CN104311614B - A kind of method extracting Mengiferin from Folium mangiferae - Google Patents
A kind of method extracting Mengiferin from Folium mangiferae Download PDFInfo
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- CN104311614B CN104311614B CN201410619517.9A CN201410619517A CN104311614B CN 104311614 B CN104311614 B CN 104311614B CN 201410619517 A CN201410619517 A CN 201410619517A CN 104311614 B CN104311614 B CN 104311614B
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- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
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- C07H1/08—Separation; Purification from natural products
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Abstract
The invention discloses a kind of method extracting Mengiferin from Folium mangiferae, comprise the steps: Feedstock treating, high pressure extract, aqueous two-phase extraction, desalination, recrystallization, obtain Mengiferin.Having content height, extraction ratio is high, and technique is simple, is suitable for producing, the advantages such as production cost is low.
Description
Technical field
The present invention relates to the extracting method of biological technical field, specifically a kind of method extracting Mengiferin from Folium mangiferae.
Background technology
Fructus Mangifera Indicae, for aiphyllium, originates in India, and various places, the existing torrid zone are all planted, and cultivate in South China, and by Guangxi, Guangdong, village, various places, Hainan or room residence, somewhat moistening soil is scattered about like the stars plant as seen.Folium mangiferae is the leaf of Anacardiaceae plant Fructus Mangifera Indicae MangiferaindicaL, Chinese medicine is commonly used for Guangxi Local, record in " Guangxi Chinese crude drug standard " nineteen ninety version, contained Mengiferin (Mangiferin) is Folium mangiferae cough-relieving, reduce phlegm, the main active of antiinflammatory, Mengiferin has antiinflammatory, antiviral, central nerve inhibition and immunosuppressive action, also has anti peroxidation of lipid, antitumor action, conventional to treat hepatitis, Mengiferin treatment chronic bronchitis has good therapeutic effect, hepatoma cell strain is had obvious toxic action by Mengiferin, energy liver cancer apoptosis reducing, Mengiferin has anti-oxidant vigor and delaying senility function.
Disclosed Mengiferin method for extraction and purification mostly is water extract-alcohol precipitation, alcohol extraction purification by macroporous resin method at present, as Chinese patent CN100475830C " high-purity Mengiferin preparation method ", patent CN101759689A " preparation method of a kind of Mengiferin " and patent CN101429222A " extract a kind of method of Mengiferin ", it is all adopt purification by macroporous resin as main separating step, but adopt purification by macroporous resin method, resin is with front needing process, purification need to pass through absorption and elution process, and the production cycle is long.When being purified eluting with macroporous resin, due to physical absorption, also easily cause a part of sample and extremely adsorb, and cause that the rate of transform reduces.Additionally adopting purification by macroporous resin effluent volume relatively big, the solvent recovery time is long, adds production cost, and solvent recovery produces more waste liquid, and environmental protection causes certain burden.Additionally due to the use of macroporous resin, add the risk introducing the organic residual solvents such as benzene,toluene,xylene, styrene, alkanes, diethylbenzene class, the safety of product is exerted a certain influence.
In sum, study a kind of simple possible, the extracting method of Mengiferin that environmental pollution is little has good realistic meaning.
Summary of the invention
It is an object of the invention to provide a kind of method extracting Mengiferin from Folium mangiferae, there is technique simple, be suitable for producing, the advantages such as the time is short.
The present invention is achieved through the following technical solutions, and specifically includes following steps:
1) Feedstock treating: Folium mangiferae is pulverized or smashes；
2) high pressure extract: by the raw material after process, put in pressure pan, adds the pure water of identical weight, is forced into 4kgf/cm2So that it is pressure is uniform, and keeps 10-15min, recovers normal pressure, filters, obtains extracting solution；
3) separate: Folium mangiferae is carried out aqueous two-phase extraction, obtain and extract upper phase and extract lower phase, the double-aqueous phase system that aqueous two-phase extraction uses is made up of Polyethylene Glycol, sodium hydroxide and water, described Polyethylene Glycol mass percent in described double-aqueous phase system is 10-20%, described sodium hydroxide mass percent in described double-aqueous phase system is 10-20%, surplus is water, and the weight average molecular weight of described Polyethylene Glycol is 1000-8000；
4) subsequent treatment: by step 3) phase in the extraction that obtains, desalination, recrystallization, by step 3) phase under the extraction that obtains, add and be equivalent to extract lower phase mass percent 5-10% sodium hydroxide, desalination, recrystallization；
5) the acquisition thing after merging recrystallization obtains Mengiferin.
