CN105079050A - Method for preparing superfine powder of extract rich in ginkgo biloba seed polysaccharide - Google Patents
Method for preparing superfine powder of extract rich in ginkgo biloba seed polysaccharide Download PDFInfo
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Abstract
The invention belongs to the technical field of processing of food and Chinese medicinal materials, in particular to a method for preparing superfine powder of an extract rich in ginkgo biloba seed polysaccharide. The technical scheme disclosed by the invention lies in that ginkgo residue is taken as the raw material, processes such as cell disruption by utilizing microscale gas synergetic extrusion expansion, enzymatic hydrolysis with cellulose, microwave extraction at intermediate temperature, vacuum concentration, vacuum drying and two-stage superfine grinding and the like are adopted, therefore the superfine powder of the extract rich in ginkgo biloba seed polysaccharide is obtained. According to the method for extracting ginkgo biloba seed polysaccharide by taking the ginkgo residue as the raw material, provided by the invention, the resources are saved and the environmental pollution is reduced, besides, as the two-stage superfine grinding is performed on the extract rich in ginkgo biloba seed polysaccharide, the superfine powder of the extract is prepared, the dissolution, absorption and utilization of the extract are facilitated, and finally the utilization ratio of the extract is greatly improved.
Description
Technical field
The invention belongs to food and Chinese crude drug processing technique field, be specifically related to a kind of method preparing the extract superfine powder being rich in Semen Ginkgo polysaccharide.
Background technology
Semen Ginkgo (Gimkgobiloba) has another name called maidenhair tree, is Ginkgoaceae, Ginkgo deciduous tree.Ginkgo is distributed more widely in China, and be mainly distributed in the ground such as Jiangsu, Shandong, Guangxi, Yunnan, Guizhou, Sichuan, the abundance of China accounts for more than 70% of world's total amount.In recent years, along with the exploitation of gingko resource, China various places in a planned way expand the plantation of ginkgo.
Semen Ginkgo is the high natural plant resource of a kind of economic worth.Last century the mid-1960s, after German medical science man finds the multiple active ingredient containing diseases such as treatment cerebrovascular atherosclerosis, hypertension, diabetes in Folium Ginkgo, the production of Semen Ginkgo and application cause the concern of common people gradually.Be rich in the bioactive substance such as Folium Ginkgo terpene lactones, ginkgetin in Folium Ginkgo resource, wherein, Folium Ginkgo terpene lactones can effectively treat the diseases such as cerebral infarction, apoplexy, asthma; Ginkgetin has increases cardiovascular and cerebrovascular vessel flows, reduce cardiovascular and cerebrovascular vessel resistance, improve the functions such as vascular circulation, coronary artery dilator, scavenging free radicals, raising immunity, above-mentioned bioactive substance can be used for developing the health food that sick new Chinese medicine such as treatment coronary heart diseases and angina pectoris, hypertension etc. or health care are waited for a long time.Chinese patent application (publication No.: CN104031160A, title: Semen Ginkgo polysaccharide, method for extraction and purification and the application as tobacco humectant thereof) discloses a kind of Semen Ginkgo polysaccharide and method for extraction and purification thereof.This invention is that raw material adopts the Integration ofTechnology such as water extraction, precipitate with ethanol, enzymolysis, decolouring, dialysis to prepare the technique of Semen Ginkgo crude polysaccharides with Semen Ginkgo.
Chinese patent application (publication No.: CN102002112A, title: process for extracting ginkgo leaf polysaccharide with aid of ultrasonic) discloses a kind of process for extracting ginkgo leaf polysaccharide with aid of ultrasonic.The method adopts Folium Ginkgo to be raw material, drying, pulverize and sieve, supersound process, centrifugal, vacuum concentration, precipitate with ethanol, centrifugal, vacuum lyophilization, polysaccharide crude.
Can produce a large amount of waste residues extract flavone and terpenoid from Folium Ginkgo after, the overwhelming majority can abandon as garbage or burn, and both causes environmental pollution, and wastes again other active substances be rich in Semen Ginkgo slag.And in residue, be rich in the material such as Semen Ginkgo polysaccharide, flavone, particularly Semen Ginkgo polysaccharide is a kind of important bioactive substance, have non-specific immunity and anti-ageing many pharmacological actions of waiting for a long time, have important research and development and be worth, it mainly extracts from Folium Ginkgo or gingko episperm.
