CN107129491A - The method that mangiferin is extracted with mango leaf - Google Patents
The method that mangiferin is extracted with mango leaf Download PDFInfo
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- CN107129491A CN107129491A CN201710570143.XA CN201710570143A CN107129491A CN 107129491 A CN107129491 A CN 107129491A CN 201710570143 A CN201710570143 A CN 201710570143A CN 107129491 A CN107129491 A CN 107129491A
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- mangiferin
- mango leaf
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- mango
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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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Abstract
A kind of method that mangiferin is extracted from mango leaf, it is that mango leaf is first subjected to ultramicro grinding, sporoderm-broken rate is improved, then mangiferin crude extract is extracted from mango leaf with edible ethanol, and the mangiferin crude extract is isolated and purified to obtain mangiferin with D101 macroreticular resins combination D296 resin anion (R.A.)s.This method is extracted using edible ethanol safety non-toxic and is separated mangiferin, can not only industrialized production safely and effectively different purity specification mango glucoside extract, and the higher value application of safe and simple, reasonable, economic Mango Resources and the industrialized production of series of products are veritably realized, fully demonstrate the theory of Green Chemistry production and the strategy of recycling economy.
Description
Technical field
It is espespecially a kind of first to use ultra micro the present invention relates to a kind of green chemistry process technology that mangiferin is extracted from mango leaf
Crush, edible ethanol extracts mangiferin, and the green of mangiferin is then isolated and purified with D101 macroreticular resins, D296 resin anion (R.A.)s
Isolation and purification method.
Background technology
Mangiferin, also known as mangiferin, light lark acicular crystal（50% ethanol）.Mangiferin is for treating chronic branch gas
Guan Yan has good therapeutic effect, is the principle active component that Swertia mussotii treats hepatitis, is antiviral active component in Asphodeloides Bge Rhizome.Awns
Fruit glycosides, which has, suppresses central nervous system, anti-inflammatory, antibacterial, anti-herpes simplex virus HSV-2, cholagogic and immunization, can alleviate
Sacrum nerve root disease, has protective effect to simulated high altitude acute hypoxia hepatic injury caused by HSV-2 viruses.
Mangiferin is present in Anacardiaceae plant mango (Mangifera indica L.) fruit, leaf, bark.Mango
Leaf contains polytype compound, and its nature difference is very big (from polarity to nonpolar)；Isomers in same type compound
It is many, its otherness and very little, it is difficult to separate, and some of compound heat sensitivitys are strong, and easily oxidation, isomery, decomposition.
Existing many extracts the method for separating mangiferin from mango leaf in the prior art, and such as CN201710057903.7 is
Extracted again with methanol after extracting mango leaf powder removal of impurities with ethyl acetate, gained filtrate thickening and washing, dry mangiferin crude product, or
Further crystallization purifying obtains mangiferin sterling；CN200910194672.X is that mango leaf powder is extracted with alkaline aqueous solution
Afterwards, filtrate is centrifuged with the acidifying of dilute ore deposit acid, concentration plus alcohol, and using SephadexLH-20 gel post separations, eluent is used after being evaporated
Alcohol is recrystallized to give mangiferin；CN201610965106.4 is to extract mango leaf powder using ethanol and antioxidant, then using solidifying
Mangiferin is made in glue post and macroporous adsorption resin chromatography combination；CN200910175781.7 is to use oil after mango leaf powder is digested
Ether degreasing, is extracted with ethanol, dried, then dissolved with ethanol water, centrifugal filtration is dried and mangiferin is made；
CN201010292465.0 is concentrated with filtrate after alcohol extracting, then is extracted with organic solvent, aqueous crystallization, crystal acetone and water
Mixed solution recrystallization mangiferin etc. is made, although those methods all can from mango leaf separation and Extraction mangiferin, but simultaneously
D101 macroreticular resins and the combination of D296 resin anion (R.A.)s mangiferin is not isolated and purified into.And CN200610079234.5, though
So refer to using single macroporous ion-exchange resin, preferably D101, D301, D318 or D296, but this method is adopted after alcohol extracting
Decolourized, rather than isolated and purified with those resins.
