CN105079050B - A kind of method preparing the extract superfine powder rich in Semen Ginkgo polysaccharide - Google Patents
A kind of method preparing the extract superfine powder rich in Semen Ginkgo polysaccharide Download PDFInfo
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Abstract
The invention belongs to food and Chinese crude drug processing technique field are and in particular to a kind of method preparing the extract superfine powder rich in Semen Ginkgo polysaccharide.Technical scheme disclosed by the invention is with Semen Ginkgo slag as raw material, extruding puffing cell wall breaking is worked in coordination with using micro- gas, cellulase degradation, the middle temperature of microwave are extracted, concentrated in vacuo, vacuum drying, two-stage micronizing etc., thus acquisition is rich in the extract superfine powder of Semen Ginkgo polysaccharide.The method that the present invention extracts polysaccharide with Semen Ginkgo slag for raw material, save resource, decrease environmental pollution, and two-stage micronizing has been carried out to the extract rich in Semen Ginkgo polysaccharide, thus the superfine powder of this extract has been obtained, so be conducive to the dissolving of this extract and absorb, finally substantially increase the utilization rate of extract.
Description
Technical field
The invention belongs to food and Chinese crude drug processing technique field are and in particular to a kind of extraction prepared rich in Semen Ginkgo polysaccharide
The method of thing superfine powder.
Background technology
Semen Ginkgo (Gimkgo biloba) also known as maidenhair tree, are Ginkgoaceae, Ginkgo deciduous tree.Ginkgo is divided in China
Cloth is wider, is distributed mainly on the ground such as Jiangsu, Shandong, Guangxi, Yunnan, Guizhou, Sichuan, and the abundance of China accounts for world's total amount
More than 70%.In recent years, with the exploitation of gingko resource, China various places in a planned way expand the plantation of ginkgo.
Semen Ginkgo is a kind of high natural plant resource of economic worth.Last century the mid-1960s, German medical science man
After finding to contain multiple active ingredient of disease such as treatment cerebrovascular atherosclerosis, hypertension, diabetes in Folium Ginkgo, silver
The production of Fructus Pruni and application gradually cause the concern of common people.It is rich in Folium Ginkgo terpene lactoness, ginkgetin etc. biological alive in Folium Ginkgo resource
Property material, wherein, Folium Ginkgo terpene lactoness can the disease such as effectively treatment cerebral infarction, apoplexy, asthma；Ginkgetin has increase heart and brain
Vascular flow, reduce cardiovascular and cerebrovascular vessel resistance, improve vascular circulation, coronary artery dilator, remove free radical, the work(such as enhance immunity
Can, above-mentioned bioactive substance can be used for developing new Chinese medicine or the health care of the diseases such as treatment coronary heart diseases and angina pectoris, hypertension
The health food waited for a long time.Chinese patent application (publication No.：CN104031160A, title：Semen Ginkgo polysaccharide, method for extraction and purification and
It is as the application of tobacco humectant) disclose a kind of Semen Ginkgo polysaccharide and its method for extraction and purification.This invention is with Semen Ginkgo as raw material
The technique that Semen Ginkgo crude polysaccharides are prepared using Integration ofTechnology such as water extraction, precipitate with ethanol, enzymolysis, decolouring, dialysis.
Chinese patent application (publication No.：CN102002112A, title：Process for extracting ginkgo leaf polysaccharide with aid of ultrasonic) public
Open a kind of process for extracting ginkgo leaf polysaccharide with aid of ultrasonic.The method adopt Folium Ginkgo be raw material, drying, pulverize and sieve,
Supersound process, centrifugation, concentrated in vacuo, precipitate with ethanol, centrifugation, vacuum lyophilization, polysaccharide crude.
Substantial amounts of waste residue can be produced, the overwhelming majority can be used as garbage after extracting flavone and terpenoid from Folium Ginkgo
Abandon or burn, both caused environmental pollution, and wasted other active substances being rich in Semen Ginkgo slag again.And in residue, it is rich in Semen Ginkgo
The materials such as polysaccharide, flavone, particularly Semen Ginkgo polysaccharide are a kind of important bioactive substances, have non-specific immunity with
Anti-ageing many pharmacological actions of waiting for a long time, have important research and development and are worth, it mainly carries from Folium Ginkgo or gingko episperm
Take.
