CN109157550A - A kind of acid infiltration high pressure frost wall breaking technology of lucidum spore powder - Google Patents
A kind of acid infiltration high pressure frost wall breaking technology of lucidum spore powder Download PDFInfo
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Abstract
The invention discloses the technical solutions that a kind of lucidum spore powder acid seeps high pressure frost broken wall, lucidum spore powder acid is first seeped bubble by the program, again by high pressure broken wall and freezing broken wall, Reishi sporule wall is set to destroy completely, the content of Reishi sporule releases completely.Specifically, seeped with acid and steep non-ganoderma spove powder, carried out sterilizing high pressure broken wall, dried in 65 DEG C of ovens, then at 4 DEG C of refrigerator freezings, after set 65 DEG C of ovens drying again, that is, complete the broken wall function of Reishi sporule.The high pressure freezes broken wall method sporoderm-broken rate up to 99% or more, and wherein the content of the principle active component ganoderma lucidum polysaccharide of Reishi sporule is 2.5~3.5 times before no broken wall, is 1.5~2.0 times of content of the lucidum spore powder of traditional technology for broken wall broken wall.Moreover, this technology for broken wall meets sanitary condition, the content of Reishi sporule does not have exposed, does not easily cause the oxidation deterioration of content, product can be directly encapsulated or be pressed into tablet, can also saved in not contaminated situation with the long period.
Description
Technical field
The invention belongs to ganoderma lucidium spore powder wall breaking technical fields, and in particular to a kind of acid infiltration high pressure frost of Ganoderma lucidum spore powder is broken
Wall method and its production technology.
Background technique
Ganoderma lucidum belongs to a kind of medicinal fungi plant of Basidiomycetes Polyporaceae Ganoderma, and Reishi sporule is ganoderma lucidum in maturation
When the atomic small spore that is ejected from cap, Reishi sporule is brown oval, and one end is truncate, and size is 8.5~11.2 μ
M × 5.2~6.9 μm have double-wall structure.The chemical component of Reishi sporule mainly has following a few classes: protein and amino acid
Class, glycopeptide class, vitamins, carrotene, sterols, triterpenes, alkaloids, fatty acid, lactone and inorganic ions etc..
Polysaccharide and oligosaccharides are rich in Reishi sporule, but due to its tough and tensile double-wall structure, the active constituent in spore, which is difficult to discharge, to be mentioned
It takes.Since Reishi sporule has double-layer cell wall, it is mainly chitin, cellulose, lignin etc., causes its cell wall hard
It is tough, it is not easy to crack, effective component therein is made to be difficult to the utilization that is absorbed by the body, currently, both at home and abroad in relation to being broken to Reishi sporule
Wall method mainly has bioanalysis, chemical method, physical method, Mechanical Method and 5 kinds of synthesis, (1) bioanalysis: this method includes main benefit
Reishi sporule cell wall is destroyed with the sprouting ability of Reishi sporule itself, " spore germination method " of ingredient intracellular is discharged, passes through benefit
It is one or more with enzyme solutions such as chitinase, cellulase or lywallzymes, make the ingredient degradation in Reishi sporule cell wall, releases
It puts " enzymatic isolation method " of its effective component and is fermented together using microorganism and Reishi sporule, microorganism is allowed to degrade during the fermentation
" the bacteriolyze method " of Reishi sporule cell wall.The advantages of bioanalysis is not consume energy substantially, and crushing effect is preferable, and equipment is simple；
It is longer that disadvantage is needed the time, and is difficult to remove remaining enzyme solution or microorganism etc..(2) chemical method: this method includes benefit
With the similar principle that mixes, Reishi sporule is set to impregnate or flow back for a long time in water, ethyl alcohol equal solvent, to make diffusion of active ingredient
" solvent extraction method " and the inorganic or Organic Acid and Base of utilization into solvent etc. destroy chitin, fiber in Reishi sporule cell wall
The structure of the ingredients such as element, " acid, alkaline degradation method " for making its effective component be easy to dissolve out.The advantages of chemical method and bioanalysis more phase
Seemingly, the disadvantage is that extractant easily leads to effective component denaturation, and dissolvent residual is not easy to remove.(3) physical method: this method including the use of
The effects of moisture in Reishi sporule crystallizes under cryogenic, crystal growth destroys the " cryogenic freezing of Reishi sporule cell wall
Method "；" supercritical ultrasonics technology " of Reishi sporule cell wall is destroyed using the empty mechanical oscillation and cavitation effect of ultrasound；Utilize microwave
Penetration capacity and fuel factor rise rapidly the temperature of cell interior, so that the pressure of cell interior be made to be more than cell wall expansion
The pressure that can bear and be crushed, " microwave method " that promotes its effective component the to discharge and stream using gas in the supercritical state
Volume property, even if the effective component of Reishi sporule is by " super critical extraction " of fluid extraction.The working principle of physical method is different,
Advantage and disadvantage are not also identical, and on the whole, the energy consumption of physical method is larger, and equipment is complex, investment is larger.(4) mechanical
Method: this method is included under the conditions of low temperature etc., swinging, mill, squeeze and break Reishi sporule rapidly using tank body and ball milling etc.
