CN107714739A - A kind of technology for broken wall of lucidum spore powder - Google Patents
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Abstract
The invention discloses a kind of technology for broken wall of lucidum spore powder, it is in the preferable technical foundation of this shell-broken effect of ultralow temperature physical wall breaking, the thick broken wall of pulverizer has been carried out to lucidum spore powder, solution of zinc sulfate and absolute ethyl alcohol mix suspending conidia powder, it is ultrasonically treated, the series of preprocessing such as vacuum freeze drying, the technique is while lucidium spore powder wall breaking rate is improved, reduce destruction of the wall breaking technology to active ingredient in lucidum spore powder, save the high medical value of lucidum spore powder, body is promoted to absorb its effective active composition, with high application value.According to single factor test and orthogonal experiments, obtaining optimum process condition is：The volume ratio of the solution of zinc sulfate of suspension solvent 7% and absolute ethyl alcohol is 1:0.1st, ultrasonic temperature be 30 DEG C, cooling time 8h, obtain ganoderma lucidium spore powder wall breaking rate up to 96.3%.
Description
Technical field
The present invention relates to a kind of technology for broken wall of lucidum spore powder, belong to the wall-breaking method technical field of Reishi sporule.
Background technology
Ganoderma lucidum (Ganoderma) is On Polyporaceae red sesame (Ganoderma lucidum) or purple sesame (Ganoderma
Sinense drying fructification), there is high medical value and bioactivity.And Reishi sporule is ganoderma lucidum growth and maturity phase
The ultrafine particle ejected from cap, belongs to ovum type reproduction cell.The inhereditary material of ganoderma lucidum can all be retained
Get off.Reishi sporule contains a variety of pharmacological components such as abundant polysaccharide, alkaloid, organic germanium and terpene, has and suppresses swollen
Knurl, immunity, hypoglycemic and anti-oxidant etc. multi-efficiency are improved, and its medical value is far above ganoderma lucidum fruitbody and mycelium.
The cell membrane of Reishi sporule is made up of the polysaccharide family macromolecule not soluble in water such as glucan, chitin, is had acidproof
The properties such as alkali resistant, the resistance to anti-digestion of enzyme, pressure-resistant heat resistanceheat resistant, hinder human body and Reishi sporule active ingredient are digested and assimilated, therefore, right
Reishi sporule, which carries out broken wall treatment, can be advantageous to the extraction of its active component.
The wall-breaking method of existing Reishi sporule have ultrasonication method, biological enzyme, supercritical CO 2 method, etc., but these
The shortcomings of method generally existing sporoderm-broken rate is relatively low, less efficient, as broken wall amount of ultrasonication method is limited；Biology enzyme
Method action time is longer；Supercritical CO 2 method can cause the forfeiture of part active ingredient in Reishi sporule.It is studies have reported that ultralow
Warm physical wall breaking technology is i.e. under the condition of ultralow temperature of subzero 40-60 degree, collected lucidum spore powder breaking-wall cell
Machine crushes.Under the crushing cutting of cryogenic high pressure, the ecosystem activity for preserving to greatest extent or not destroying lucidum spore powder has
Composition is imitated, hard Reishi sporule cell membrane is easy to be broken, and has just obtained ganoderma spove powder, then pass through low-temperature stratification
Purification process, removes the broken Reishi sporule wall of no bioactive ingredients, and this technology has effect preferably and do not destroy spore
The advantages of sub- active ingredient.
The present invention is based on ultralow temperature physical wall breaking technology, it is proposed that a kind of new ganoderma lucidium spore powder wall breaking technique, and
Process conditions are optimized using single factor test and orthogonal test, to improve the sporoderm-broken rate of Reishi sporule, reduce Reishi sporule
The loss of middle active ingredient.
