10% and mass fraction is 15% is according to volume ratio 1:1
It is compounded.
(3) refine: the ethanol solution that the volume fraction of 8 times of its weight is 55% is added in the precipitating that step (2) is obtained, and returns
Stream extracts 2 times, each 80min, recycles ethyl alcohol, and mangiferin crystal is precipitated, is dried to obtain mangiferin finished product.
According to the extracting method of Examples 1 to 4, the finished product mangiferin extracted is detected, testing result is such as
Under:
As seen from the above table, it is relatively high that mangiferin yield is extracted in the embodiment of the present invention, the mangiferin in 0.70% or more, finished product
Purity also reached 93.7~95%.
Claims (4)
1. a kind of method for extracting mangiferin, which comprises the following steps:
(1) it just extracts: taking fresh mango leaf, spray or immature mango, the stone of 2~5 times of its weight is added after crushing
Grey buck extracting solution, stirring extract 8~12h, are filtered to remove sediment, taking filtrate is first extract；
(2) acid solution clean: in the first extract that step (1) obtains be added acid solution tune pH5~6, stand generate precipitating, before 8h produce
Raw precipitating is filtered to remove, and continuously adds acid solution tune pH3~4, places 72~120h, generates precipitating completely, worry takes precipitating；
(3) refine: it is molten that the ethyl alcohol that the volume fraction of 5~10 times of its weight is 45~65% is added in the precipitating that step (2) is obtained
Liquid, refluxing extraction 1~2 time, 60~90min, recycles ethyl alcohol every time, and mangiferin crystal is precipitated, is dried to obtain mangiferin finished product.
2. extracting the method for mangiferin according to claim 1, it is characterised in that: the immature mango refers to mango core
To form the mango before stone, growth duration is no more than 2 months mango；It is enucleated before use.
3. extracting the method for mangiferin according to claim 1, it is characterised in that: the preparation of the lime buck extracting solution
Method are as follows: take suitable water, be added quick lime and sodium hydrate solid, the weight ratio of quick lime and sodium hydrate solid is 10:
0.8~1.2, it stirs to dissolve to saturation state, is then diluted with water 10~20 times, obtain lime buck extracting solution.
4. extracting the method for mangiferin according to claim 1, it is characterised in that: the acid solution be mass fraction be 5~
Perhaps mass fraction is 10~15% phosphoric acid solution or the compounding of two kinds of acid solutions to 20% sulfuric acid solution.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4518592A (en) * | 1980-07-16 | 1985-05-21 | Rusakova Svetlana V | Process for preparing mangiferin |
| CN101973985A (en) * | 2010-11-15 | 2011-02-16 | 广西中医学院 | Method for preparing mangiferin |
| CN101993437A (en) * | 2009-08-27 | 2011-03-30 | 上海新康制药厂 | Method for extracting mangiferin from mango leaf |
-
2019
- 2019-04-26 CN CN201910344794.6A patent/CN110156764B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4518592A (en) * | 1980-07-16 | 1985-05-21 | Rusakova Svetlana V | Process for preparing mangiferin |
| CN101993437A (en) * | 2009-08-27 | 2011-03-30 | 上海新康制药厂 | Method for extracting mangiferin from mango leaf |
| CN101973985A (en) * | 2010-11-15 | 2011-02-16 | 广西中医学院 | Method for preparing mangiferin |
Non-Patent Citations (1)
| Title |
|---|
| 李学坚，等: "采用水基溶剂提取芒果苷的工艺研究", 《中成药》 * |
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