Folium mangiferae of the present invention is fresh and/or dried Folium mangiferae.
Described desalination preferably employs ultrafiltration or dialysis, the ultrafilter membrane desalination that ultrafiltration adopts molecular cut off to be 1000-100000, the bag filter desalination that dialysis adopts molecular cut off to be 1000-100000.
The Mengiferin that the present invention obtains, detects through HPLC, and content is more than 98.5%.
Compared with prior art, advantages of the present invention:
1, prior art is when carrying out the extraction of Mengiferin, pre-treatment is typically all with water or ethanol etc. for solvent, by heating extraction by effective ingredient dissolution, and the present invention adopts high pressure extract, compare heating extraction, through high pressure effect so that the composition such as the organic acid that contains in Folium mangiferae, polyphenol, Mengiferin can be fully dissolved out, it is beneficial to the process of subsequent technique, is beneficial to the yield improving active component.
2, Mengiferin poorly water-soluble, is soluble in rare alcohol, hot methanol and ethanol, is soluble in sig water；Mengiferin 7-O-glycoside (Mangiferin-7-0-R-D-glucopy-ranoside) of its amount 5% of generally entail that coexists in leaf.Because 3 hydroxyl acidity in structure are relatively strong, therefore two compounds are all soluble in alkaline water liquid, and Mengiferin 7-0-glycoside also can be hydrolyzed into Mengiferin in alkaline water liquid, thus yield and the purity of Mengiferin can be improved.The present invention adds alkaline solution when extracting, it is possible to be sufficiently separated Mengiferin and Mengiferin 7-O-glycoside, again through subsequent technique so that Mengiferin 7-O-glycoside can be converted into Mengiferin, improves yield.
3, the Mengiferin content that prior art obtains is usually no more than 98%, the present invention adopts the combination of high pressure extract and aqueous two phase extraction technique, production efficiency can be improved greatly, resin used by prior art column chromatography, for being generally non-polar resin, can only obtain the extract of Mengiferin content 40-50% through primary sorption；If employing polar resin, also can only obtain Mengiferin content about 50% through primary sorption, the Mengiferin wanting to obtain higher amount must flow through 2 times or more times Adsorption, thus adding process time and cost.Aqueous two phase extraction technique is as a kind of novel isolation technics, have mild condition, easy and simple to handle, be prone to series of advantages such as amplifying, separating power is strong, and adopt the technology of the present invention to combine, the raising of matter occurs, content and the extraction efficiency of Mengiferin can be increased, comparing water to carry or column chromatography after alcohol extraction, the present invention time is short, and Mengiferin content is high.
4, present invention, avoiding the use of a large amount of organic solvent such as dehydrated alcohol, methanol, more environmentally-friendly.
Detailed description of the invention
With embodiment, the invention will be further described below, but the invention is not limited in these embodiments.
Embodiment 1:
A kind of method extracting Mengiferin from Folium mangiferae, specifically includes following steps:
1) Feedstock treating: fresh mango leaf is smashed；
2) high pressure extract: by the raw material after process, put in pressure pan, adds the pure water of identical weight, is forced into 4kgf/cm2So that it is pressure is uniform, and keeps 10min, recovers normal pressure, filters, obtains extracting solution；
3) separate: Folium mangiferae is carried out aqueous two-phase extraction, obtain and extract upper phase and extract lower phase, the double-aqueous phase system that aqueous two-phase extraction uses is made up of Polyethylene Glycol, sodium hydroxide and water, Polyethylene Glycol mass percent in described double-aqueous phase system is 20%, sodium hydroxide mass percent in described double-aqueous phase system is 10%, surplus is water, and the weight average molecular weight of Polyethylene Glycol is 1000-8000；
4) subsequent treatment: by step 3) phase in the extraction that obtains, ultrafiltration adopts molecular cut off to be the ultrafilter membrane desalination of 1000-100000, recrystallization, by step 3) phase under the extraction that obtains, adding and be equivalent to extract lower phase mass percent 10% sodium hydroxide, ultrafiltration adopts molecular cut off to be the ultrafilter membrane desalination of 1000-100000, recrystallization；
5) merge dried acquisition thing and obtain Mengiferin.
