A kind of method of shelling of the lucidum spore powder for improving effect
Technical field
The invention belongs to Chinese herbal medicine manufacture field, and in particular to a kind of method of shelling of the lucidum spore powder of raising effect,
The method is included Reishi sporule powder raw material by grinding and separating step, spray drying step, Reishi sporule after being shelled
Powder.
Background technology
Ganoderma lucidum (Ganoderma lucidum) belongs to fungi for Basidiomycetes Polyporaceae, is a kind of extensive medicinal effect
Fungi.Wherein, Reishi sporule is brown, avette, has double-wall structure.From eucaryotic cell structure, the double-wall structure, by chitin
Matter and glucose are constituted, and quality is more tough and tensile, hinder the dissolution of active ingredient, influence body absorption.Therefore it is most at present
Product all crushes conidial cell wall using different technology for broken wall, and to improve bioavilability in active component body, curative effect is controlled in enhancing
Really.But chitin is still mixed with active ingredient in wall after broken wall, the polysaccharide and triterpene content of final products are influenceed.Existing
In some ganoderma lucidium spore powder wall breaking methods, the polysaccharide of obtained lucidum spore powder and the content of triterpene are only 1.5-1.8%.This
Outward, the particularly patient of some disease of digestive tracts, after they take ganoderma spove powder relatively largely, it tends to be difficult to digestion spirit
The housing of Ganoderma lucidum spore powder, causes indigestion even to influence the negative effect of feed.
So, a kind of method for needing double-wall structure by lucidum spore powder to remove (shelling) at present, raising is shelled
The yield of lucidum spore powder, while improving polysaccharide therein and triterpene content.
The content of the invention
The present invention provides a kind of method of shelling of the lucidum spore powder for improving effect, and the method is included wall-broken ganoderma spore
Powder raw material through over grinding step, through water dilution and centrifugation shell meat, the step such as shell, concentrate and be spray-dried, shelled
Lucidum spore powder afterwards.Product meat content of the present invention is high, and polysaccharide and triterpene content are high.
The present invention is achieved by the following technical solutions:
A kind of method of shelling of the lucidum spore powder for improving effect, the method for shelling includes:By Reishi sporule powder raw material
By grinding and separating step, spray drying step, lucidum spore powder after being shelled.
Further, it is described grinding and separating step include it is following step by step:
First order grinding is separated step by step:
Reishi sporule powder raw material and water are mixed, treatment is ground, the product after first order grinding is obtained;Again will be described
Product after first order grinding carries out centrifugal treating, obtains supernatant and sediment;The supernatant is carried out into filtration treatment again,
Retain filtrate;
Second level grinding is separated step by step:
The sediment and water are mixed, treatment, filtration treatment is ground, retains filtrate.
Further, during the first order grinding is separated step by step, the Reishi sporule powder raw material is with the weight ratio of water
1:(3-6);The milled processed uses nanoscale colloid mill, is ground to more than 850 mesh, grinds 1-4 times;The centrifugal treating
Rotating speed is 4000-10000rpm, and the time is 10-40min;The filtration treatment uses the filter screen of 800-1000 mesh.
Further, during the second level grinding is separated step by step, the sediment is 1 with the weight ratio of water:(3-6);
The milled processed uses nanoscale colloid mill, is ground to more than 850 mesh, grinds 1-4 times;The filtration treatment uses 800-
The filter screen of 1000 mesh.
Further, the spray drying step includes:Merge the first order grinding separation to be ground with the second level step by step
Mill separates the filtrate for obtaining step by step, then carries out concentration, spray drying treatment, obtains the lucidum spore powder that shells.
Further, the concentration is carried out under vacuo, and temperature is 70-85 DEG C, be concentrated into (1/2) of original volume-
(2/3);The nozzle temperature of the spray drying treatment is 120-130 DEG C.
Further, the preparation method of the Reishi sporule powder raw material is comprised the following steps:By lucidum spore powder and proportion
After water is mixed, mixture is obtained;The mixture is carried out into precipitation process again, with different levels mixture is obtained;Described point is taken again
The intermediate layer of the mixture of level;The intermediate layer is carried out into concentration again, enriched product is obtained;The enriched product conduct
Reishi sporule powder raw material.
