CN1844133A - Process for preparing high purity mangiferin - Google Patents
Process for preparing high purity mangiferin Download PDFInfo
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- CN1844133A CN1844133A CN 200610079234 CN200610079234A CN1844133A CN 1844133 A CN1844133 A CN 1844133A CN 200610079234 CN200610079234 CN 200610079234 CN 200610079234 A CN200610079234 A CN 200610079234A CN 1844133 A CN1844133 A CN 1844133A
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Abstract
The invention relates to a process for preparing high purity mango glycosides by using mango leaf or amygdale leaf as the raw material through resin method decolorization. The extracted mango glycosides has a purity higher than 90%.
Description
Technical field
The present invention relates to a kind of method for preparing the Mangiferin of purity 〉=90%, technology comprises several critical processes such as alcohol extracting, macroporous resin decolour, make with extra care.
Background technology
Mango and almond are delicious flavour, nutritious tropical fruit, and along with the generally raising of people's life, the plantation area is more and more.Especially mango, two during the last ten years, and provinces and regions such as the Guangxi of China, Guangdong, Hainan, Yunnan are constantly introduced and are cultivated new variety, make China become mango big producing country.The mango cultivated area in Guangxi just surpasses 100,000 hectares, 50,000 hectares of almond cultivated areas, so the quantity of Folium mangiferae and almond leaf is also a lot, annual pruning and fruit tree are eliminated the leaf that is produced up to ten million tons.The orchard worker generally was they to be used as firewood burn or let alone and rot in the orchard to the processing of Folium mangiferae and almond leaf in the past, had caused the significant wastage of resource.Folium mangiferae is close with almond leaf nature and flavor, is the Chinese medicinal materials that pharmaceutical value is arranged very much; The chemical ingredients aspect all contains compositions such as Mangiferin, Isomangiferin, homomangiferin.According to relevant bibliographical information, Folium mangiferae nature and flavor acid, sweet, cool, flat, having promoting the circulation of qi dredges stagnant, go that acute diseases such as cholera and sunstroke is long-pending, clearing heat and detoxicating, swelling and pain relieving, move back wet function, be used for cat fever, diseases such as swelling and pain in the throat, rheumatism, effect such as that the Mangiferin that extracts has is antibiotic, antiviral, eliminate the phlegm, antibechic from Folium mangiferae and almond leaf." Fujian Chinese materia medica " 2001, " thin-layer chromatography of compound Folium mangiferae and the antibacterial tests " of 32 (2) publications mentioned, mango leaf extract is carried out the in-vitro antibacterial experiment, the result shows that Folium mangiferae all has strong anti-microbial effect to golden Portugal 25023 bacterium, the anti-bacterium in capital, golden Portugal, white Portugal coccus, Nai Shi coccus, Pseudomonas aeruginosa, intestinal bacteria, Fu Shi bacillus, Corynebacterium diphtheriae.The surplus victory people of Guangxi Nationality Medical ﹠ Parmaceutical Research Inst., Zhong Ming are in " Chinese Chinese materia medica science and technology " 1999,6 (3) " the Mangiferin pharmacological research progress " delivered have been summarized some medical mechanisms of Mangiferin, pointed out that Mangiferin (mangiferin) is a kind of carbon glycoside of tetrahydroxy pyrrone, belong to two benzene pyrrones compounds, modern pharmacology and clinical study show that Mangiferin has many-sided physiologically active and pharmacological action.