The content of the invention
The technical problems to be solved by the invention are：Carried for above-mentioned the deficiencies in the prior art there is provided one kind with mango leaf
The method for taking mangiferin, this method extracts mangiferin with D101 macroreticular resins combination D296 resin anion (R.A.)s from mango leaf, high
Effect, green safety, low cost, high yield pulp1, high-purity, it is adaptable to industrial production.
In order to solve the above technical problems, the technical solution adopted in the present invention is：It is a kind of that mangiferin is extracted with mango leaf
Method, it is characterised in that this method is first to crush mango leaf for the ultrafine powder below 300 mesh, using edible ethanol from awns
Mangiferin crude extract is extracted in fruit leaf powder, then mangiferin crude extract is combined D296 resin anion (R.A.)s with D101 macroreticular resins and is carried out
Isolate and purify, produce mangiferin.
It is above-mentioned refer to by mangiferin crude extract with D101 macroreticular resins combination D296 resin anion (R.A.)s isolated and purified
Refer to mangiferin crude extract being adsorbed to by the chromatographic column of D101 macroreticular resins with the BV/h of 2.0 BV/h~4.0 flow velocity full
With rinsed with the ethanol solution of 1BV~3BV 50% volumetric concentration with 1BV/h~3BV/h flow velocity to colourless, collect elution
Liquid；By D296 resin anion (R.A.)s chromatographic column on eluent, with the ethanol solution of 1BV~3BV 50% volumetric concentration with 1BV/h~
3BV/h flow velocitys are rinsed to colourless, eluent are collected, by eluent under the conditions of -0.05 MPa~-0.09MPa, 45 DEG C~55 DEG C
Concentration, reclaims edible ethanol, -0.05 MPa~-0.09MPa, 40 DEG C~60 DEG C vacuum freeze dryings are produced.
The above-mentioned use edible ethanol referred to extracts mangiferin crude extract from mango leaf powder and referred to 50%~80% volume
The edible ethanol that concentration and pH are 5~8 extracts mangiferin crude extracts in 70 DEG C~90 DEG C from mango leaf powder.Further, it is
Refer to and use 50%~80% volumetric concentration and pH is 5~8 edible ethanol, add 8 by 1g mango leaf powder~ratios of 12mL edible ethanols
Example, addition edible ethanol is extracted 2 times at 70 DEG C~90 DEG C in mango leaf powder, and each extraction time is 1~2h, by extract solution
Filtering, merging filtrate produces mangiferin crude extract.
It is above-mentioned refer to crush mango leaf be to carry out being crushed to the ultrafine powder below 300 mesh with airslide disintegrating mill,
To improve sporoderm-broken rate.
In the inventive method, using through Static Adsorption and the D101 macroporous absorbent resins that screen of desorption and D296 it is cloudy from
Sub- resin adsorption mangiferin, to not by macroporous absorbent resin absorbed portion, through the recovery edible ethanol that is concentrated under reduced pressure.To above-mentioned steps
It is middle absorption macroporous absorbent resin mango leaf mangiferin carry out elution reclaim when, be first washed to distillation it is colourless, then with eat
Ethanol elution mangiferin, the purity and yield of obtained mangiferin is all higher.
The processing of the D101 macroreticular resins and D296 resin anion (R.A.)s that are used in this method：New resin is soaked using 95% ethanol
48h is steeped, no muddiness is washed with ethanol afterwards, no alcohol taste is then washed to distillation.Used resin be first washed till with 95% it is colourless,
Then no alcohol taste is washed to distillation；It is washed till colourless, is washed with water to neutrality with 5% hydrochloric acid；With 5%NaOH be washed till it is colourless after, use
Neutrality is washed to, it is standby.