Further, the lucidum spore powder and than heavy water weight ratio be 1:(6-11);Described is quality hundred than heavy water
Divide the sodium chloride solution than 10-30%;The time of the precipitation process is 2-10 minutes;The concentration is entered under vacuo
OK, temperature is 70-85 DEG C, and the volume of the enriched product is (1/2)-(2/3) of original volume.
Further, the preparation method of the Reishi sporule powder raw material is further comprising the steps of:
The enriched product is carried out into drying and processing, Reishi sporule powder raw material is obtained.
Further, the temperature of the drying and processing is 60-90 DEG C.
Compared to existing technology, the present invention has the advantages that:
1st, the present invention partially or completely removes the double-wall structure (i.e. shell) of lucidum spore powder, is conducive to active component to fill
Point discharge and be absorbed by the body, it is to avoid be difficult to the side effect of the housing that digests to Patients With Digestive Tract Diseases.
2nd, lucidum spore powder is carried out many heavy cuttings by the present invention, not only contributes to releasing for lucidum spore powder inside active ingredient
Put, be also beneficial to the extraction of active ingredient in lucidum spore powder outer wall, be conducive to improving polysaccharide and triterpene content.
3rd, other new reagents are not introduced substantially in addition to deionized water in broken wall of the invention, step of shelling, can be true
Protect the high-purity of ganoderma spove powder.
4th, each step of the invention and parameter synergy, improve the yield of lucidum spore powder Raw material processing, many jointly
The content of sugar and triterpene.
5th, easy to operate, low production cost of the invention, is conducive to widely using.
Specific embodiment
The present invention provides a kind of method of shelling of the lucidum spore powder for improving effect, and the method for shelling is comprised the following steps:
Step one, precipitation and concentration:
Collect lucidum spore powder, will be added in the lucidum spore powder than heavy water (this than heavy water be sodium chloride solution, quality hundred
Point concentration is 10-30% (preferably 20%)), wherein, lucidum spore powder and be 1 than the weight ratio of heavy water:(6-11) (preferably
1:7), mixture is obtained after mixing;The mixture is carried out into precipitation process 2-10 minutes (preferably 5 minutes) in room temperature, is obtained
With different levels mixture;In with different levels mixture, upper strata is the flat grain of lucidum spore powder, and intermediate layer is lucidum spore powder
Grain, lower floor is the impurity such as silt;Removal the upper and lower, take the intermediate layer of the mixture;
The Reishi sporule powder raw material in the intermediate layer is carried out into concentration again, enriched product is obtained after treatment, as ganoderma lucidum
Spore powder raw material carries out the grinding of next step;The concentration is carried out under vacuo, and temperature is 70-85 DEG C, is concentrated into substance
Long-pending (1/2)-(2/3);
The enriched product can also carry out drying and processing then at 60-90 DEG C, to (the preferably 6- of water content more than 5%
9%) grinding of next step, is carried out as glossy ganoderma powder spore powder raw material.
Exemplarily, above-mentioned lucidum spore powder and the weight ratio than heavy water can be 1:6、1:7、1:7.5、1:8、1:10、
1:Arbitrary value or any scope between the two in 11 grades, the above-mentioned sedimentation time can be in 2min, 5min, 8min, 10min etc.
Arbitrary value or any scope between the two, the temperature of above-mentioned concentration can be 70 DEG C, 75 DEG C, 80 DEG C, the middle arbitrary values such as 85 DEG C
Or any scope between the two, the volume after above-mentioned concentration can be the middle arbitrary value such as 1/2,3/5,2/3 of original volume or appoint
Meaning scope between the two.