" rolling, extrusion " of wall, by a certain time maintaining the Reishi sporule of non-broken wall in the state of high pressure, then
Pressure release is to lower pressure within another time, " the high pressure gas explosion method " for making the hole on Reishi sporule cell wall increase and increase,
So that compressed air is entered grinding chamber by the grinding mouth of special angle, generates the helical airflow of high speed, material is in spiral air flow
Drive under in grinding chamber high speed rotation, collision is generated due to friction speed between particle, to achieve the effect that crushing
" comminution by gas stream " and using high pressure homogenizer shock, shearing, cavitation, turbulent flow the effects of, material is ground into small
Grain, achievees the effect that " high pressure homogenization method " to homogenize；The advantages of Mechanical Method be it is easy to operate, easy, the disadvantage is that mechanical equipment
Investment is big, operating cost is higher.(5) synthesis: this method refers to 2 kinds or more in 4 kinds of methods of conjunctive use or more to spirit
Ganoderma lucidum spore carries out wall-breaking method.Currently, breaking trachytectum of glossy ganoderma technology and methods both domestic and external, are seldom used alone, it is most
Be while or successively using above-mentioned several method, to increase the sporoderm-broken rate of Reishi sporule.Since Reishi sporule is very small, and it is thin
Cell wall is very tough and tensile, individually it is a kind of effect be difficult to quick, thorough destructions Reishi sporule wall, therefore, synthesis at
For the main flow direction of current ganoderma lucidium spore powder wall breaking research.But current all these wall-breaking methods, are all by the spore of Reishi sporule
Wall damage, keeps the content of Reishi sporule exposed, this easily causes the oxidation deterioration of content, and being highly detrimental to Reishi sporule has
Imitate the preservation of ingredient.
Summary of the invention
The invention discloses the technical solutions that a kind of lucidum spore powder acid seeps high pressure frost broken wall, and the program is first ganoderma lucidum spore
Sub- powder is seeped with hydrochloric acid and is steeped, and then, then by high pressure broken wall and freezing broken wall, so that Reishi sporule wall is destroyed completely, ganoderma lucidum spore
The content of son releases completely.It specifically, is that the non-ganoderma spove powder acid of 1 ~ 3 times of volume is first seeped bubble 1~2
Hour, then, using 121 DEG C, 30 minutes autoclavings being maintained, the Reishi sporule after bubble is seeped to acid carries out high pressure broken wall,
Then, it is dried in 65 DEG C of ovens, then places 4 DEG C of refrigerator freezings 12~24 hours, set 65 DEG C after taking-up again and dry 1~6 hour,
Complete the broken wall function of Reishi sporule.Acid for broken wall of the invention refers to hydrochloric acid, acetic acid, sulfuric acid, nitric acid, phosphoric acid etc.,
It is 0.1~3% with the concentration that hydrochloric acid seeps bubble, is 0.5~5% with the concentration that acetic acid seeps bubble, the time is 1 ~ 3 hour, and this acid seeps high
Pressure frost broken wall method sporoderm-broken rate can reach 99% or more, and wherein the content of the principle active component ganoderma lucidum polysaccharide of Reishi sporule is that do not have
3 times before having broken wall, be 2 times of content using the lucidum spore powder of traditional technology for broken wall broken wall.Moreover, this technology for broken wall
Meet sanitary condition, the content of Reishi sporule does not have exposed, does not easily cause the oxidation deterioration of content, product can be filled directly
Capsule is pressed into tablet, can also be saved in not contaminated situation with the long period.