Because Mangiferin has multiple biological activity, so Folium mangiferae and almond leaf are used widely at pharmaceutical industry.Colleges Of Traditional Chinese Medicine Of Guangxi and Pharmaceutical Factory of Guangxi Traditional Chinese Medicine College utilize the unit of Folium mangiferae for raw material development tcm product at first and for a long time.The MANGGUO ZHIKE PIAN that Pharmaceutical Factory of Guangxi Traditional Chinese Medicine College produces, containing mango leaf extract, Toldrin, Sodium Houttuyfonate (synthetic product), is the Chinese-western medicine compound preparation, has and ventilatings the lung and resolving phlegm, relieving cough and asthma effect is mainly used in diseases such as cough, asthma, many phlegm.The open source literature that extracts Mangiferin at present from Folium mangiferae and almond leaf also has, 03128247.4[apply for (patent right) people as Chinese patent [title] mango general glycoside preparation and production method thereof [application (patent) number]] the western end of the bridge in county town, Tiandong Natural Plant Products Factory [address] Tiandong County, Guangxi Zhuang Autonomous Region [summary] the invention provides a kind of Chinese medicine preparation with cough-suppressing phlegm-dispelling functions, and the composition that plays the cough-relieving phlegm-dispelling functions in the said preparation extracts from Folium mangiferae or almond leaf, the mixture of various glycoside compounds.The main component of this glucoside mixture is a Mengiferin, because of the extraction process difference may contain a spot of isomangiferin, homomangiferin, new Mengiferin and gallic acid; The content summation of various glucosides reaches more than 50%.Invention does not add or adds proper quantity of medicinal auxiliary material based on this glucoside mixture, is prepared into preparation or the formulation that oral administration is used by common pharmaceutical technology.The experimental result of invention shows, is the Chinese medicine preparation that raw material is made with this glucoside mixture, uses on one's body at animal model and patient, and the result shows good cough-relieving apophlegmatic effect.Chinese patent [title] Rhizoma Anemarrhenae extract and its production and use [application (patent) number] 03115509.X[summary] the present invention relates to medical technical field, be Rhizoma Anemarrhenae extract and preparation method thereof and Rhizoma Anemarrhenae extract is used to prepare the purposes of preventing and treating diabetes medicament.Rhizoma ane marrhenae is carried with aqueous ethanol heat or cold soaking gets extracting solution, adopted macroporous adsorbent resin to separate, refining Rhizoma Anemarrhenae extract.The main active ingredient of Rhizoma Anemarrhenae extract is Mangiferin and Neomangiferin, and the two total content is up to more than 50%, and Mangiferin is 1: 1～5: 1 with the content ratio of Neomangiferin.Through animal experiment, can effectively prevent and treat diabetes, so Rhizoma Anemarrhenae extract can be used for preparing the medicine of preventing and treating diabetes.Chinese patent [title] Folium mangiferae total glycosides cough relief traditional Chinese medicine preparation and production method thereof [application (patent) number] 03125270.2[applies for (patent right) people] Pharmaceutical Factory of Guangxi Traditional Chinese Medicine College [address] 530023 Dongge Road,, Nanning City, Guangxi Zhuang Autonomous Region No. 60 [summaries] the present invention relates to a kind of cough-relieving that has, reduce phlegm, relieving asthma, the Chinese medicine preparation of anti-inflammatory action, be that raw material extracts Chinese medicine preparation and the production method thereof of its effective constituent as antitussive particularly with Folium mangiferae or almond leaf, the method of extracting the total glycosides of Folium mangiferae from Folium mangiferae and almond leaf comprises the pulverizing of Folium mangiferae or almond leaf, alcohol reflux, the non-polar solvent extraction, decolouring, filter, operations such as crystallization, with the total glycosides production of Folium mangiferae cough relief traditional Chinese medicine, do not add or only add an amount of auxiliary material, be prepared into the oral preparations of relieving cough and reducing sputum effect, has the active constituent content height, characteristics such as taking dose is little.Extraction (extraction) method of above-mentioned 3 kinds of Mangiferins mentioning, mainly be that liquid such as water, hexane, alcohol, methane dioxide, sherwood oil, benzene, ether, industrial naptha are as extracting solvent, its result other impurity often is extracted out with Mangiferin, needs aftertreatment (making with extra care) process; In addition, also there are problems such as harmful dissolvent residual in these technologies.
Summary of the invention
The inventor herein is through exploring for many years, and extraction, the process for purification of Mangiferin carried out many-sided research and test, obtained technical breakthrough.
Technical scheme of the present invention comprises extraction, decolouring and the process for purification of Mangiferin.
The raw material that the present invention uses is the Chinese medicinal herbs that contains Mangiferin, as Anacardiaceae plant Folium mangiferae and almond leaf, the liliaceous plant wind-weed, Polypodiaceae plant pyrrosia lingua etc., preferred in the present invention Folium mangiferae and almond leaf.