Step 2, grinding and separation:
Step by step one, first order grinding is separated:
By above-mentioned Reishi sporule powder raw material and deionized water by weight 1:(3-6) (preferably 1:4) mix, using nanometer
Level colloid mill is ground treatment, and grinding 1-4 to more than 850 mesh, obtains the product after first order grinding all over (preferably 2 times);
Product after the first order is ground again carries out centrifugal treating in room temperature, rotating speed 4000-10000rpm (preferably 5800rpm)
10-40min, retains the supernatant and sediment for obtaining respectively;The supernatant is used into 800-1000 mesh (preferably 800 again
Mesh) filter screen carry out filtration treatment after, retain filtrate.
Exemplarily, above-mentioned Reishi sporule powder raw material can be 1 with deionized water by weight:3、1:4、1:5、1:6 etc.
Middle arbitrary value or any scope between the two, the pass of above-mentioned grinding can for the middle arbitrary values such as 2,3,4 or it is any both it
Between scope, above-mentioned centrifugal rotational speed can be the middle arbitrary value such as 4000rpm, 5000rpm, 6000rpm, 8000rpm, 10000rpm
Or any scope between the two, above-mentioned centrifugation time for middle arbitrary values such as 10min, 20min, 30min, 40min or can appoint
Meaning scope between the two, the mesh number of above-mentioned filter screen can for the middle arbitrary values such as 800,850,900,950,1000 or it is any both
Between scope.
Step by step two, second level grinding is separated:
By above-mentioned sediment and deionized water by weight 1:(3-6) (preferably 1:6) mix, again using nanoscale glue
Body mill is ground treatment, and grinding 1-4 to more than 850 mesh, obtains the product after the grinding of the second level all over (preferably 2 times);Again will
Product after the grinding of the second level carries out filtration treatment with the filter screen of 800-1000 mesh (preferably 800 mesh), retains filtrate.
Exemplarily, above-mentioned sediment can be 1 with deionized water by weight:3、1:4、1:5、1:Arbitrary value in 6 grades
Or any scope between the two, the pass of above-mentioned grinding can be the middle arbitrary values such as 2,3,4 or any scope between the two,
The mesh number of above-mentioned filter screen can be the middle arbitrary values such as 800,850,900,950,1000 or any scope between the two.
Above-mentioned nanoscale colloid mill is preferably preferably IKN board CMS2000 types nano-colloid mill using nano-colloid mill, excellent
Choose from Shanghai Yi Ken plant equipment Co., Ltd.
Step 3, spray drying:
The filtrate (the as aqueous solution of lucidum spore powder content) obtained after above-mentioned two-stage is ground merges,
Concentration is carried out in 70-85 DEG C (preferably 80 DEG C) under vacuum environment, concentrate is obtained, to (1/2) of original volume-(2/3)
(preferably 1/2), spray drying treatment is carried out then at nozzle temperature 120-130 DEG C (preferably 125 DEG C), obtains the ganoderma lucidum spore that shells
Sub- powder.
The concentration preferably uses vacuum concentration pot.
Exemplarily, the temperature of above-mentioned concentration can for 70 DEG C, 75 DEG C, 80 DEG C, the middle arbitrary values such as 85 DEG C or it is any both
Between scope, above-mentioned concentrate can be to the 1/2 of original volume, 3/5,2/3 etc. middle arbitrary value or any model between the two
Enclose, the nozzle temperature of above-mentioned spray drying can be 120 DEG C, 123 DEG C, 125 DEG C, 128 DEG C, the middle arbitrary values such as 130 DEG C or any
Scope between the two.
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments be only used for the present invention without
For limiting the scope of the present invention.Externally it should be understood that after present disclosure has been read, those skilled in the art are to this hair
Bright to make various changes or modifications, these equivalent form of values equally fall within the application appended claims limited range.
Embodiment 1
The method of shelling of the lucidum spore powder of the present embodiment, comprises the following steps successively:
(1) lucidum spore powder is collected.
(2) will be added than heavy water in the lucidum spore powder, wherein, lucidum spore powder and (25% sodium chloride is molten than heavy water
Liquid) weight ratio be 1:8, mixture is obtained after mixing;The mixture is carried out into precipitation process 5 minutes in room temperature again, is divided
The mixture of level, takes its intermediate layer;The intermediate layer is carried out into concentration to original volume in 80 DEG C under vacuum conditions again
3/5, as Reishi sporule powder raw material.