The content of the invention
To achieve the above object, the present invention provides following technical scheme：A kind of technology for broken wall of lucidum spore powder, its feature
It is, it comprises the following steps：
(1) before broken wall accurately with processing：Screen the intact Reishi sporule of quality；
(2) pulverization process：Reishi sporule sampling pulverizer was crushed to 80 mesh sieves；
(3) suspension is made as solvent using 7% solution of zinc sulfate and appropriate absolute ethyl alcohol in the conidia powder of sieving；
(4) ultrasound pretreatment：Sampling ultrasound pretreatment lucidum spore powder；
(5) vacuum freeze drying；
(6) ultralow temperature physical wall breaking equipment spore powder with crushed sporoderm is utilized；
(7) lucidum spore powder of broken wall is obtained.
Further, preferably, in the step (3), the volume ratio of 7% solution of zinc sulfate and absolute ethyl alcohol is 1: 0.2
To between 1: 0.1.
Further, preferably, in the step (4), ultrasonic time is 10 or 20min, and ultrasonic temperature is at 30~35 DEG C
In the range of.
Further, preferably, in the step (5), cooling time is in 6~8h, and cryogenic temperature is -25~-15
In the range of DEG C.
Further, preferably, the volume ratio of 7% solution of zinc sulfate and absolute ethyl alcohol is 1:0.1, ultrasonic temperature 30
DEG C, cooling time 8h.
Further, preferably, the sporoderm-broken rate detection method of the technique is：Blood count is used to ganoderma spove powder
Plate counts, and draws standard curve y=8069.2x+1.6944 (y is conidia powder average, and x is conidia powder quality, R2=
0.9995) sporoderm-broken rate, is calculated according to the following formula：
In formula：X is sporoderm-broken rate/%；N1For the non-wall-breaking lucidum with testing sample phase homogenous quantities found from standard curve
Spore number；N2For the Reishi sporule number of non-broken wall in the ganoderma spove powder that counts to get.
The present invention proposes a kind of new ganoderma lucidium spore powder wall breaking technique, i.e., in this broken wall effect of ultralow temperature physical wall breaking
In the preferable technical foundation of fruit, lucidum spore powder has been carried out the thick broken wall of pulverizer, solution of zinc sulfate mixed with absolute ethyl alcohol it is outstanding
The series of preprocessing such as floating conidia powder, supersound process, vacuum freeze drying, the technique while lucidium spore powder wall breaking rate is improved,
Reduce destruction of the wall breaking technology to active ingredient in lucidum spore powder, save the high medical value of lucidum spore powder, promote
Body is entered to absorb its effective active composition, there is high application value.According to single factor test and orthogonal test knot
Fruit, obtaining optimum process condition is：The volume ratio of the solution of zinc sulfate of suspension solvent 7% and absolute ethyl alcohol is 1:0.1st, ultrasound temperature
Spend for 30 DEG C, cooling time 8h, obtain ganoderma lucidium spore powder wall breaking rate up to 96.3%.
Compared with existing wall breaking technology, it is an advantage of the invention that：
(1) before broken wall, series of preprocessing (the thick broken wall of pulverizer, 7% solution of zinc sulfate are carried out to lucidum spore powder
With absolute ethyl alcohol mix suspending conidia powder, supersound process, vacuum freeze drying), improve the sporoderm-broken rate of conidia powder.
(2) what the technology for broken wall used is physical wall breaking method, the active ingredient in conidia powder will not be produced larger
Influence, technological process is simpler, workable, and broken wall efficiency is also high, can be widely used in ganoderma spove powder product
Production.
Brief description of the drawings
Fig. 1 is the influence that suspension solvent volume compares lucidium spore powder wall breaking rate；
Fig. 2 is influence of the ultrasonic time to lucidium spore powder wall breaking rate；
Influence of Fig. 3 ultrasonic temperatures to lucidium spore powder wall breaking rate；
Influence of Fig. 4 cooling times to lucidium spore powder wall breaking rate；
Influence of Fig. 5 cryogenic temperatures to lucidium spore powder wall breaking rate；
The SEM of the non-ganoderma spove powders of Fig. 6 (A) and ganoderma spove powder (B, C, D) schemes；
Note：Letter is different in figure represents significant difference (p<0.05).