Extraction, refining solvent that the present invention uses are alcohol-water mixed solution, and alcohol wherein can be methyl alcohol, also can be ethanol.The solubility scope of using between 35%-85%, preferred 50%-60%.
The present invention adopts macroporous adsorbent resin that the Mangiferin extracting solution is decoloured, and can adopt a kind ofly separately, or adopts the series connection of 2-3 kind to use.The preferred resin tandem plan of the present invention is: D101-D900, D101-D301, D101-D296, D101-D318.
This suction is carried out the purified method to the Mangiferin crude product and is, with the alcoholic solution dissolving crude product of 50-60%, behind the recovery alcohol, Mangiferin is separated out in water; Perhaps the method for thermosol cold analysis is carried out crystallization, separates out Mangiferin.
Compared with prior art, outstanding substantive distinguishing features of the present invention and obvious improvement are:
1. the present invention adopts alcohol-water solution to extract, and use other organic solvent is in addition arranged in the technology, uses the macroporous resin decolouring, has avoided harmful organic solvent such as sherwood oil residual.
2. the invention provides the preparation technology of the Mangiferin that can obtain purity 〉=90%.And patent 03125270.2 and 03128227.4 can only obtain the mixture of Mangiferin and Isomangiferin, homomangiferin.
3. the present invention has industrial amplification, easily technology is amplified, and reaches to expand the scale of production, and realizes the purpose of industrialization.
Embodiment
The following example is used to illustrate the present invention, is not any restriction to protection domain of the present invention.
Embodiment one
Fresh Folium mangiferae dries, and removes impurity, shreds or break into meal, with 40% aqueous ethanolic solution refluxing extraction 2 times, each 10 times of amounts * 2 hours, united extraction liquid is chilled to room temperature, D101 post in the elder generation, go up the D900 post again, collect effluent liquid, reclaim ethanol, obtain the Mangiferin crude product.Crude product is with 55% ethanol heating for dissolving, filtered while hot, and filtrate is chilled to room temperature, separates out the Mangiferin elaboration, and Mangiferin purity reaches more than 90%.
Embodiment two
Fresh almond leaf is put under the sun and is dried, and breaks into meal, with 55% aqueous ethanolic solution refluxing extraction 2 times, and each 12 times of amounts * 1.5 hours, united extraction liquid is chilled to room temperature, and D101 post elder generation in is gone up the D301 post again, the collection effluent liquid, recovery ethanol obtains the Mangiferin crude product.Crude product reclaims ethanol and flings to most of water with 65% ethanol heating for dissolving, separates out Mangiferin, carries out so repeatedly 2 times, and the Mangiferin purity that obtains reaches more than 90%.
Embodiment three
Dried almond leaf breaks into meal, with 65% methanol aqueous solution refluxing extraction 2 times, and each 12 times of amounts * 2 hours, united extraction liquid is chilled to room temperature, and first D101 post is gone up the D296 post again,, collect effluent liquid, recovery ethanol obtains the Mangiferin crude product.Crude product reclaims ethanol and flings to most of water with 75% ethanol heating for dissolving, separates out Mangiferin, carries out so repeatedly 2 times, and the Mangiferin purity that obtains reaches more than 90%.
Embodiment four
Dried Folium mangiferae is removed impurity, shreds or break into meal, with 55% aqueous ethanolic solution diacolation, collects the fluid of filtering, and D101 post in the elder generation is gone up the D318 post again, collects effluent liquid, reclaims ethanol, obtains the Mangiferin crude product.Crude product is with 50% methyl alcohol heating for dissolving, filtered while hot, and filtrate putting is chilled to room temperature, separates out the Mangiferin elaboration, and the Mangiferin purity that obtains reaches more than 90%.
Embodiment five
Fresh Folium mangiferae dries, and removes impurity, shreds or break into meal, with 60% n-propyl alcohol aqueous solution refluxing extraction 2 times, each 10 times of amounts * 2 hours, united extraction liquid is chilled to room temperature, last D101 macroporous resin column, collect effluent liquid, reclaim ethanol, obtain the Mangiferin crude product.Crude product reclaims ethanol and flings to most of water with 50% methyl alcohol heating for dissolving, separates out Mangiferin, carries out so repeatedly 2 times, and the Mangiferin purity that obtains reaches more than 90%.
