CN104739904B - A kind of method that sugar-lowering components are extracted from Leaves of Hippophae L - Google Patents

A kind of method that sugar-lowering components are extracted from Leaves of Hippophae L Download PDF

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CN104739904B
CN104739904B CN201510168193.6A CN201510168193A CN104739904B CN 104739904 B CN104739904 B CN 104739904B CN 201510168193 A CN201510168193 A CN 201510168193A CN 104739904 B CN104739904 B CN 104739904B
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hippophae
leaves
extract
powder
sugar
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CN104739904A (en
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张小民
郭海利
张吉科
林美珍
姚莹
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SHANXI JINKEHAI BIOLOGICAL PRODUCT CO., LTD.
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SHANXI LIFE FORCE BIOLOGICAL PRODUCTS CO Ltd
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Abstract

A kind of method that sugar-lowering components are extracted from Leaves of Hippophae L of the present invention, belongs to plant hypoglycemic Component Extraction field;Technical problem to be solved is that sugar-lowering components extraction is difficult in Leaves of Hippophae L;The technical scheme used is a kind of method that sugar-lowering components are extracted from Leaves of Hippophae L, according to following steps:By Leaves of Hippophae L through finishing, after drying, coarse powder is ground into, the boiling boiling of 10 20 times of meal quality is added, is cooled to room temperature, obtains Leaves of Hippophae L pre-boiled liquid;1 5wt% Daqu is added by the quality of pre-boiled liquid, mixes, 35 days is incubated under the conditions of 26 36 DEG C;Pre-boiled liquid after heat-insulation soaking is filtered, filter residue and drying obtains Leaves of Hippophae L powder, standby;Extract solution in mass ratio:Leaves of Hippophae L powder=5:1 takes extract solution carries out refluxing extraction to Leaves of Hippophae L powder, flows back 23 times;Extract solution is recovered under reduced pressure after refluxing extraction, obtains paste sea-buckthorn leaf extract.