Consider Semen Ginkgo polysaccharide, flavone has above-mentioned special remarkable efficacy, be necessary to recycle above-mentioned Semen Ginkgo slag, and obtain the extract being rich in Semen Ginkgo polysaccharide.And the domestic research to Semen Ginkgo polysaccharide compounds extraction and isolation is less, extracting method mainly based on extraction, ultrasound wave extraction, ultrafiltration membrance filter, gel chromatography separation (such as,
jiang Bo, Wang Yanying, Liu Changjian, Liu Yubin, Ning Yanchao, Fan Sheng. " time precious traditional Chinese medical science traditional Chinese medicines ", 2007,18 (11): 2729-2731;
chen Qun, Yang Guiwen, Amway state. " Chinese Pharmaceutical Journal ", 2002,37 (5): 331-333).
But very few about the research report of the polysaccharide in the Semen Ginkgo slag extracted after flavone and terpenoid, the report applied in Folium Ginkgo extraction process about superfine communication technique is just less.
Summary of the invention
The object of the present invention is to provide a kind of method being rich in the extract superfine powder of Semen Ginkgo polysaccharide by the preparation of Semen Ginkgo slag, thus solution extracts polysaccharide and the obtained technical problem being conducive to the superfine powder absorbed from Semen Ginkgo slag.
To achieve these goals, technical scheme of the present invention provides a kind of method preparing the extract superfine powder being rich in Semen Ginkgo polysaccharide, and the method comprises the steps:
1) cell wall breaking: Semen Ginkgo slag (extracting the residue after the effective ingredient such as most of ginkgetin, bilobalide from Folium Ginkgo) is dried to water content and is less than 8%, then carry out micro-gas and work in coordination with extruding puffing cell wall breaking;
2) enzymolysis: the Semen Ginkgo slag after cell wall breaking is placed in enzymatic vessel, purified water is added by solid-liquid ratio 1:3 ~ 6 (w/v), and add the cellulase of Semen Ginkgo slag weight 0.2 ~ 0.6%, mixing, makes the Semen Ginkgo slag after cell wall breaking at temperature 36 ~ 42 DEG C, carry out the enzymolysis of 120 ~ 150min;
3) microwave extraction: add purified water and solid-liquid ratio is adjusted to 1:8 ~ 15 (w/v) in the feed liquid after enzymolysis, the temperature of initial feed liquid be 30 ~ 40 DEG C, under microwave power is 400 ~ 700W, each extraction time is the condition of 2 ~ 10min, above-mentioned feed liquid is extracted 2 ~ 3 times, more above-mentioned feed liquid is filtered and obtains filtrate;
4) vacuum concentration: carry out vacuum rotating to above-mentioned filtrate and concentrate, thickening temperature 55 ~ 75 DEG C, vacuum 0.06 ~ 0.07MPa, rotating speed 40 ~ 60r/min, is condensed into solid content;
5) vacuum drying: vacuum drying is carried out to above-mentioned solid content, baking temperature 50 ~ 70 DEG C, vacuum 0.07 ~ 0.08MPa, time 6 ~ 12h;
6) micronizing: adopt two-stage to pulverize integrated mode to the extract after above-mentioned vacuum drying and carry out micronizing.
Preferably, step 1) described in micro-gas be one or more in carbon dioxide, nitrogen and helium.In order to transport and measure conveniently, the step 1 in technique scheme) in the carbon dioxide that adopts be its solid-state form---dry ice, step 1) in the nitrogen, the helium that adopt be its liquid form---liquid nitrogen, liquid helium.
Preferably, step 2) in add the cellulase of Semen Ginkgo slag weight 0.3%.
Further preferably, the addition of described micro-gas is 0.03 ~ 0.05% (w/w) of Semen Ginkgo slag weight.
More preferably, 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.
Further preferably, step 6) described in two-stage to pulverize integrated mode be first adopt mechanical type super micron mill to pulverize, obtain 300 ~ 600 object extract superfine powder, pulverized by air-stream type ultrafine pulverizer again, obtain the extract superfine powder of more than 1000 orders.