Embodiment six
The dried wind-weed breaks into meal, with 60% aqueous ethanolic solution diacolation, collects the fluid of filtering, and D101 post in the elder generation is gone up the D301 post again, collects effluent liquid, reclaims ethanol, obtains the Mangiferin crude product.Crude product reclaims methyl alcohol and flings to most of water with 70% methyl alcohol heating for dissolving, separates out Mangiferin, carries out so repeatedly 2 times, and the Mangiferin purity that obtains reaches more than 90%.
Claims (7)
1. Mangiferin preparation technology, it is characterized in that: technical process is as follows:
Contain the raw material of Mangiferin → with alcoholic solution extraction → alcohol extract → decolouring → destainer → recovery solvent → separate out Mangiferin crude product → dilute alcohol solution dissolving → Mangiferin solution → recovery solvent → separate out Mangiferin elaboration.
2. the raw material that contains Mangiferin according to claim 1 is characterized in that: with the plant that contains Mangiferin serves as to extract raw material, preferred Anacardiaceae plant Folium mangiferae and almond leaf, the liliaceous plant wind-weed.
3. alcoholic solution according to claim 1 is characterized in that: the solution that nail alcohol, ethanol or both mixtures and water form.
4. extraction according to claim 1 is characterized in that: refer to methods such as immersion, refluxing extraction, normal temperature and pressure diacolation.
5. decolouring according to claim 1 is characterized in that: adopt resin decolorization.
6. Mangiferin elaboration according to claim 1 is characterized in that: Mangiferin purity 〉=90%.
7. resin according to claim 5 is characterized in that: refer to macroporous ion-exchange resin, preferred D101, D301, D318, D296.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100792345A CN100475830C (en) | 2006-04-18 | 2006-04-18 | Process for preparing high purity mangiferin |
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| CNB2006100792345A CN100475830C (en) | 2006-04-18 | 2006-04-18 | Process for preparing high purity mangiferin |
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| CN100475830C CN100475830C (en) | 2009-04-08 |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100393691C (en) * | 2006-10-25 | 2008-06-11 | 福州大学 | Method for preparing mandelic acid by macroporous adsorptive resin |
| CN100450991C (en) * | 2006-10-13 | 2009-01-14 | 福州大学 | Process for preparing peach leaf mandelic acid extract |
| CN101214254B (en) * | 2008-01-09 | 2010-12-29 | 昆明制药集团股份有限公司 | New use of mangiferin compounds |
| CN101973985A (en) * | 2010-11-15 | 2011-02-16 | 广西中医学院 | Method for preparing mangiferin |
| CN102161657A (en) * | 2010-02-24 | 2011-08-24 | 昆明制药集团股份有限公司 | Mangiferin crystal I and preparation method thereof |
| CN102512359A (en) * | 2012-01-13 | 2012-06-27 | 广西中医学院 | Mangiferin cream with anti-herpes simplex virus effect |
| CN101993437B (en) * | 2009-08-27 | 2012-07-25 | 上海新康制药厂 | Method for extracting mangiferin from mango leaf |
| CN102617669A (en) * | 2012-03-03 | 2012-08-01 | 浙江大学 | Method for separating and purifying mangiferin from mango pericarp |
| CN101993438B (en) * | 2009-08-27 | 2014-04-09 | 上海新康制药厂 | Method for extracting mangiferin and total saponins of rhizoma anemarrhenae from rhizoma anemarrhenae |
| CN104311614A (en) * | 2014-11-05 | 2015-01-28 | 桂林益元素生物科技有限公司 | Method for extracting mangiferin from mango leaves |
| CN106831909A (en) * | 2016-12-29 | 2017-06-13 | 晨光生物科技集团邯郸有限公司 | The extracting method of double benzene pyrrones compounds in wind-weed fibrous root |