Embodiment 2:
A kind of method extracting Mengiferin from Folium mangiferae, specifically includes following steps:
1) Feedstock treating: dry Folium mangiferae is pulverized；
2) high pressure extract: by the raw material after process, put in pressure pan, adds the pure water of identical weight, is forced into 4kgf/cm2So that it is pressure is uniform, and keeps 15min, recovers normal pressure, filters, obtains extracting solution；
3) separate: Folium mangiferae is carried out aqueous two-phase extraction, obtain and extract upper phase and extract lower phase, the double-aqueous phase system that aqueous two-phase extraction uses is made up of Polyethylene Glycol, sodium hydroxide and water, Polyethylene Glycol mass percent in described double-aqueous phase system is 10%, sodium hydroxide mass percent in described double-aqueous phase system is 20%, surplus is water, and the weight average molecular weight of Polyethylene Glycol is 1000-8000；
4) subsequent treatment: by step 3) phase in the extraction that obtains, dialysis adopts molecular cut off to be the bag filter desalination of 1000-100000, recrystallization, by step 3) phase under the extraction that obtains, adding and be equivalent to extract lower phase mass percent 5% sodium hydroxide, dialysis adopts molecular cut off to be the bag filter desalination of 1000-100000, recrystallization；
5) merge dried acquisition thing and obtain Mengiferin.
Embodiment 3:
A kind of method extracting Mengiferin from Folium mangiferae, specifically includes following steps:
1) Feedstock treating: dry Folium mangiferae is pulverized；
2) high pressure extract: by the raw material after process, put in pressure pan, adds the pure water of identical weight, is forced into 4kgf/cm2So that it is pressure is uniform, and keeps 12min, recovers normal pressure, filters, obtains extracting solution；
3) separate: Folium mangiferae is carried out aqueous two-phase extraction, obtain and extract upper phase and extract lower phase, the double-aqueous phase system that aqueous two-phase extraction uses is made up of Polyethylene Glycol, sodium hydroxide and water, Polyethylene Glycol mass percent in described double-aqueous phase system is 15%, sodium hydroxide mass percent in described double-aqueous phase system is 15%, surplus is water, and the weight average molecular weight of Polyethylene Glycol is 1000-8000；
4) subsequent treatment: by step 3) phase in the extraction that obtains, ultrafiltration adopts molecular cut off to be the ultrafilter membrane desalination of 1000-100000, recrystallization, by step 3) phase under the extraction that obtains, adding and be equivalent to extract lower phase mass percent 10% sodium hydroxide, ultrafiltration adopts molecular cut off to be the ultrafilter membrane desalination of 1000-100000, recrystallization；
5) merge dried acquisition thing and obtain Mengiferin.
Result:
Claims (2)
1. the method extracting Mengiferin from Folium mangiferae, it is characterised in that:
Comprise the steps:
1) Feedstock treating: Folium mangiferae is pulverized or smashes；
2) high pressure extract: by the raw material after process, put in pressure pan, adds the pure water of identical weight, is forced into 4kgf/cm2So that it is pressure is uniform, and keeps 10-15min, recovers normal pressure, filters, obtains extracting solution；
3) separate: to step 2) obtain extracting solution and carry out aqueous two-phase extraction, obtain and extract upper phase and extract lower phase, the double-aqueous phase system that aqueous two-phase extraction uses is made up of Polyethylene Glycol, sodium hydroxide and water, described Polyethylene Glycol mass percent in described double-aqueous phase system is 10-20%, described sodium hydroxide mass percent in described double-aqueous phase system is 10-20%, surplus is water, and the weight average molecular weight of described Polyethylene Glycol is 1000-8000；
4) subsequent treatment: by step 3) phase in the extraction that obtains, desalination, recrystallization, by step 3) phase under the extraction that obtains, add and be equivalent to extract lower phase mass percent 5-10% sodium hydroxide, desalination, recrystallization；
5) the acquisition thing after merging recrystallization obtains Mengiferin.
2. a kind of method extracting Mengiferin from Folium mangiferae according to claim 1, it is characterised in that: described Folium mangiferae is fresh and/or dried Folium mangiferae.
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