Specific embodiment:
The following is specific embodiments of the present invention, and technical scheme of the present invention is further described, but guarantor of the invention
Shield range be not limited to these examples, it is all be included in without departing substantially from the change of present inventive concept or equivalent substitute it is of the invention
Within protection scope.
Embodiment one:
Non- ganoderma spove powder is taken, three experimental groups are divided into, every group 40 grams, No. 1 compares for non-ganoderma spove powder, and No. 2
1% hydrochloric acid of non-ganoderma spove powder+65ml seeps bubble experimental group, and 3% acetic acid of No. 3 non-ganoderma spove powder+65ml seeps bubble
Experimental group, No. 1 not acid adding seep bubble, No. 2 with No. 3 with acid seep bubble 1 hour, put pressure cooker high pressure into, heat up, be warming up within 25 minutes
It at 121 DEG C, is kept for 121 DEG C, maintained 30 minutes, cooling when being down to 65 DEG C within 2.5 hours, is taken out, and it is small to be put into 65 DEG C of baking oven drying 6
When, then place 4 DEG C of refrigerators and save 12 hours, take out, then set 65 DEG C and dry 1 hour, weighing to get.
The weight change situation of sample drying after high pressure is shown in Table 1.
The dry weight variation of lucidum spore powder after 1 high pressure of table
Note: 1 compares for the Reishi sporule dry powder of not acid adding；2 be the lucidum spore powder for adding 1% hydrochloric acid to seep bubble；3 be that 3% acetic acid is added to seep
The lucidum spore powder of bubble.
The weight that lucidum spore powder is dried after frost is shown in Table 2.
The weight change of the drying of lucidum spore powder after table 2 freezes
Note: 1 compares for the Reishi sporule dry powder of not acid adding；2 be the lucidum spore powder for adding 1% hydrochloric acid to seep bubble；3 be that 3% acetic acid is added to seep
The lucidum spore powder of bubble.
Content method such as result according to CP method measurement ganoderma spove powder ganoderma lucidum polysaccharide is as follows.
It is prepared by the mother liquor of 1 reference substance solution: take DEXTROSE ANHYDROUS reference substance appropriate, it is accurately weighed, and add water that every lml is made
Solution containing 0.12mg is to get (0.12mg/ml).
The preparation of 2 test solutions: taking each 1g of powder of above-mentioned number 1,2 and 3, and round bottom burning is set in accurately weighed, pack
In bottle, water 30ml is added to stand 1 hour, (95 DEG C ± 2 DEG C) are heated to reflux 4 hours, filter while hot, with a small amount of hot water washing nozzle and
Filter residue sets filter residue and filter paper in flask, adds water 30ml, is heated to reflux 3 hours, filters while hot, merging filtrate, and 90 DEG C of revolvings are extremely
Dry, residue water 2.5ml dissolves, and ethyl alcohol 37.5ml is slowly added dropwise while stirring, shakes up, and places 12 hours at 4 DEG C, 3000r/
Min is centrifuged 10min, discards supernatant liquid, sediment is with hot water dissolving and is transferred in 25ml measuring bottle, lets cool, adds water to scale, shakes
It is even, take solution appropriate, 3000r/min is centrifuged 10min, and precision measures supernatant 0.2ml and sets in 1.8ml water, shakes up to get for examination
Product solution.