| CN107129491A (en) * | 2017-07-13 | 2017-09-05 | 湖南原草生物技术有限公司 | The method that mangiferin is extracted with mango leaf |
| CN107242428A (en) * | 2017-06-14 | 2017-10-13 | 百色学院 | A kind of preparation method of mangrove bark bacteriostatic agent |
| CN107383130A (en) * | 2017-07-20 | 2017-11-24 | 广西南宁桂知科技有限公司 | A kind of method that mangiferin is prepared using myrica rubra leaf |
| CN109081859A (en) * | 2018-09-27 | 2018-12-25 | 那坡康正天然植物提取有限责任公司 | The production method of mangiferin |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101671330B (en) * | 2009-10-13 | 2012-05-02 | 刘全胜 | Preparation method of mangiferin |
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2006
- 2006-04-18 CN CNB2006100792345A patent/CN100475830C/en not_active Expired - Fee Related
Cited By (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100450991C (en) * | 2006-10-13 | 2009-01-14 | 福州大学 | Process for preparing peach leaf mandelic acid extract |
| CN100393691C (en) * | 2006-10-25 | 2008-06-11 | 福州大学 | Method for preparing mandelic acid by macroporous adsorptive resin |
| CN101214254B (en) * | 2008-01-09 | 2010-12-29 | 昆明制药集团股份有限公司 | New use of mangiferin compounds |
| CN101993437B (en) * | 2009-08-27 | 2012-07-25 | 上海新康制药厂 | Method for extracting mangiferin from mango leaf |
| CN101993438B (en) * | 2009-08-27 | 2014-04-09 | 上海新康制药厂 | Method for extracting mangiferin and total saponins of rhizoma anemarrhenae from rhizoma anemarrhenae |
| CN102161657A (en) * | 2010-02-24 | 2011-08-24 | 昆明制药集团股份有限公司 | Mangiferin crystal I and preparation method thereof |
| CN102161657B (en) * | 2010-02-24 | 2013-12-11 | 昆明制药集团股份有限公司 | Mangiferin crystal I and preparation method thereof |
| CN101973985B (en) * | 2010-11-15 | 2013-06-05 | 广西中医学院 | Method for preparing mangiferin |
| CN101973985A (en) * | 2010-11-15 | 2011-02-16 | 广西中医学院 | Method for preparing mangiferin |
| CN102512359A (en) * | 2012-01-13 | 2012-06-27 | 广西中医学院 | Mangiferin cream with anti-herpes simplex virus effect |
| CN102512359B (en) * | 2012-01-13 | 2013-01-09 | 广西中医学院 | Mangiferin cream with anti-herpes virus effect |
| CN102617669A (en) * | 2012-03-03 | 2012-08-01 | 浙江大学 | Method for separating and purifying mangiferin from mango pericarp |
| CN102617669B (en) * | 2012-03-03 | 2014-06-04 | 浙江大学 | Method for separating and purifying mangiferin from mango pericarp |
| CN104311614A (en) * | 2014-11-05 | 2015-01-28 | 桂林益元素生物科技有限公司 | Method for extracting mangiferin from mango leaves |
| CN104311614B (en) * | 2014-11-05 | 2016-07-20 | 桂林益元素生物科技有限公司 | A kind of method extracting Mengiferin from Folium mangiferae |
| CN106831909A (en) * | 2016-12-29 | 2017-06-13 | 晨光生物科技集团邯郸有限公司 | The extracting method of double benzene pyrrones compounds in wind-weed fibrous root |
| CN106831909B (en) * | 2016-12-29 | 2019-10-22 | 晨光生物科技集团邯郸有限公司 | The extracting method of double benzene pyrrones compounds in rhizoma anemarrhenae fibrous root |
| CN107242428A (en) * | 2017-06-14 | 2017-10-13 | 百色学院 | A kind of preparation method of mangrove bark bacteriostatic agent |
| CN107242428B (en) * | 2017-06-14 | 2020-06-30 | 百色学院 | Preparation method of mango peel bacteriostatic agent |
| CN107129491A (en) * | 2017-07-13 | 2017-09-05 | 湖南原草生物技术有限公司 | The method that mangiferin is extracted with mango leaf |
| CN107383130A (en) * | 2017-07-20 | 2017-11-24 | 广西南宁桂知科技有限公司 | A kind of method that mangiferin is prepared using myrica rubra leaf |
| CN109081859A (en) * | 2018-09-27 | 2018-12-25 | 那坡康正天然植物提取有限责任公司 | The production method of mangiferin |
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| CN100475830C (en) | 2009-04-08 |
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