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out it is clear,；It is complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other under the premise of creative work is not made
Embodiment, belong to the scope of protection of the invention.
1 materials and methods：
1.1 test material
Lucidum spore powder is provided by wide Zhejiang Essence Fungi Development Co., Ltd., is 100% lucidum spore powder.
1.2 method
1.2.1 technology for broken wall
Broken wall forespore powder → pulverizer be crushed to 80 mesh sieves → using 7% solution of zinc sulfate with appropriate absolute ethyl alcohol to be molten
Agent is made suspension → pretreatment lucidum spore powder (supersound process) → vacuum freeze drying → and set using ultralow temperature physical wall breaking
Standby spore powder with crushed sporoderm → ganoderma spove powder
1.2.2 sporoderm-broken rate detects
Ganoderma spove powder is counted using blood counting chamber, and draws standard curve y=8069.2x+1.6944 (y
For conidia powder average, x is conidia powder quality, R2=0.9995) sporoderm-broken rate, is calculated according to the following formula：
In formula：X is sporoderm-broken rate/%；N1For the non-wall-breaking lucidum with testing sample phase homogenous quantities found from standard curve
Spore number；N2For the Reishi sporule number of non-broken wall in the ganoderma spove powder that counts to get.
1.2.3 single factor experiment
Technology for broken wall in " 1.2.1 " carries out broken wall treatment to lucidum spore powder, using ganoderma lucidium spore powder wall breaking rate as
Test index, analyze the volume ratio of 7% solution of zinc sulfate and absolute ethyl alcohol in suspension solvent, ultrasonic time, ultrasonic temperature, cold
Freeze time, cryogenic temperature to the influence degree of ganoderma lucidium spore powder wall breaking rate, single factor experiment design such as table 1.
The single factor design of table 1
Note：Rigid condition：Suspension solvent volume ratio is 1: 0.1；Ultrasonic time is 20min；Ultrasonic temperature is 25 DEG C；It is cold
The jelly time is 5h；Cryogenic temperature is -20 DEG C
1.2.4 orthogonal test
According to the Pearson coefficients of each factor in " 1.2.3 " single factor experiment result and ganoderma lucidium spore powder wall breaking rate, select
The factor being had a significant impact to ganoderma lucidium spore powder wall breaking rate carries out orthogonal test, and orthogonal experiments are verified, obtains
Optimal technique process.
1.2.5 the sign of ganoderma spove powder
Utilize the configuration of surface of scanning electron microscope sem observation ganoderma spove powder and non-ganoderma spove powder.
1.2.6 data process＆analysis
All data are represented with average value (mean) ± standard deviation (SD), and single factor test variance is carried out with SPSS22.0 softwares
Analyze (ANOVA), then carry out Tukey Multiple range tests, work as P<0.05 is thought with significant difference；Divided with Pearson is related
Analysis draws the factor having a significant impact to ganoderma lucidium spore powder wall breaking rate.
2 results are with discussing：
2.1 single factor experiment results
2.1.1 suspension solvent volume compares the influence of ganoderma lucidium spore powder wall breaking rate
(note as seen from Figure 1：Letter is different in Fig. 1 represents significant difference (p<0.05)), when two kinds of suspension solvent bodies
Product is than being 1: 0, i.e., when only making suspension solvent with solution of zinc sulfate, ganoderma lucidium spore powder wall breaking rate will be significantly higher than suspension volume
Than the sporoderm-broken rate (p to be obtained when 0: 1 (only making solvent with absolute ethyl alcohol)<0.05), illustrate compared to absolute ethyl alcohol, zinc sulfate
Solution can preferably suspend Reishi sporule.In addition, when two kinds of solvents are with certain volume ratio (1: 0.4,1: 0.3,1: 0.2,1: 0.1)
During common suspension conidia powder, obtained lucidium spore powder wall breaking rate is all remarkably higher than two kinds of solvents and acts solely on what is obtained during conidia powder
Sporoderm-broken rate, lucidium spore powder wall breaking rate can be improved by illustrating to mix both, and this is probably due to containing spore oil in spore powder with crushed sporoderm, making
Obtain spore generation when microscopy counts and stick and gather, influence to count, addition absolute ethyl alcohol can be such that spore oil is dissolved in wherein, avoid spore
It is glutinous poly-, reduce experimental error.As shown in Figure 1, when the volume ratio of 7% solution of zinc sulfate and absolute ethyl alcohol is left 1: 0.2,1: 0.1
When right, obtained lucidium spore powder wall breaking rate is higher.