(3) by the Reishi sporule powder raw material and deionized water by weight 1:6 mix, and are ground using nanoscale colloid mill
Mill treatment, grinds 2 times, to more than 850 mesh, obtains the product after first order grinding.
(4) product after the first order is ground carries out centrifugal treating 30min in room temperature, rotating speed 5800rpm, retains respectively
The supernatant and sediment for obtaining.
(5) supernatant is taken, after carrying out filtration treatment using the filter screen of 800 mesh, retains filtrate.
(6) sediment is taken, with deionized water by weight 1:6 are mixed, and treatment is ground using nanoscale colloid mill,
Grinding 2 times, to more than 850 mesh, obtains the product after the grinding of the second level.
(7) product after the second level is ground carries out filtration treatment with the filter screen of 800 mesh, retains filtrate.
(8) filtrate that combining step (5) and step (7) are obtained, the filtrate is the aqueous solution of lucidum spore powder content.
(9) carry out concentration in 80 DEG C under vacuum conditions and obtain concentrate, to the 3/5 of original volume.
(10) concentrate is carried out into spray drying treatment for 125 DEG C in nozzle temperature, obtains the lucidum spore powder that shells.
(11) by the lucidum spore powder packaging of aluminium foil bag that shells, storage storage.
On the premise of polyoses content 4.2-4.5%, triterpene content 5-5.8%, yield is the above-mentioned lucidum spore powder that shells
15-20%.
Embodiment 2
The method of shelling of the lucidum spore powder of the present embodiment, comprises the following steps successively:
(1) lucidum spore powder is collected.
(2) will be added than heavy water in the lucidum spore powder, wherein, lucidum spore powder and (10% sodium chloride is molten than heavy water
Liquid) weight ratio be 1:10, mixture is obtained after mixing;The mixture is carried out into precipitation process 5 minutes in room temperature again, is divided
The mixture of level, takes its intermediate layer;The intermediate layer is carried out into concentration to original volume in 70 DEG C under vacuum conditions again
1/2, as Reishi sporule powder raw material.
(3) by the Reishi sporule powder raw material and deionized water by weight 1:3 mix, and are ground using nanoscale colloid mill
Mill treatment, grinds 4 times, to more than 850 mesh, obtains the product after first order grinding.
(4) product after the first order is ground carries out centrifugal treating 40min in room temperature, rotating speed 4000rpm, retains respectively
The supernatant and sediment for obtaining.
(5) supernatant is taken, after carrying out filtration treatment using the filter screen of 1000 mesh, retains filtrate.
(6) sediment is taken, with deionized water by weight 1:3 are mixed, and treatment is ground using nanoscale colloid mill,
Grinding 2 times, to more than 850 mesh, obtains the product after the grinding of the second level.
(7) product after the second level is ground carries out filtration treatment with the filter screen of 1000 mesh, retains filtrate.
(8) filtrate that combining step (5) and step (7) are obtained, the filtrate is the aqueous solution of lucidum spore powder content.
(9) carry out concentration in 70 DEG C under vacuum conditions and obtain concentrate, to the 1/2 of original volume.
(10) concentrate is carried out into spray drying treatment for 120 DEG C in nozzle temperature, obtains the lucidum spore powder that shells.
(11) by the lucidum spore powder packaging of aluminium foil bag that shells, storage storage.
On the premise of polyoses content 4.2-4.5%, triterpene content 5-5.8%, yield is the above-mentioned lucidum spore powder that shells
15-20%.
Embodiment 3
The method of shelling of the lucidum spore powder of the present embodiment, comprises the following steps successively:
(1) lucidum spore powder is collected.
(2) will be added than heavy water in the lucidum spore powder, wherein, lucidum spore powder and (25% sodium chloride is molten than heavy water
Liquid) weight ratio be 1:11, mixture is obtained after mixing;The mixture is carried out into precipitation process 10 minutes in room temperature again, is obtained
With different levels mixture, takes its intermediate layer;The intermediate layer is carried out into concentration to original volume in 85 DEG C under vacuum conditions again
2/3, as Reishi sporule powder raw material.