The preparation of 3 Reishi sporule powder raw material contrast solutions: " spore powder with crushed sporoderm " and " non-spore powder with crushed sporoderm powder " is taken
Each 1g, accurately weighed, pack is set in round-bottomed flask, adds water 30ml to stand 1h, (95 DEG C ± 2 DEG C) are heated to reflux 4h, filter while hot
It crosses, with a small amount of hot water washing nozzle and filter residue, filter residue and filter paper is set in flask, add water 30ml, be heated to reflux 3 hours, while hot
Filtration, merging filtrate, to doing, residue water 2.5ml dissolves 90 DEG C of revolvings, and ethyl alcohol 37.5ml is slowly added dropwise while stirring, shakes up,
It is placed 12 hours at 4 DEG C, 3000r/min is centrifuged 10min, discards supernatant liquid, sediment is with hot water dissolving and is transferred to 25ml amount
It in bottle, lets cool, adds water to scale, shake up, take solution appropriate, 3000r/min is centrifuged 10min, and precision measures supernatant 0.2ml and sets
In 1.8ml water, shake up to get raw material contrast solution.Raw material control number are as follows: 4A broken wall；4B broken wall；The non-broken wall of 5A；5B
Non- broken wall.
The preparation of 4 reference substance solution standard curves: taking DEXTROSE ANHYDROUS reference substance appropriate, accurately weighed, and water is added to be made often
Solution of the lml containing 0. 12mg is to get reference substance solution mother liquor.Precision measure reference substance solution 0.2ml, 0.4ml, 0.6ml,
0.8ml, 1.0ml, 1.2ml, 1.4ml, 1.6ml are set respectively in 10ml tool plug test tube, and respectively plus sulfuric acid is added in 2.0ml, rapid precision
Green onion ketone solution (precision weighs 0. lg of green onion ketone, adds sulfuric acid 100ml to make to dissolve, shakes up) 6ml, shakes up immediately, after placing 15 minutes,
15 minutes cooling in ice bath, taking-up is set immediately, using corresponding reagent as the synchronous color operation of blank, according to UV-vis spectroscopy light
Degree method measures absorbance at 625nm wavelength, and using absorbance as ordinate, concentration is abscissa, draws standard curve.
Glucose standard curve ultraviolet testing result is shown in Table 3, and standard curve is shown in attached drawing 1.
3 glucose standard curve ultraviolet testing result of table
Calibration curve equation is found out according to 3 glucose standard curve ultraviolet testing result of table: y=7.8016x-0.039, R2=
0.9975, the range of linearity: the abs of 0.064 abs~0.721.
The measuring method of 5 ganoderma lucidum polysaccharide: precision measures test solution 2ml, sets in 10ml EP pipe, the preparation of sighting target directrix curve
Method under, it is accurate rapidly that sulfuric acid green onion ketone solution 6ml is added, it shakes up, after placing 15 minutes, sets immediately cooling in ice bath immediately
It 15 minutes, takes out, using corresponding reagent as the synchronous color operation of blank, according to UV-VIS spectrophotometry, in 625nm wavelength
Place measurement absorbance, from standard curve read test solution in DEXTROSE ANHYDROUS content, calculate to get.
Ganoderma lucidum polysaccharide ultraviolet testing result is shown in Table 4.
4 ganoderma lucidum polysaccharide ultraviolet testing result of table
Note: 1 compares for the Reishi sporule dry powder of not acid adding；2 be the lucidum spore powder for adding 1% hydrochloric acid to seep bubble；3 be that 3% acetic acid is added to seep
The lucidum spore powder of bubble；4A is the lucidum spore powder of broken wall；4B is the lucidum spore powder of broken wall；5A is the ganoderma lucidum of non-broken wall
Conidia powder；5B is the lucidum spore powder of non-broken wall.