Compared with prior art, it is an advantage of the invention that：
1st, the present invention uses ultramicro grinding mango leaf, can effectively be increased operation rate using ultrafine powder.
2nd, extract integrated use edible ethanol safety non-toxic mango leaf active component, D101 macroreticular resins, D296 it is cloudy from
The methods such as sub- resin separation purification mangiferin, can not only industrialized production safely and effectively different purity specification mangiferin extract
Thing for the functional product such as follow-up liver protecting, anti-inflammatory, anti-oxidant research and development, and veritably realize it is safe and simple,
Rationally, the higher value application and the industrialized production of series of products of economic mango leaf resource, fully demonstrate greenization student
The theory of production and the strategy of recycling economy.Thus, the present invention has theoretical novelty, technological sciences, operation and product safety, technique
Simplicity, economically feasible, it is environment-friendly the features such as.
3rd, mango leaf main active mango is purified using natural product chemistry and modern production technology extracting and developing
Glycosides, is made into the mango glucoside extract of the various pureness specifications of the current international practice, preferably comply with and meet modern functions food,
The health fields such as health products, medicine, daily chemical product, to its is natural, safely, effectively, convenient demand.
Embodiment
Embodiment 1
Take mango leaf, by mango leaf using airslide disintegrating mill crushing as 300 mesh below ultrafine powder, with 50% volumetric concentration and pH
It is Extraction solvent for 8 edible ethanol, the ratio of 12mL edible ethanols is added in 1g mango leaf powder, is added in mango leaf powder edible
Ethanol extracts 2h at 70 DEG C, extracts 2 times, extract solution is filtered, merging filtrate, produce mangiferin crude extract.
From processed D101 macroporous absorbent resins and D296 resin anion (R.A.)s resin is isolated and purified as mangiferin.
The chromatographic column that mangiferin crude extract is first passed through into D101 macroreticular resins with 2.0 BV/h flow velocity is adsorbed to saturation, with the 50% of 1BV
The ethanol solution of volumetric concentration is rinsed to colourless with 1BV/h flow velocity, collects eluent；Again by D296 anion tree on eluent
Fat chromatographic column, is rinsed to colourless with 1BV/h flow velocitys with the ethanol solution of 1BV 50% volumetric concentration, collects eluent, will elute
Liquid is concentrated under the conditions of -0.05MPa, 55 DEG C, reclaims edible ethanol, -0.05 MPa, 60 DEG C of vacuum freeze dryings produce purifying
Mango glucoside extract, measure mangiferin yield for 85%, purity is 94%.
Embodiment 2
Take mango leaf, by mango leaf using airslide disintegrating mill crushing as 300 mesh below ultrafine powder, with 70% volumetric concentration and pH
It is Extraction solvent for 7 edible ethanol, the ratio of 10mL edible ethanols is added in 1g mango leaf powder, is added in mango leaf powder edible
Ethanol extracts 1.5h at 80 DEG C, extracts 2 times, extract solution is filtered, merging filtrate, produce mangiferin crude extract.
From processed D101 macroporous absorbent resins and D296 resin anion (R.A.)s resin is isolated and purified as mangiferin.
The chromatographic column that mangiferin crude extract is first passed through into D101 macroreticular resins with 3.0 BV/h flow velocity is adsorbed to saturation, with the 50% of 2BV
The ethanol solution of volumetric concentration is rinsed to colourless with 2BV/h flow velocity, collects eluent；Again by D296 anion tree on eluent
Fat chromatographic column, is rinsed to colourless with 2BV/h flow velocitys with the ethanol solution of 2BV 50% volumetric concentration, collects eluent, will elute
Liquid is concentrated under the conditions of -0.07 MPa, 50 DEG C, reclaims edible ethanol, -0.07MPa, 50 DEG C of vacuum freeze dryings produce purifying
Mango glucoside extract, measure mangiferin yield for 83%, purity is 93%.