(3) by the Reishi sporule powder raw material and deionized water by weight 1:4 mix, and are ground using nanoscale colloid mill
Mill treatment, grinds 3 times, to more than 850 mesh, obtains the product after first order grinding.
(4) product after the first order is ground carries out centrifugal treating 10min in room temperature, rotating speed 10000rpm, protects respectively
Stay the supernatant and sediment for obtaining.
(5) supernatant is taken, after carrying out filtration treatment using the filter screen of 900 mesh, retains filtrate.
(6) sediment is taken, with deionized water by weight 1:4 are mixed, and treatment is ground using nanoscale colloid mill,
Grinding 2 times, to more than 850 mesh, obtains the product after the grinding of the second level.
(7) product after the second level is ground carries out filtration treatment with the filter screen of 1000 mesh, retains filtrate.
(8) filtrate that combining step (5) and step (7) are obtained, the filtrate is the aqueous solution of lucidum spore powder content.
(9) carry out concentration in 85 DEG C under vacuum conditions and obtain concentrate, to the 2/3 of original volume.
(10) concentrate is carried out into spray drying treatment for 130 DEG C in nozzle temperature, obtains the lucidum spore powder that shells.
(11) by the lucidum spore powder packaging of aluminium foil bag that shells, storage storage.
On the premise of polyoses content 4.2-4.5%, triterpene content 5-5.8%, yield is the above-mentioned lucidum spore powder that shells
15-20%.
Test case:
This test case is to detect that the yield of the lucidum spore powder that shells in embodiment of the present invention 1-3, polyoses content, triterpene contain
Amount.
In embodiment 1-3, the lucidum spore powder that shells is in polyoses content 4.2-4.5%, the premise of triterpene content 5-5.8%
Under, yield is 15-20%.
(1) calculation of above-mentioned yield is:(lucidum spore powder that shells obtained after spray drying in step (10)
The weight of lucidum spore powder is collected into weight/step (1)) × 100%
(2) above-mentioned measurement of the polysaccharide content method is as follows:
A.1, method summary:
Phend-sulphuric acid is that monose is hydrolyzed into the presence of sulfuric acid using polysaccharide, and rapid dehydration generation furfural derives
Thing, furfural and phenol condensation into colored compound.Polyoses content is determined at suitable wavelength with AAS.
A.2, instrument:
(1) centrifuge:3000r/min, (2) 50ml, 100ml volumetric flask, 10ml centrifuge tubes, 10ml tool plug glass tubes, (3)
Spectrophotometer, (4) water-bath, (5) electric boiling plate, (6) ten a ten thousandth electronic balances.
A.3, reagent:(1) DEXTROSE ANHYDROUS, (2) phenol, (3) sulfuric acid, (4) absolute ethyl alcohol.
A.4, determination step:
(1) reference substance solution:The glucose about 80mg of 105 DEG C of dryings to constant weight is taken, it is accurately weighed, in putting 100ml measuring bottles,
Scale is dissolved in water and be diluted to, is shaken up, obtained final product (containing about DEXTROSE ANHYDROUS 0.7mg in per 1ml).
(2) preparation of standard curve:Precision measure reference substance solution 0.0ml.1.0ml, 1.5ml, 2.0ml, 2.5ml,
3.0ml, 3.5ml, 4.0ml, put in 50ml measuring bottles respectively, add water to scale, shake up.Precision measures above-mentioned each solution 2ml, puts tool
In plug test tube, add face with 4% phenol solution 1ml of brand-new respectively, mix, be rapidly added sulfuric acid 7.0ml, shake up.In 40 DEG C of water
30 minutes are incubated in bath, are taken out, put in ice-water bath and place 5 minutes, taken out, be blank with first part, according to UV-vis spectroscopy
Photometry (one annex IVA of Chinese Pharmacopoeia version in 2010), the mensuration absorbance at the wavelength of 485nm is vertical seat with absorbance
Mark, concentration is abscissa, draws standard curve.