There is above-mentioned special remarkable efficacy it is necessary to reclaim to above-mentioned Semen Ginkgo slag in view of Semen Ginkgo polysaccharide, flavone
Using, and obtain the extract rich in Semen Ginkgo polysaccharide.And domestic less to the detached research of Semen Ginkgo polysaccharide class compound extraction, carry
Take method mainly based on extraction, ultrasound wave extraction, ultrafiltration membrance filter, gel chromatography separation (for example,Jiang Bo,
Wang Yanying, Liu Changjian, Liu Yubin, Ning Yanchao, Fan Sheng.《When precious traditional Chinese medical science traditional Chinese medicines》, 2007,18 (11)：2729-2731；Old
Group, Yang Guiwen, Amway state.《Chinese Pharmaceutical Journal》, 2002,37 (5):331-333).
But, the research report with regard to extracting the polysaccharide in the Semen Ginkgo slag after flavone and terpenoid is very few, with regard to super
The report that Crushing of Ultrafine technology is applied in Folium Ginkgo extraction process is just less.
Content of the invention
It is an object of the invention to provide a kind of method by the preparation of Semen Ginkgo slag rich in the extract superfine powder of Semen Ginkgo polysaccharide,
Thus solving to extract polysaccharide from Semen Ginkgo slag and the technical problem of the superfine powder that be conducive to absorb is obtained.
To achieve these goals, technical scheme provides a kind of extract prepared rich in Semen Ginkgo polysaccharide and surpasses
The method of micropowder, the method comprises the steps：
1) cell wall breaking：Semen Ginkgo slag (is extracted the effective ingredient such as most of ginkgetin, bilobalide from Folium Ginkgo
Residue afterwards) it is dried to water content less than 8%, then carry out the collaborative extruding puffing cell wall breaking of micro- gas；
2) digest：Semen Ginkgo slag after cell wall breaking is placed in enzymatic vessel, by solid-liquid ratio 1:3～6 (w/v) adds purification
Water, and add the cellulase of Semen Ginkgo slag weight 0.2～0.6%, mix, make the Semen Ginkgo slag after cell wall breaking in temperature 36～42
Carry out the enzymolysis of 120～150min at DEG C；
3) microwave extraction：Add purified water in the feed liquid after enzymolysis and solid-liquid ratio is adjusted to 1:8～15 (w/v), in starting material
The temperature of liquid be 30～40 DEG C, microwave power be 400～700W, each extraction time be 2～10min under conditions of, to above-mentioned
Feed liquid is extracted 2～3 times, more above-mentioned feed liquid is filtered and is obtained filtrate；
4) concentrated in vacuo：Above-mentioned filtrate is carried out with vacuum rotating concentration, 55～75 DEG C of thickening temperature, vacuum 0.06～
0.07MPa, rotating speed 40～60r/min, are condensed into solid content；
5) it is vacuum dried：Above-mentioned solid content is vacuum dried, 50～70 DEG C of baking temperature, vacuum 0.07～
0.08MPa, time 6～12h；
6) micronizing：Using two-stage, integrated mode is pulverized to the extract after above-mentioned vacuum drying and carries out micronizing.
Preferably, step 1) described in micro- gas be one or more of carbon dioxide, nitrogen and helium.In order to transport
And measure conveniently, in the step 1 of technique scheme) employed in carbon dioxide be its solid-state form dry ice, step
Nitrogen employed in rapid 1), helium are its liquid form liquid nitrogen, liquid helium.
Preferably, step 2) the middle cellulase adding Semen Ginkgo slag weight 0.3%.
It is further preferred that the addition of described micro- gas is 0.03～0.05% (w/w) of Semen Ginkgo slag weight.
It is highly preferred that the addition of described micro- gas is 0.04% (w/w) of Semen Ginkgo slag weight.
Preferably, step 3) described in microwave power be 600W.