Comparative example 1
Take mango leaf to crush, using 70% volumetric concentration and pH be 7 edible ethanol as Extraction solvent, add 10mL by 1g mango leaf powder
The ratio of edible ethanol, edible ethanol is added in mango leaf powder 1.5h is extracted at 80 DEG C, extract solution is filtered in extraction 2 times,
Merging filtrate, produces mangiferin crude extract.
From processed D101 macroporous absorbent resins resin is isolated and purified as mangiferin.By mangiferin crude extract with
The chromatographic column that 3.0 BV/h flow velocity first passes through D101 macroreticular resins is adsorbed to saturation, and the ethanol with 2BV 50% volumetric concentration is molten
Liquid is rinsed to colourless with 2BV/h flow velocity, collects eluent；Eluent is concentrated under the conditions of -0.07 MPa, 50 DEG C, reclaimed
Edible ethanol, -0.07MPa, 50 DEG C of vacuum freeze dryings, produces the mango glucoside extract of purifying, measures mangiferin yield and is
67%, purity is 50%.
Comparative example 2
Take mango leaf to crush, using 70% volumetric concentration and pH be 7 edible ethanol as Extraction solvent, add 10mL by 1g mango leaf powder
The ratio of edible ethanol, edible ethanol is added in mango leaf powder 1.5h is extracted at 80 DEG C, extract solution is filtered in extraction 2 times,
Merging filtrate, produces mangiferin crude extract.
From processed D296 resin anion (R.A.)s resin is isolated and purified as mangiferin.By mangiferin crude extract with
The chromatographic column that 3.0 BV/h flow velocity first passes through D296 resin anion (R.A.)s is adsorbed to saturation, with the ethanol of 2BV 50% volumetric concentration
Solution is rinsed to colourless with 2BV/h flow velocity, collects eluent；Eluent is concentrated under the conditions of -0.07 MPa, 50 DEG C, returned
Edible ethanol is received, -0.07MPa, 50 DEG C of vacuum freeze dryings produce the mango glucoside extract of purifying, and measuring mangiferin yield is
55%, purity is 32%.
Embodiment 3
Take mango leaf, by mango leaf using airslide disintegrating mill crushing as 300 mesh below ultrafine powder, with 80% volumetric concentration and pH
It is Extraction solvent for 5 edible ethanol, the ratio of 8mL edible ethanols is added in 1g mango leaf powder, is added in mango leaf powder edible
Ethanol extracts 1h at 90 DEG C, extracts 2 times, extract solution is filtered, merging filtrate, produce mangiferin crude extract.
From processed D101 macroporous absorbent resins and D296 resin anion (R.A.)s resin is isolated and purified as mangiferin.
The chromatographic column that mangiferin crude extract is first passed through into D101 macroreticular resins with 4.0 BV/h flow velocity is adsorbed to saturation, with the 50% of 3BV
The ethanol solution of volumetric concentration is rinsed to colourless with 3BV/h flow velocity, collects eluent；Again by D296 anion tree on eluent
Fat chromatographic column, is rinsed to colourless with 3BV/h flow velocitys with the ethanol solution of 3BV 50% volumetric concentration, collects eluent, will elute
Liquid is concentrated under the conditions of -0.09MPa, 45 DEG C, reclaims edible ethanol, -0.09MPa, 40 DEG C of vacuum freeze dryings produce purifying
Mango glucoside extract, it is 82% to measure mangiferin yield, and purity is 91%.
Claims (5)
1. it is a kind of with mango leaf extract mangiferin method, it is characterised in that this method be first by mango leaf crush for 300 mesh with
Under ultrafine powder, mangiferin crude extract is extracted from mango leaf powder using edible ethanol, then by mangiferin crude extract with D101
Macroreticular resin combination D296 resin anion (R.A.)s are isolated and purified, and produce mangiferin.