Technique scheme of the present invention provide a kind of with Semen Ginkgo slag for raw material extracts the method for the extract of Semen Ginkgo polysaccharide of being rich in, save resource, decrease environmental pollution, and two-stage micronizing has been carried out to the extract being rich in Semen Ginkgo polysaccharide, thus obtained the superfine powder of this extract, be conducive to the dissolving of this extract like this and absorb, finally substantially increasing the utilization rate of extract.By the extract superfine powder being rich in Semen Ginkgo polysaccharide that preparation method provided by the invention obtains, for Semen Ginkgo polysaccharide content >=40% and the superfine powder of Ginkgo total flavones content >=10%.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described:
Embodiment 1
1) take 1kg Semen Ginkgo slag (water content 7.2%), carry out cell wall breaking by twin-screw extruder is expanded, in above-mentioned extruding puffing cell wall breaking process, add 0.4g dry ice work in coordination with;
2) cellulase is adopted to carry out enzymolysis: in enzymatic vessel, to add 4L purified water, 3g cellulase according to solid-liquid ratio 1:4 (w/v), controlled enzymatic hydrolysis temperature 39 DEG C, time 120min;
3) microwave extraction: add 6L purified water again, is adjusted to 1:10 (w/v) by solid-liquid ratio, control the temperature 35 DEG C of initial feed liquid, microwave power 600W, at every turn extraction time are 2min, extract 3 times, is filtered obtain filtrates by 120 mesh filter screens;
4) vacuum concentration: the temperature 70 C of concentrated filtrate, vacuum 0.06MPa, speed of agitator 50r/min, is condensed into solid content;
5) vacuum drying: dry temperature 60 C, vacuum 0.07MPa, time 10h;
6) micronizing: micronizing adopts two-stage combination pulverizing pattern, first adopt mechanical super micron mill can obtain the above superfine powder of 300 order, if again by comminution by gas stream, the superfine powder 138.6g of more than 1000 orders can be obtained, wherein Semen Ginkgo polysaccharide content 41.3%, Ginkgo total flavones content 10.2%.
Embodiment 2
1) take 1kg Semen Ginkgo slag (water content 8%), carry out cell wall breaking by twin-screw extruder is expanded, in above-mentioned extruding puffing cell wall breaking process, add 0.5g liquid nitrogen work in coordination with;
2) cellulase is adopted to carry out enzymolysis: in enzymatic vessel, to add 3L purified water, 2g cellulase according to solid-liquid ratio 1:3 (w/v), controlled enzymatic hydrolysis temperature 42 DEG C, time 150min;
3) microwave extraction: add 5L purified water again, is adjusted to 1:8 (w/v) by solid-liquid ratio, the temperature controlling initial feed liquid is 30 DEG C, microwave power 700W, at every turn extraction time are 5min, extract 2 times, is filtered obtain filtrates by 120 mesh filter screens;
4) vacuum concentration: the temperature of concentrated filtrate 75 DEG C, vacuum 0.07MPa, speed of agitator 60r/min, is condensed into solid content;
5) vacuum drying: dry temperature 50 C, vacuum 0.08MPa, time 12h;
6) micronizing: micronizing adopts two-stage combination pulverizing pattern, first adopt mechanical super micron mill can obtain the above superfine powder of 400 order, if again by comminution by gas stream, the superfine powder 141.8g of more than 1000 orders can be obtained, wherein Semen Ginkgo polysaccharide content 40.9%, Ginkgo total flavones content 10.5%.
Embodiment 3
1) take 1kg Semen Ginkgo slag (water content 7.2%), carry out cell wall breaking by twin-screw extruder is expanded, in above-mentioned extruding puffing cell wall breaking process, add 0.3g liquid helium work in coordination with;
2) cellulase is adopted to carry out enzymolysis: in enzymatic vessel, to add 6L purified water, 6g cellulase according to solid-liquid ratio 1:6 (w/v), controlled enzymatic hydrolysis temperature 36 DEG C, time 150min;
3) microwave extraction: add 9L purified water again, is adjusted to 1:15 (w/v) by solid-liquid ratio, the temperature controlling initial feed liquid is 40 DEG C, microwave power 400W, at every turn extraction time are 10min, extract 2 times, is filtered obtain filtrates by 120 mesh filter screens;
4) vacuum concentration: the temperature of concentrated filtrate 55 DEG C, vacuum 0.07MPa, speed of agitator 60r/min, is condensed into solid content;
5) vacuum drying: dry temperature 70 C, vacuum 0.08MPa, time 6h;
6) micronizing: micronizing adopts two-stage combination pulverizing pattern, first adopt mechanical super micron mill can obtain the above superfine powder of 600 order, if again by comminution by gas stream, the superfine powder 139.4g of more than 1000 orders can be obtained, wherein Semen Ginkgo polysaccharide content 42.1%, Ginkgo total flavones content 10.7%.
Assay is tested
1. adopt phenol-sulfuric acid and colorimetric method to measure Semen Ginkgo polysaccharide content
Get 3 increment product respectively in extract superfine powder obtained in embodiment 1 ~ 3, adopt the Semen Ginkgo polysaccharide content of phenol-sulfuric acid and colorimetric method to above-mentioned sample to measure, measurement result as shown in Table 1 below, is averaged:.