It is further preferred that step 6) described in two-stage to pulverize integrated mode be first to adopt mechanical type super micron mill
Pulverized, obtain the extract superfine powder of 300～600 mesh, then pulverized by air-stream type ultrafine pulverizer, obtained 1000
Extract superfine powder more than mesh.
The technique scheme of the present invention provides a kind of extract extracting rich in Semen Ginkgo polysaccharide with Semen Ginkgo slag for raw material
Method, saved resource, decreased environmental pollution, and two-stage micronizing has been carried out to the extract rich in Semen Ginkgo polysaccharide,
Thus the superfine powder of this extract has been obtained, is so conducive to the dissolving of this extract and absorbs, finally substantially increase
The utilization rate of extract.The extract superfine powder rich in Semen Ginkgo polysaccharide being obtained by the preparation method that the present invention provides, for silver
Fructus Pruni polyoses content >=40% and the superfine powder of Ginkgo total flavones content >=10%.
Specific embodiment
With reference to specific embodiment, the invention will be further described：
Embodiment 1
1) weigh 1kg Semen Ginkgo slag (water content 7.2%), carry out cell wall breaking by twin-screw extruder is expanded, in above-mentioned extruding
Add 0.4g dry ice during expanded cell wall breaking to work in coordination with；
2) digested using cellulase：In enzymatic vessel, according to solid-liquid ratio 1:4 (w/v) adds 4L purified water, 3g fibre
The plain enzyme of dimension, 39 DEG C of controlled enzymatic hydrolysis temperature, time 120min；
3) microwave extraction：Add 6L purified water again, solid-liquid ratio is adjusted to 1:10 (w/v), control the temperature 35 of initial feed liquid
DEG C, microwave power 600W, each extraction time be 2min, extract 3 times, by 120 mesh filter screens filter obtain filtrates；
4) concentrated in vacuo：Concentrate the temperature 70 C of filtrate, vacuum 0.06MPa, speed of agitator 50r/min, be condensed into solid
Shape thing；
5) it is vacuum dried：The temperature 60 C being dried, vacuum 0.07MPa, time 10h；
6) micronizing：Micronizing adopts two-stage to combine pulverizing pattern, first can obtain 300 using mechanical super micron mill
The above superfine powder of mesh, if passing through comminution by gas stream again, can obtain the superfine powder 138.6g of more than 1000 mesh, wherein Semen Ginkgo polysaccharide content
41.3%th, Ginkgo total flavones content 10.2%.
Embodiment 2
1) weigh 1kg Semen Ginkgo slag (water content 8%), carry out cell wall breaking by twin-screw extruder is expanded, swollen in above-mentioned extruding
Add 0.5g liquid nitrogen during changing cell wall breaking to work in coordination with；
2) digested using cellulase：In enzymatic vessel, according to solid-liquid ratio 1:3 (w/v) adds 3L purified water, 2g fibre
The plain enzyme of dimension, 42 DEG C of controlled enzymatic hydrolysis temperature, time 150min；
3) microwave extraction：Add 5L purified water again, solid-liquid ratio is adjusted to 1:8 (w/v), the temperature controlling initial feed liquid is 30
DEG C, microwave power 700W, each extraction time be 5min, extract 2 times, by 120 mesh filter screens filter obtain filtrates；
4) concentrated in vacuo：Concentrate 75 DEG C of the temperature of filtrate, vacuum 0.07MPa, speed of agitator 60r/min, be condensed into solid
Shape thing；
5) it is vacuum dried：The temperature 50 C being dried, vacuum 0.08MPa, time 12h；
6) micronizing：Micronizing adopts two-stage to combine pulverizing pattern, first can obtain 400 using mechanical super micron mill
The above superfine powder of mesh, if passing through comminution by gas stream again, can obtain the superfine powder 141.8g of more than 1000 mesh, wherein Semen Ginkgo polysaccharide content
40.9%th, Ginkgo total flavones content 10.5%.