2. the method as claimed in claim 1 that mangiferin is extracted with mango leaf, it is characterised in that described by mangiferin crude extract
Isolate and purify referring to mangiferin crude extract with 2.0 BV/h~4.0 with D101 macroreticular resins combination D296 resin anion (R.A.)s
BV/h flow velocity is adsorbed to saturation by the chromatographic column of D101 macroreticular resins, and the ethanol with 1BV~3BV 50% volumetric concentration is molten
Liquid is rinsed to colourless with 1BV/h~3BV/h flow velocity, collects eluent；By D296 resin anion (R.A.)s chromatographic column on eluent, use
The ethanol solution of 1BV~3BV 50% volumetric concentration is rinsed to colourless with 1BV/h~3BV/h flow velocitys, is collected eluent, will be eluted
Liquid is concentrated under the conditions of -0.05 MPa~-0.09MPa, 45 DEG C~55 DEG C, recovery edible ethanol, and -0.05 MPa~-
0.09MPa, 40 DEG C~60 DEG C vacuum freeze dryings, are produced.
3. the as claimed in claim 1 method that mangiferin is extracted with mango leaf, it is characterised in that the use edible ethanol from
Extracted in mango leaf powder mangiferin crude extract refer to the edible ethanol that 50%~80% volumetric concentration and pH are 5~8 in 70 DEG C~
90 DEG C are extracted mangiferin crude extract from mango leaf powder.
4. the method as claimed in claim 3 that mangiferin is extracted with mango leaf, it is characterised in that be to use 50%~80% volume
Concentration and pH are 5~8 edible ethanol, add 8 in 1g mango leaf powder~ratios of 12mL edible ethanols, are added in mango leaf powder
Edible ethanol is extracted 2 times at 70 DEG C~90 DEG C, and each extraction time is 1~2h, extract solution is filtered, merging filtrate is produced
Mangiferin crude extract.
5. the method as claimed in claim 1 that mangiferin is extracted with mango leaf, it is characterised in that described to be by mango leaf crushing
Crushed using airslide disintegrating mill.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710570143.XA CN107129491A (en) | 2017-07-13 | 2017-07-13 | The method that mangiferin is extracted with mango leaf |
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| CN201710570143.XA CN107129491A (en) | 2017-07-13 | 2017-07-13 | The method that mangiferin is extracted with mango leaf |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107788531A (en) * | 2017-11-10 | 2018-03-13 | 西华大学 | Method for extracting polyphenol from mango kernels |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1844133A (en) * | 2006-04-18 | 2006-10-11 | 广西中医学院 | Process for preparing high purity mangiferin |
| CN101973985A (en) * | 2010-11-15 | 2011-02-16 | 广西中医学院 | Method for preparing mangiferin |
| CN106543158A (en) * | 2016-11-05 | 2017-03-29 | 王密治 | A kind of method that chimonin is extracted from Folium mangiferae |
-
2017
- 2017-07-13 CN CN201710570143.XA patent/CN107129491A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1844133A (en) * | 2006-04-18 | 2006-10-11 | 广西中医学院 | Process for preparing high purity mangiferin |
| CN101973985A (en) * | 2010-11-15 | 2011-02-16 | 广西中医学院 | Method for preparing mangiferin |
| CN106543158A (en) * | 2016-11-05 | 2017-03-29 | 王密治 | A kind of method that chimonin is extracted from Folium mangiferae |
Non-Patent Citations (2)
| Title |
|---|
| 孙晓明: "《探究大麦嫩苗的奥秘》", 31 October 2016, 《东南大学出版社》 * |
| 邓家刚，等: ""提取高纯度芒果苷的工艺研究"", 《中国中医药科技》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107788531A (en) * | 2017-11-10 | 2018-03-13 | 西华大学 | Method for extracting polyphenol from mango kernels |
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