2.1.2 influence of the ultrasonic time to ganoderma lucidium spore powder wall breaking rate
As shown in Figure 2, the sporoderm-broken rate obtained when carrying out the supersound process of certain time to conidia powder, which is significantly higher than, not to be carried out
Sporoderm-broken rate (p during supersound process<0.05), ultrasound not only contributes to the scattered of conidia powder, and its caused energy can also make spore
Powder does violent forced vibration and crushed, and improves the sporoderm-broken rate of conidia powder to a certain extent, but ultrasonic time is long, can
Can the active ingredient that can destroy in conidia powder, so in order to obtain higher lucidium spore powder wall breaking rate, reduce in conidia powder effectively into
The destruction divided, selects optimal ultrasonic time as 10 or 20min.
2.1.3 influence of the ultrasonic temperature to ganoderma lucidium spore powder wall breaking rate
From the figure 3, it may be seen that ultrasonic temperature, at 20,25 DEG C, lucidium spore powder wall breaking rate is without significant difference (p>0.05), when temperature liter
During to 30 DEG C, sporoderm-broken rate significantly improves (p<0.05), and temperature is risen to after 40 DEG C, and becoming of slowly reducing is presented in sporoderm-broken rate again
Gesture, this be probably because as the velocity of sound of the rise of temperature, ultrasonic wave can be gradually reduced, its caused energy is also gradually reduced,
Its active force to conidia powder also can decrease to some degree.By Fig. 3 optimal ultrasonic temperature can be speculated in 30~35 DEG C of models
In enclosing.
2.1.4 influence of the cooling time to ganoderma lucidium spore powder wall breaking rate
As shown in Figure 4, in 3~6h cooling time, the sporoderm-broken rate of conidia powder is in the trend gradually stepped up, after 6h,
Sporoderm-broken rate slowly declines, and illustrates that the different of cooling time can produce a certain degree of influence to the size of lucidium spore powder wall breaking rate.It is cold
When the jelly time is 6,7h, sporoderm-broken rate is significantly higher than the sporoderm-broken rate (p of other groups<0.05), respectively 82.2%, 82.1%, in addition,
Sporoderm-broken rate when cooling time is 8h is also up to 80.0%, therefore selects optimal cooling time in 6~8h.
2.1.5 influence of the cryogenic temperature to ganoderma lucidium spore powder wall breaking rate
As shown in Figure 5, for cryogenic temperature at -25~-15 DEG C, lucidium spore powder wall breaking rate is without significant difference (p>0.05) it is, and aobvious
Write the sporoderm-broken rate (p more than other temperature groups<0.05), thus speculate optimal cryogenic temperature in the range of -25~-15 DEG C.
2.1.6 the correlation of each factor and ganoderma lucidium spore powder wall breaking rate
Pearson correlation coefficient is also known as simple correlation coefficient, is typically represented with r values, is correlation between a kind of two variables of measurement
The method of degree.It is a value between 1 and -1, and r values are that positive number represents that two variables are proportionate, and are negative for negative
Correlation, its absolute value represent two respectively in 0.00-0.19,0.20-0.39,0.40-0.69,0.70-0.89,0.90-1.00
The extremely low correlation of variable, lower correlation, moderate correlation, height correlation, high correlation.In SPSS, Pearson correlation coefficient is not only
R values are seen, r values represent the size of two correlation of variables, also to see p value, and p value is test value, examine two variables to be come from sample
Totality in whether there is as sample.