Embodiment 3
1) weigh 1kg Semen Ginkgo slag (water content 7.2%), carry out cell wall breaking by twin-screw extruder is expanded, in above-mentioned extruding
Add 0.3g liquid helium during expanded cell wall breaking to work in coordination with；
2) digested using cellulase：In enzymatic vessel, according to solid-liquid ratio 1:6 (w/v) adds 6L purified water, 6g fibre
The plain enzyme of dimension, 36 DEG C of controlled enzymatic hydrolysis temperature, time 150min；
3) microwave extraction：Add 9L purified water again, solid-liquid ratio is adjusted to 1:15 (w/v), the temperature controlling initial feed liquid is
40 DEG C, microwave power 400W, each extraction time be 10min, extract 2 times, by 120 mesh filter screens filter obtain filtrates；
4) concentrated in vacuo：Concentrate 55 DEG C of the temperature of filtrate, vacuum 0.07MPa, speed of agitator 60r/min, be condensed into solid
Shape thing；
5) it is vacuum dried：The temperature 70 C being dried, vacuum 0.08MPa, time 6h；
6) micronizing：Micronizing adopts two-stage to combine pulverizing pattern, first can obtain 600 using mechanical super micron mill
The above superfine powder of mesh, if passing through comminution by gas stream again, can obtain the superfine powder 139.4g of more than 1000 mesh, wherein Semen Ginkgo polysaccharide content
42.1%th, Ginkgo total flavones content 10.7%.
Assay is tested
1. using phenol-sulfuric acid and colorimetric method, Semen Ginkgo polysaccharide content is measured
3 parts of samples are taken respectively, using phenol-sulfuric acid and colorimetric method pair in the extract superfine powder being obtained in embodiment 1 ~ 3
The Semen Ginkgo polysaccharide content of above-mentioned sample is measured, and measurement result as shown in Table 1 below, is averaged：.
Table 1
2. the mensure of Ginkgo total flavones content
3 parts of samples are taken respectively in the extract superfine powder being obtained in embodiment 1 ~ 3, according to《Chinese Pharmacopoeia》One annex
Ultraviolet visible spectrophotometry in V A, mensuration absorbance at the wavelength of 420nm, according to standard curve regression equation calculation
Go out the content of Ginkgo total flavones in each sample as shown in Table 2 below, average：
Table 2
Claims (1)
1. a kind of method preparing the extract superfine powder rich in Semen Ginkgo polysaccharide is it is characterised in that step is：
1) weigh 1kg Semen Ginkgo slag, carry out cell wall breaking by twin-screw extruder is expanded, in above-mentioned extruding puffing cell wall breaking process
Middle interpolation 0.3g liquid helium is worked in coordination with；
2) digested using cellulase：In enzymatic vessel, add 6L purified water, 6g cellulose according to solid-liquid ratio 1: 6 (w/v)
Enzyme, 36 DEG C of controlled enzymatic hydrolysis temperature, time 150min；
3) microwave extraction：Add 9L purified water again, solid-liquid ratio is adjusted to 1: 15 (w/v), control the temperature initiateing feed liquid to be 40 DEG C,
Microwave power 400W, each extraction time are 10min, extract 2 times, are filtered by 120 mesh filter screens and obtain filtrate；
4) concentrated in vacuo：Concentrate 55 DEG C of the temperature of filtrate, vacuum 0.07MPa, speed of agitator 60r/min, be condensed into solid content；
5) it is vacuum dried：The temperature 70 C being dried, vacuum 0.08MPa, time 6h；
6) micronizing：Micronizing adopt two-stage combine pulverizing pattern, first adopt mechanical super micron mill can obtain 600 mesh with
Upper superfine powder, if passing through comminution by gas stream again, can obtain the superfine powder 139.4g of more than 1000 mesh, wherein Semen Ginkgo polysaccharide content
42.1%th, Ginkgo total flavones content 10.7%.
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| CN108451988A (en) * | 2018-04-17 | 2018-08-28 | 合肥工业大学 | A kind of preparation method of highly-water-soluble ginkgo biloba p.e |
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| CN110558509A (en) * | 2019-10-14 | 2019-12-13 | 上海夜草生物科技有限公司 | Preparation method of fruit powder containing fructus momordicae |
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