(3) determination method:This product about 0.3g is taken, accurately weighed, in putting round-bottomed flask, precision adds water 50ml, weighed weight, plus
Heat backflow 3 hours, is let cool, then weighed weight, and less loss weight is supplied with water, is shaken up, and 15 minutes (3000 turns per minute), essence are centrifuged
Close to measure supernatant 2ml, plus absolute ethyl alcohol 8ml, stirring is centrifuged 15 minutes (3000 turns per minute), takes precipitation and be dissolved in water, puts
In 100ml measuring bottles, and scale is diluted to, shaken up, precision measures 2ml, the method under the preparation of sighting target directrix curve, from " plus face
With 4% phenol solution 1ml of brand-new " rise, mensuration absorbance in accordance with the law, many sugar weights from need testing solution is read on standard curve
(μ g), calculates, and obtains final product.
A.5, calculate:
In formula:A --- the content of containing water-soluble polysaccharide in every 100 grams of samples;Cx --- it is the concentration of polysaccharide in test sample
(ug/ml);W --- it is the weighing (g) of test sample.
(3) assay method of above-mentioned triterpene content is as follows:
(1) preparation of reference substance solution:Take oleanolic acid reference substance appropriate, it is accurately weighed, plus methyl alcohol is made every 1ml and contains
The solution of 0.2mg, obtains final product;
(2) drafting of standard curve:Precision measures reference substance solution 0.1,0.2,0.3,0.4,0.5ml, is respectively placed in
In 15ml tool plug test tubes, volatilize, let cool, precision add it is new prepare vanillic aldehyde glacial acetic acid solution (precision weighs vanillic aldehyde 0.5g,
Acetic acid on the rocks makes to be dissolved into 100ml, obtains final product) 0.2ml, perchloric acid 0.8ml, shake up, heating 15 minutes in 70 DEG C of water-baths, immediately
Put in ice bath and cool down 5 minutes, take out, precision adds ethyl acetate 4ml, shakes up, with corresponding reagent as blank, according to it is ultraviolet-can
See AAS (the one annex VA of version pharmacopeia in 2010), the mensuration absorbance at 546nm wavelength is vertical seat with absorbance
Mark, concentration are that abscissa draws standard curve;
(3) preparation of prepare liquid:The Reishi sporule amidin that will shell (accurately weighs the above-mentioned lucidum spore powder that shells, uses
Distilled water prepares the aqueous solution for turning into 5%) to filter, filtrate is put in the volumetric flask of 100ml, uses appropriate distilled water, respectively washing filter
Device and filter residue, washing lotion are incorporated in above-mentioned volumetric flask, plus ethanol is to scale, shakes up, then precision measures 0.2ml, are placed in 15ml tool plugs
In test tube, it is evaporated, lets cool, precision adds the new vanillic aldehyde glacial acetic acid prepared, and (precision weighs vanillic aldehyde 0.5g, and ice acetic acid makes molten
Solution is obtained final product into 10ml) 0.2ml and perchloric acid 0.8ml, shake up, heated 15 minutes in 70 DEG C of water-baths, take out, it is immediately placed on ice bath
Middle cooling 5 minutes, takes out, and precision adds ethyl acetate 4ml, shakes up, and obtains prepare liquid;
(4) measure of triterpene content:Precision measures 0.2ml water, is placed in 15ml tool plug test tubes, is evaporated, and lets cool, and precision adds
Enter vanillic aldehyde glacial acetic acid (precision weighs vanillic aldehyde 0.5g, ice acetic acid make the to be dissolved into 10ml obtain final product) 0.2ml and height of new preparation
Chloric acid 0.8ml, shakes up, and is heated 15 minutes in 70 DEG C of water-baths, takes out, and is immediately placed in ice bath and cools down 5 minutes, takes out, accurate
Ethyl acetate 4ml is added, blank liquid is obtained final product;With above-mentioned blank liquid as blank, according to UV-VIS spectrophotometry
Determine absorbance of the above-mentioned prepare liquid at 546nm wavelength.The content of oleanolic acid in prepare liquid, three are read according to standard curve
The content of terpene is based on oleanolic acid.