As seen from Table 2, when the volume ratio of the solution of zinc sulfate of suspension solvent 7% and absolute ethyl alcohol, ultrasonic temperature, freezing
Between significantly correlated (p between ganoderma lucidium spore powder wall breaking rate respectively be present<0.05), ultrasonic time, cryogenic temperature and sporoderm-broken rate
Between without significant correlation (p>0.05), meanwhile, it can be seen from r values, suspension solvent volume ratio, ultrasonic temperature with ganoderma lucidum spore
Sub- powder sporoderm-broken rate shows height correlation, and it is related that cooling time and sporoderm-broken rate show moderate, considers r values and p value, selects
Three suspension solvent volume ratio, ultrasonic temperature, cooling time factors carry out ensuing orthogonal test, draw lucidum spore powder
The optimal conditions of technology for broken wall.
Pearson correlation coefficient between 2 each factor of table and ganoderma lucidium spore powder wall breaking rate
Note：p<0.05 represents there is significant difference
2.2 orthogonal test
The factor level table of table 3
The orthogonal experiments of table 4 and range analysis
The orthogonal test variance analysis of table 5
Note：F values are statistics value；P values are significance probability, P<0.05 represents there is significant difference
The orthogonal test Tukey method Multiple range tests of table 6
Note：Difference letter under each factor varying level represents there is significant difference (P<0.05)
According to the result of above single factor experiment, the orthogonal test of Three factors-levels is carried out, the factor level of selection is such as
Shown in table 3.It was found from the range analysis of table 4, each factor primary-slave relation for influenceing ganoderma lucidium spore powder wall breaking rate is：(suspension is molten by A
Agent volume ratio)>B (ultrasonic temperature)>C (cooling time).The variance analysis of table 5 shows that influence of these three factors to sporoderm-broken rate is equal
Significant difference (p be present<0.05), result above matches with the Pearson results analyzed.
As seen from Table 6, significant difference (p be present between each level of three factors<0.05) Tukey method multiple ratios, are passed through
Compared with optimal preparation condition should be A in theory3B1C3。
2.3 checking test
To A3B1C3This combination carries out parallel verified three times and tested, the results showed that, A is tested three times3B1C3Obtain sporoderm-broken rate
Respectively 95.7%, 96.2%, 96.9%, average value 96.3%, matched with orthogonal experiments, further demonstrate this
The feasibility of technique.By single factor test and orthogonal test, it is A to obtain Optimal technique process3B1C3, i.e. the sulfuric acid of suspension solvent 7%
The volume ratio of zinc solution and absolute ethyl alcohol is 1:0.1st, ultrasonic temperature be 30 DEG C, cooling time 8h.
The surface topography of 2.4 ganoderma spove powders
The surface topography of non-ganoderma spove powder and ganoderma spove powder under SEM observations is as shown in fig. 6, non-broken wall
Lucidum spore powder (A) field range endospore is complete, and most of spore is broken ganoderma spove powder (B) within sweep of the eye
Wall, difference of them is obvious, also can conidia powder outer wall visible in detail from the ganoderma spove powder SEM figures (C, D) after amplification
Rupture.
3 summarize：This experiment proposes a kind of new ganoderma lucidium spore powder wall breaking technique, i.e., this in ultralow temperature physical wall breaking
In the preferable technical foundation of shell-broken effect, the thick broken wall of pulverizer, solution of zinc sulfate and absolute ethyl alcohol have been carried out to lucidum spore powder
The series of preprocessing such as mix suspending conidia powder, supersound process, vacuum freeze drying, the technique are improving lucidium spore powder wall breaking rate
Meanwhile reduce destruction of the wall breaking technology to active ingredient in lucidum spore powder, save the high medicinal valency of lucidum spore powder
Value, promotes body and its effective active composition is absorbed, have high application value.