Table 1
2. the mensuration of Ginkgo total flavones content
3 increment product are got respectively in extract superfine powder obtained in embodiment 1 ~ 3, according to " Chinese Pharmacopoeia " annex V A medium ultraviolet-visible spectrophotometry, absorbance is measured at the wavelength place of 420nm, go out the content of Ginkgo total flavones in each sample as shown in Table 2 below according to standard curve regression equation calculation, average:
Table 2
Claims (7)
1. prepare a method for the extract superfine powder being rich in Semen Ginkgo polysaccharide, the method comprises the steps:
1) cell wall breaking: Semen Ginkgo slag is dried to water content and is less than 8%, then carry out micro-gas and work in coordination with extruding puffing cell wall breaking;
2) enzymolysis: the Semen Ginkgo slag after breaking cellular wall is placed in enzymatic vessel, purified water is added by solid-liquid ratio 1:3 ~ 6 (w/v), and add the cellulase of Semen Ginkgo slag weight 0.2 ~ 0.6%, mixing, makes the Semen Ginkgo slag after cell wall breaking at temperature 36 ~ 42 DEG C, carry out the enzymolysis of 120 ~ 150min;
3) microwave extraction: add purified water and solid-liquid ratio is adjusted to 1:8 ~ 15 (w/v) in the feed liquid after enzymolysis, the temperature of initial feed liquid be 30 ~ 40 DEG C, under microwave power is 400 ~ 700W, each extraction time is the condition of 2 ~ 10min, above-mentioned feed liquid is extracted 2 ~ 3 times, more above-mentioned feed liquid is filtered and obtains filtrate;
4) vacuum concentration: carry out vacuum rotating to above-mentioned filtrate and concentrate, thickening temperature 55 ~ 75 DEG C, vacuum 0.06 ~ 0.07MPa, rotating speed 40 ~ 60r/min, is condensed into solid content;
5) vacuum drying: vacuum drying is carried out to above-mentioned solid content, baking temperature 50 ~ 70 DEG C, vacuum 0.07 ~ 0.08MPa, time 6 ~ 12h;
6) micronizing: adopt two-stage to pulverize integrated mode to the extract after above-mentioned vacuum drying and carry out micronizing.
2. the method for the extract superfine powder of Semen Ginkgo polysaccharide is rich in preparation according to claim 1, it is characterized in that: step 1) described in micro-gas be one or more in carbon dioxide, nitrogen and helium.
3. the method for the extract superfine powder of Semen Ginkgo polysaccharide is rich in preparation according to claim 1, it is characterized in that: step 2) in add the cellulase of Semen Ginkgo slag weight 0.3%.
4. the method for the extract superfine powder of Semen Ginkgo polysaccharide is rich in preparation according to claim 1 and 2, it is characterized in that: the addition of described micro-gas is 0.03 ~ 0.05% (w/w) of Semen Ginkgo slag weight.
5. the method for the extract superfine powder of Semen Ginkgo polysaccharide is rich in preparation according to claim 3, it is characterized in that: the addition of described micro-gas is 0.04% (w/w) of Semen Ginkgo slag weight.
6. the method for the extract superfine powder of Semen Ginkgo polysaccharide is rich in preparation according to claim 1, it is characterized in that: step 3) described in microwave power be 600W.
7. the method for the extract superfine powder of Semen Ginkgo polysaccharide is rich in preparation according to claim 1, it is characterized in that: step 6) described in two-stage pulverize integrated mode be, mechanical type super micron mill is first adopted to pulverize, obtain 300 ~ 600 object extract superfine powder, pulverized by air-stream type ultrafine pulverizer again, obtain the extract superfine powder of more than 1000 orders.
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Cited By (5)
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| CN107669713A (en) * | 2017-11-17 | 2018-02-09 | 浙江工业大学上虞研究院有限公司 | A kind of extraction process of ginko leaves flavone class compound |
| 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 |
| CN109849148A (en) * | 2019-04-15 | 2019-06-07 | 吴勇 | A kind of preparation method of antimildew and antibacterial particle board |
| 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 |
| CN111019011A (en) * | 2019-12-31 | 2020-04-17 | 武汉轻工大学 | Method for extracting rice bran polysaccharide |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107669713A (en) * | 2017-11-17 | 2018-02-09 | 浙江工业大学上虞研究院有限公司 | A kind of extraction process of ginko leaves flavone class compound |
| 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 |
| CN109849148A (en) * | 2019-04-15 | 2019-06-07 | 吴勇 | A kind of preparation method of antimildew and antibacterial particle board |
| 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 |
| CN111019011A (en) * | 2019-12-31 | 2020-04-17 | 武汉轻工大学 | Method for extracting rice bran polysaccharide |
| CN111019011B (en) * | 2019-12-31 | 2021-08-10 | 武汉轻工大学 | Method for extracting rice bran polysaccharide |
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