From 4 ganoderma lucidum polysaccharide ultraviolet testing result of table as it can be seen that after the ganoderma lucidium spore powder wall breaking of present invention acid infiltration high pressure broken wall, spirit
Sesame polysaccharide is apparently higher than the lucidum spore powder of non-broken wall, wherein the ganoderma lucidum polysaccharide of the lucidum spore powder (No. 2) of bubble is seeped with hydrochloric acid
Content is 3.33 times (5B)~3.54 times (5A) of non-broken wall, be using traditional technology for broken wall broken wall lucidum spore powder 1.91
Again (4B)~2.03 times (4A).The content that the ganoderma lucidum polysaccharide of the lucidum spore powder (No. 3) of bubble is seeped with acetic acid is the 2.54 of non-broken wall
It again (5A)~2.71 times (5B), is 1.46 times (4B)~1.55 times for applying the lucidum spore powder of traditional technology for broken wall broken wall
(4A).The result shows that after the broken wall that wall-breaking method of the invention obtains the main ingredient ganoderma lucidum polysaccharide of lucidum spore powder content
Higher, high pressure wall-breaking method of the invention is to obtain the higher more simple and practical technical solution of effective component.
Technical solution of the present invention preparation ganoderma spove powder can directly it is encapsulated, tabletting or this be prepared into it
His pharmaceutical dosage form.
Detailed description of the invention:
Attached drawing 1 is glucose standard curve figure.
Claims (4)
1. a kind of acid of lucidum spore powder seeps high pressure frost wall-breaking method in the application for preparing ganoderma spove powder production technology.
2. acid as described in claim 1 seeps high pressure wall-breaking method in the application for preparing ganoderma spove powder production technology,
It is characterized in taking non-ganoderma spove powder, 1% hydrochloric acid of 1.0~3.0 times of addition seeps bubble 1~2 hour, with pressure cooker high pressure 121
DEG C, 30 minutes broken walls take out, and are put into 65 DEG C of baking oven drying, then place 4 DEG C of refrigerators and freeze 12 ~ 24 hours, take out, then set 65 DEG C
Drying 1 ~ 6 hour to get.
3. acid as described in claim 1 seeps high pressure wall-breaking method in the application for preparing ganoderma spove powder production technology,
It is characterized in taking 40 grams of non-ganoderma spove powder, 1% hydrochloric acid for adding 65ml seeps bubble 1 hour, puts pressure cooker high pressure into, it heats up,
It when being warming up to 121 DEG C within 25 minutes, is kept for 121 DEG C, maintained 30 minutes, cooling when being down to 65 DEG C within 2.5 hours, takes out, is put into 65
DEG C baking oven is dried 6 hours, then is placed 4 DEG C of refrigerators and saved 12 hours, is taken out, then is set 65 DEG C and dried 1 hour, weighing to get.
4. acid as described in claim 1 seeps high pressure wall-breaking method in the application for preparing ganoderma spove powder production technology,
It is characterized in taking 40 grams of non-ganoderma spove powder, 3% acetic acid for adding 65ml seeps bubble 1 hour, puts pressure cooker high pressure into, it heats up,
It when being warming up to 121 DEG C within 25 minutes, is kept for 121 DEG C, maintained 30 minutes, cooling when being down to 65 DEG C within 2.5 hours, takes out, is put into 65
DEG C baking oven is dried 6 hours, then is placed 4 DEG C of refrigerators and saved 12 hours, is taken out, then is set 65 DEG C and dried 1 hour, weighing to get.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101697981A (en) * | 2009-06-12 | 2010-04-28 | 李长田 | Fast, non-heat change and high-efficiency method for breaking ganoderma lucidum spore |
| CN101768554A (en) * | 2008-12-31 | 2010-07-07 | 胡如军 | Technological method for breaking cell walls of ganoderma lucidum spore powder |
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2018
- 2018-09-14 CN CN201811070854.1A patent/CN109157550A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101768554A (en) * | 2008-12-31 | 2010-07-07 | 胡如军 | Technological method for breaking cell walls of ganoderma lucidum spore powder |
| CN101697981A (en) * | 2009-06-12 | 2010-04-28 | 李长田 | Fast, non-heat change and high-efficiency method for breaking ganoderma lucidum spore |
Non-Patent Citations (3)
| Title |
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| 卢宝驹等: "高温湿热酸法破壁提取法夫酵母胞内虾青素", 《生物工程学报》 * |
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Application publication date: 20190108 |