Description

A kind of method that sugar-lowering components are extracted from Leaves of Hippophae L
Technical field
A kind of method that sugar-lowering components are extracted from Leaves of Hippophae L of the present invention, belongs to plant hypoglycemic Component Extraction field.
Background technology
Corosolic acid also known as 2α-Hydroxyursolic Acid, it is a kind of pentacyclic triterpene acid, from the extract of banaba. Garcia(1940)Common rabbit is fed with banaba cured leaf, it is found that the blood glucose of rabbit declines, and with 1956 again using big Flower banaba leaf extract carries out clinical trial, it is found that it has the effect for reducing diabetes patient blood sugar.Murakami(1993) Deng isolating 2 kinds of triterpenic acids from the leaf of banaba(Corosolic acid and crataegolic acid), it is found that it is hypoglycemic Corosolic acid has Effect.Hamamoto(1999)There is obvious hypoglycemic effect after taking Corosolic acid Deng discovery mouse and rabbit, with using pancreas The effect of island element is identical.Toshihiro Miura(2004)Think that Corosolic acid can be by the glucose transporter in muscle (GLUT4)Glucose transport is promoted so as to reduce blood glucose, the effect of insulin analog to be served, so being claimed to intracellular For " insulin of plant kingdom ".Ren Xinfeng(2011)Point out Corosolic acid can make HepG2 cells it is obvious to glucose utilization rate on Rise, demonstrate the viewpoint of forefathers.Corosolic acid is primarily present in Lagerstroemia speciosa and loguat leaf, also there is report in other plant Road, but content is not high.Corosolic acid can dissociate presence in plant, can also the form of saponin exist, and usually with its Isomer crataegolic acid(2 Alpha-hydroxy oleanolic acids)Common to exist, structure is similar with chemical property, and separation is more difficult.2014 The pentacyclic triterpene acidoid in sea-buckthorn is determined first, because such material composition is complicated, some analogs into Point be not readily separated, therefore content is using the amount of Corosolic acid as standard, is 0.05% in sea-buckthorn, content is relatively low, up to the present there is not yet The report concentrated to it.
Sea-buckthorn is fruit, leaf dual purpose plant, and Leaves of Hippophae L has been treated as tealeaves and drunk at present, there is higher nutritive value. Extraction and concentration of the prior art to plant Corosolic acid have a variety of methods, but undesirable for seabuckthorn plant effect.According to Existing method carries out purification concentration to Leaves of Hippophae L, and in obtained enriched product, the content of Corosolic acid does not reach 0.3%.This journey The extract hypoglycemic effect of degree is very undesirable.
The content of the invention
Overcome the deficiencies in the prior art of the present invention, technical problem to be solved be to provide it is a kind of extracted from Leaves of Hippophae L it is dense The method of contracting sugar-lowering components.
In order to solve the above technical problems, the technical solution adopted in the present invention is as follows:
1st, through finishing and drying(Temperature is unsuitable too high, to be advisable not higher than 60 DEG C, preserves the effective of active material as far as possible Property)Leaves of Hippophae L afterwards is ground into the coarse powder of the mesh of 20 mesh -60, is put into 10-20 times of boiling tap water, is cooled to room temperature, standby With.
2nd, heat-insulation soaking
Any of three kinds of methods can be selected, in the case of other conditions identical, medicinal extract section that three kinds of methods obtain The content of Roseau acid improves successively;
Method one:Add 1%-5% wine brewing Daqu(Beer yeast powder can also be added), 26 DEG C -36 DEG C, 3-5 days are incubated, Make polysaccharose substance, the large biological molecule substance decomposition such as protein and lipid, increase the content of water extraction.If temperature is less than 26℃(Room temperature has to be higher than 18 DEG C), soaking time can be increased 2-3 days;If room temperature is higher than 36 DEG C, 3 days;
Method two:Add mixing enzyme preparation(Cellulase:Amylase:Pectase=1:1:1)0.5%, 28 DEG C of -38 DEG C of guarantors Warm 12-24h, increase plant tissue permeability, increase Corosolic acid from the dissolution rate in cell;
Method three:The vinegar room temperature for adding 0.5%-1% places 24h.
3rd, dry:Leaves of Hippophae L after immersion is filtered, abandons filtrate, is dried(60 DEG C of temperature highest), it is standby to obtain Leaves of Hippophae L powder.
4th, extract
Method one:It is more than Leaves of Hippophae L powder more than 5 times with weight ratio(The bigger recovery rate of amount for adding ethanol is higher)85%- 100% ethanol, in 80 DEG C of -90 DEG C of extractions, flow back 2 times, filtering, ethanol is recovered under reduced pressure and obtains medicinal extract;
Method two:Methanol is configured to 80%-90% methanol extract liquid with 1% NaOH(The higher Corosolic acid of NaOH concentration Solubility it is higher), extracted, flowed back 2 times with methanol extract liquid room temperature of the weight than more than 5 times more than Leaves of Hippophae L powder, filtering, Methanol is recovered under reduced pressure and obtains medicinal extract.
Compared with prior art the invention has the advantages that:According to the present processes to koroso in Leaves of Hippophae L Acid is concentrated, and its content can be made to reach more than 1%, has stronger hypoglycemic effect by rat test, and hypoglycemic effect is better than Corosolic acid sterling, the not exploitation of only Leaves of Hippophae L play larger impetus, also have found one kind for the treatment of diabetes New medicine.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
A kind of method that sugar-lowering components are extracted from Leaves of Hippophae L, according to following steps:
First, pre-treatment