According to single factor test and orthogonal experiments, obtaining optimum process condition is：The solution of zinc sulfate of suspension solvent 7% with
The volume ratio of absolute ethyl alcohol is 1:0.1st, ultrasonic temperature be 30 DEG C, cooling time 8h, it is reachable to obtain ganoderma lucidium spore powder wall breaking rate
96.3%.
It is an advantage of the invention that：
(1) before broken wall, series of preprocessing (the thick broken wall of pulverizer, 7% solution of zinc sulfate are carried out to lucidum spore powder
With absolute ethyl alcohol mix suspending conidia powder, supersound process, vacuum freeze drying), improve the sporoderm-broken rate of conidia powder.
(2) what the technology for broken wall used is physical wall breaking method, the active ingredient in conidia powder will not be produced larger
Influence, technological process is simpler, workable, and broken wall efficiency is also high, can be widely used in ganoderma spove powder product
Production.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (6)
1. a kind of technology for broken wall of lucidum spore powder, it is characterised in that it comprises the following steps：
（1）Before broken wall accurately with processing：Screen the intact Reishi sporule of quality；
（2）Pulverization process：Reishi sporule sampling pulverizer was crushed to 80 mesh sieves；
（3）Suspension is made as solvent using 7% solution of zinc sulfate and appropriate absolute ethyl alcohol in the conidia powder of sieving；
（4）Ultrasound pretreatment：Sampling ultrasound pretreatment lucidum spore powder；
（5）Vacuum freeze drying；
（6）Utilize ultralow temperature physical wall breaking equipment spore powder with crushed sporoderm；
（7）Obtain the lucidum spore powder of broken wall.
A kind of 2. technology for broken wall of lucidum spore powder according to claim 1, it is characterised in that：The step（3）In, 7%
The volume ratio of solution of zinc sulfate and absolute ethyl alcohol is between 1: 0.2 to 1: 0.1.
A kind of 3. technology for broken wall of lucidum spore powder according to claim 1, it is characterised in that：The step（4）In, surpass
The sound time is 10 or 20min, and ultrasonic temperature is in the range of 30~35 DEG C.
A kind of 4. technology for broken wall of lucidum spore powder according to claim 1, it is characterised in that：In the step（5）In,
Cooling time is in 6~8h, and cryogenic temperature is in the range of -25~-15 DEG C.
A kind of 5. technology for broken wall of lucidum spore powder according to claim 1, it is characterised in that：7% solution of zinc sulfate with
The volume ratio of absolute ethyl alcohol is 1:0.1, ultrasonic temperature is 30 DEG C, cooling time 8h.
A kind of 6. technology for broken wall of lucidum spore powder according to claim 1, it is characterised in that：The sporoderm-broken rate inspection of the technique
Survey method is：Ganoderma spove powder is counted using blood counting chamber, and draws standard curve y=8069.2x+1.6944（y
For conidia powder average, x is conidia powder quality, R2=0.9995）, sporoderm-broken rate is calculated according to the following formula：
X=；
In formula：X is sporoderm-broken rate/%；N1For the non-wall-broken ganoderma spore number with testing sample phase homogenous quantities found from standard curve
Mesh；N2For the Reishi sporule number of non-broken wall in the ganoderma spove powder that counts to get.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108853151A (en) * | 2018-09-19 | 2018-11-23 | 山东药乡生物工程有限公司 | A kind of broken wall of the Reishi sporule containing spore oil goes wall method |
| CN115338001A (en) * | 2022-08-12 | 2022-11-15 | 武夷山元生泰生物科技有限公司 | Wall breaking method of ganoderma lucidum spore powder |
| CN115944078A (en) * | 2022-12-20 | 2023-04-11 | 南京中科药业有限公司 | Method for improving fluidity of wall-broken ganoderma lucidum spore powder |
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