By Leaves of Hippophae L through finishing, after drying, coarse powder is ground into, the boiling boiling of 15 times of meal quality is added, is cooled to room temperature, Obtain Leaves of Hippophae L pre-boiled liquid;
2nd, heat-insulation soaking
3wt% Daqu is added by the quality of pre-boiled liquid, mixes, 3 days is incubated under the conditions of 26-30 DEG C;
3rd, dry
Pre-boiled liquid after heat-insulation soaking is filtered, filter residue and drying obtains Leaves of Hippophae L powder, standby;
4th, extract
Ethanol extract in mass ratio:Leaves of Hippophae L powder=5:1 takes extract solution carries out refluxing extraction, temperature to Leaves of Hippophae L powder 80-90 DEG C, flow back 2 times;Extract solution is recovered under reduced pressure after refluxing extraction, obtains paste sea-buckthorn leaf extract;
The volumetric concentration of the ethanol extract is 95%.
Embodiment 2
A kind of method that sugar-lowering components are extracted from Leaves of Hippophae L, according to following steps:
First, pre-treatment
By Leaves of Hippophae L through finishing, after drying, coarse powder is ground into, the boiling boiling of 10 times of meal quality is added, is cooled to room temperature, Obtain Leaves of Hippophae L pre-boiled liquid;
2nd, heat-insulation soaking
2wt% Daqu is added by the quality of pre-boiled liquid, mixes, 5 days is incubated under the conditions of 30-35 DEG C;
3rd, dry
Pre-boiled liquid after heat-insulation soaking is filtered, filter residue and drying obtains Leaves of Hippophae L powder, standby;
4th, extract
Ethanol extract in mass ratio:Leaves of Hippophae L powder=5:1 takes extract solution carries out refluxing extraction, temperature to Leaves of Hippophae L powder 80-90 DEG C, flow back 3 times;Extract solution is recovered under reduced pressure after refluxing extraction, obtains paste sea-buckthorn leaf extract;
The volumetric concentration of the ethanol extract is 90%.
Embodiment 3
A kind of method that sugar-lowering components are extracted from Leaves of Hippophae L, according to following steps:
First, pre-treatment
By Leaves of Hippophae L through finishing, after drying, coarse powder is ground into, the boiling boiling of 20 times of meal quality is added, is cooled to room temperature, Obtain Leaves of Hippophae L pre-boiled liquid;
2nd, heat-insulation soaking
5wt% Daqu is added by the quality of pre-boiled liquid, mixes, 5 days is incubated under the conditions of 32-36 DEG C;
3rd, dry
Pre-boiled liquid after heat-insulation soaking is filtered, filter residue and drying obtains Leaves of Hippophae L powder, standby;
4th, extract
Methanol extract liquid in mass ratio:Leaves of Hippophae L powder=5:1 takes methanol extract liquid carries out refluxing extraction to Leaves of Hippophae L powder, Backflow 2 times;Methanol is recovered under reduced pressure after refluxing extraction, obtains paste sea-buckthorn leaf extract;
The methanol extract liquid is that the methanol for the volumetric concentration 85% being made into the NaOH solution and methanol of mass concentration 1% is molten Liquid.
Embodiment 4
A kind of method that sugar-lowering components are extracted from Leaves of Hippophae L, according to following steps:
First, pre-treatment
By Leaves of Hippophae L through finishing, after drying, coarse powder is ground into, the boiling boiling of 15 times of meal quality is added, is cooled to room temperature, Obtain Leaves of Hippophae L pre-boiled liquid;
2nd, heat-insulation soaking
1wt% Daqu is added by the quality of pre-boiled liquid, mixes, 5 days is incubated under the conditions of 32-36 DEG C;
3rd, dry
Pre-boiled liquid after heat-insulation soaking is filtered, filter residue and drying obtains Leaves of Hippophae L powder, standby;
4th, extract
Methanol extract liquid in mass ratio:Leaves of Hippophae L powder=5:1 takes methanol extract liquid carries out refluxing extraction to Leaves of Hippophae L powder, Backflow 2 times;Methanol is recovered under reduced pressure after refluxing extraction, obtains paste sea-buckthorn leaf extract;
The methanol extract liquid is that the methanol for the volumetric concentration 80% being made into the NaOH solution and methanol of mass concentration 1% is molten Liquid.
Embodiment 5
A kind of method that sugar-lowering components are extracted from Leaves of Hippophae L, according to following steps:
First, pre-treatment
By Leaves of Hippophae L through finishing, after drying, coarse powder is ground into, the boiling boiling of 13 times of meal quality is added, is cooled to room temperature, Obtain Leaves of Hippophae L pre-boiled liquid;
2nd, heat-insulation soaking
0.5wt% mixing enzyme preparations are added by the quality of pre-boiled liquid, mixes, 24 hours is incubated under the conditions of 28-32 DEG C;
3rd, dry
Pre-boiled liquid after heat-insulation soaking is filtered, filter residue and drying obtains Leaves of Hippophae L powder, standby;
4th, extract
Methanol extract liquid in mass ratio:Leaves of Hippophae L powder=5:1 takes methanol extract liquid carries out refluxing extraction to Leaves of Hippophae L powder, Backflow 2 times;Methanol is recovered under reduced pressure after refluxing extraction, obtains paste sea-buckthorn leaf extract;
The methanol extract liquid is the first for the volumetric concentration 80-90% being made into the NaOH solution and methanol of mass concentration 1% Alcoholic solution.
Embodiment 6
A kind of method that sugar-lowering components are extracted from Leaves of Hippophae L, according to following steps:
First, pre-treatment
By Leaves of Hippophae L through finishing, after drying, coarse powder is ground into, the boiling boiling of 18 times of meal quality is added, is cooled to room temperature, Obtain Leaves of Hippophae L pre-boiled liquid;
2nd, heat-insulation soaking
0.5wt% mixing enzyme preparations are added by the quality of pre-boiled liquid, mixes, 12 hours is incubated under the conditions of 35-38 DEG C;
3rd, dry
Pre-boiled liquid after heat-insulation soaking is filtered, filter residue and drying obtains Leaves of Hippophae L powder, standby;
4th, extract
Ethanol extract in mass ratio:Leaves of Hippophae L powder=5:1 takes extract solution carries out refluxing extraction, temperature to Leaves of Hippophae L powder 80-90 DEG C, flow back 3 times;Extract solution is recovered under reduced pressure after refluxing extraction, obtains paste sea-buckthorn leaf extract;
The volumetric concentration of the ethanol extract is 85%.
Embodiment 7
A kind of method that sugar-lowering components are extracted from Leaves of Hippophae L, according to following steps:
First, pre-treatment
By Leaves of Hippophae L through finishing, after drying, coarse powder is ground into, the boiling boiling of 14 times of meal quality is added, is cooled to room temperature, Obtain Leaves of Hippophae L pre-boiled liquid;
2nd, heat-insulation soaking
0.5wt% vinegars are added by the quality of pre-boiled liquid, are mixed, room temperature is placed 30 hours;
3rd, dry
Pre-boiled liquid after heat-insulation soaking is filtered, filter residue and drying obtains Leaves of Hippophae L powder, standby;
4th, extract
Methanol extract liquid in mass ratio:Leaves of Hippophae L powder=5:1 takes methanol extract liquid carries out refluxing extraction to Leaves of Hippophae L powder, Backflow 2 times;Methanol is recovered under reduced pressure after refluxing extraction, obtains paste sea-buckthorn leaf extract;
The methanol extract liquid is that the methanol for the volumetric concentration 83% being made into the NaOH solution and methanol of mass concentration 1% is molten Liquid.
Embodiment 8
A kind of method that sugar-lowering components are extracted from Leaves of Hippophae L, according to following steps:
First, pre-treatment
By Leaves of Hippophae L through finishing, after drying, coarse powder is ground into, the boiling boiling of 14 times of meal quality is added, is cooled to room temperature, Obtain Leaves of Hippophae L pre-boiled liquid;
2nd, heat-insulation soaking
1wt% vinegars are added by the quality of pre-boiled liquid, are mixed, room temperature is placed 18 hours;
3rd, dry
Pre-boiled liquid after heat-insulation soaking is filtered, filter residue and drying obtains Leaves of Hippophae L powder, standby;
4th, extract
Methanol extract liquid in mass ratio:Leaves of Hippophae L powder=5:1 takes methanol extract liquid carries out refluxing extraction to Leaves of Hippophae L powder, Backflow 3 times;Methanol is recovered under reduced pressure after refluxing extraction, obtains paste sea-buckthorn leaf extract;
The methanol extract liquid is that the methanol for the volumetric concentration 85% being made into the NaOH solution and methanol of mass concentration 1% is molten Liquid.
Embodiment 9
A kind of method that sugar-lowering components are extracted from Leaves of Hippophae L, according to following steps:
First, pre-treatment
By Leaves of Hippophae L through finishing, after drying, coarse powder is ground into, the boiling boiling of 14 times of meal quality is added, is cooled to room temperature, Obtain Leaves of Hippophae L pre-boiled liquid;
2nd, heat-insulation soaking
0.8wt% vinegars are added by the quality of pre-boiled liquid, are mixed, room temperature is placed 24 hours;
3rd, dry
Pre-boiled liquid after heat-insulation soaking is filtered, filter residue and drying obtains Leaves of Hippophae L powder, standby;
4th, extract
Methanol extract liquid in mass ratio:Leaves of Hippophae L powder=5:1 takes methanol extract liquid carries out refluxing extraction to Leaves of Hippophae L powder, Backflow 2 times;Methanol is recovered under reduced pressure after refluxing extraction, obtains paste sea-buckthorn leaf extract;
The methanol extract liquid is that the methanol for the volumetric concentration 86% being made into the NaOH solution and methanol of mass concentration 1% is molten Liquid.
Comparative example 1
A kind of method that sugar-lowering components are extracted from Leaves of Hippophae L, according to following steps:
Dry
Leaves of Hippophae L is finished, is dried to obtain sea-buckthorn leaf coarse powder;
Extraction
Ethanol extract in mass ratio:Sea-buckthorn leaf coarse powder=5:1, which takes extract solution, carries out refluxing extraction, temperature to Leaves of Hippophae L powder 80-90 DEG C of degree, flow back 2-3 times;Extract solution is recovered under reduced pressure after refluxing extraction, obtains paste sea-buckthorn leaf extract;
The volumetric concentration of the ethanol extract is 85-100%.
Comparative example 2
A kind of method that sugar-lowering components are extracted from Leaves of Hippophae L, according to following steps:
Dry
Leaves of Hippophae L is finished, is dried to obtain sea-buckthorn leaf coarse powder;
Extraction
Methanol extract liquid in mass ratio:Sea-buckthorn leaf coarse powder=5:1, which takes methanol extract liquid, carries out backflow to Leaves of Hippophae L powder and carries Take, 80-90 DEG C of temperature, flow back 2-3 times;Methanol is recovered under reduced pressure after refluxing extraction, obtains paste sea-buckthorn leaf extract;
The methanol extract liquid is the first for the volumetric concentration 80-90% being made into the NaOH solution and methanol of mass concentration 1% Alcoholic solution.
Corosolic acid comparision contents in gained paste extract in embodiment 1-6 and comparative example 1-2
Numbering Corosolic acid content(wt%) Numbering Corosolic acid content(wt%)
Embodiment 1 0.83 Embodiment 7 1.88
Embodiment 2 0.87 Embodiment 8 1.91
Embodiment 3 1.03 Embodiment 9 1.93
Embodiment 4 1.11 Comparative example 1 0.17
Embodiment 5 1.37 Comparative example 2 0.19
Embodiment 6 1.21
The present invention can be summarized with others without prejudice to the concrete form of the spirit or essential characteristics of the present invention.Therefore, nothing By from the point of view of which point, the embodiment above of the invention can only all be considered the description of the invention and can not limit invention, Claims indicate the scope of the present invention, and above-mentioned explanation does not point out the scope of the present invention, therefore, with the present invention The suitable implication and scope of claims in any change, be all considered as being included within the scope of the claims.

Claims (3)

  1. A kind of 1. method that sugar-lowering components are extracted from Leaves of Hippophae L, it is characterised in that according to following steps:
    First, pre-treatment
    By Leaves of Hippophae L through finishing, after drying, coarse powder is ground into, the boiling boiling of 10-20 times of meal quality is added, is cooled to room temperature, Obtain Leaves of Hippophae L pre-boiled liquid;
    2nd, heat-insulation soaking
    0.5-1wt% vinegars are added by the quality of pre-boiled liquid, are mixed, room temperature places 18-30 hours;
    3rd, dry
    Pre-boiled liquid after heat-insulation soaking is filtered, filter residue and drying obtains Leaves of Hippophae L powder, standby;
    4th, extract
    Extract solution in mass ratio:Leaves of Hippophae L powder=5:1 takes extract solution carries out refluxing extraction to Leaves of Hippophae L powder, flows back 2-3 times;Return Extract solution is recovered under reduced pressure after stream extraction, obtains paste sea-buckthorn leaf extract;
    The extract solution is ethanol extract or methanol extract liquid;
    The volumetric concentration of the ethanol extract is 85-100%, and palpus temperature conditionss is 80-90 DEG C when being extracted using ethanol extract;
    The methanol extract liquid is that the methanol for the volumetric concentration 80-90% being made into the NaOH solution and methanol of mass concentration 1% is molten Liquid.
  2. A kind of 2. method that sugar-lowering components are extracted from Leaves of Hippophae L according to claim 1, it is characterised in that:The step One and step 3 in the drying program that is related to, drying temperature is no more than 60 DEG C.
  3. A kind of 3. method that sugar-lowering components are extracted from Leaves of Hippophae L according to claim 1, it is characterised in that:By Leaves of Hippophae L Through finishing, after drying, the coarse powder of 20-60 mesh is ground into.
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CN108208793B (en) * 2017-12-18 2021-05-04 山西金海利生物科技有限公司 Preparation method of fermented sea buckthorn composition capable of improving intestinal immunity
CN110317239A (en) * 2019-08-13 2019-10-11 南京津奇生物科技有限公司 A kind of preparation method for extracting Corosolic acid from fructus hippophae
CN115530374A (en) * 2019-10-22 2022-12-30 内蒙古宇航人高技术产业有限责任公司 Sharpleaf quebracho extract and application thereof

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CN101274953B (en) * 2008-05-19 2012-05-09 福州大学 Method for extracting corosolic acid from plant
CN101434636B (en) * 2008-12-12 2011-06-29 桂林莱茵生物科技股份有限公司 Method for extracting corosolic acid from plant
CN103204894A (en) * 2012-12-25 2013-07-17 中国人民解放军海军医学研究所 Novel corosolic acid derivative, preparation method thereof and application thereof in preparing diabetes medicaments

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