CN1250233C - Method for sufficient releasing effective component of ganoderma lucidum spore powder - Google Patents
Method for sufficient releasing effective component of ganoderma lucidum spore powder Download PDFInfo
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- CN1250233C CN1250233C CN 03133778 CN03133778A CN1250233C CN 1250233 C CN1250233 C CN 1250233C CN 03133778 CN03133778 CN 03133778 CN 03133778 A CN03133778 A CN 03133778A CN 1250233 C CN1250233 C CN 1250233C
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Abstract
The present invention relates to a technique for processing ganoderma lucidum spore powder, and particularly to discloses a method capable of sufficiently releasing the effective component of ganoderma lucidum spore powder. The present invention adopts a microwave softening processing mode which specifically comprises the following procedures: 1), the raw material of ganoderma lucidum spore powder is put in a microwave reaction chamber, organic acid solution is added, and the mixture is sufficiently agitated and uniformly moistened; 2), the mixture is processed by microwaves, microwave power is exerted, the reaction of the organic acid solution with chitin and gelatine in an epispore structure are reinforced by the microwaves to make part of the chitin and the gelatine dissolved, and nanometer-size holes or cracks which are densely distributed on epispores are manufactured; 3), distillation is carried out under reduced pressure, and the organic acid solution is removed; continuous microwaves and pulse microwaves are combined in the microwave power application mode, radiation is firstly carried out by the continuous microwaves until the organic acid solution is refluxed, and then, the continuous microwaves are converted into the pulse microwaves for carry out radiation for 5 min to 100 min. The present invention improves the release capability of the effective component (particularly polysaccharide) of the spore powder, guarantees the integrity of the integral appearance of the spore powder, and prevents the effective component which is easily oxidized from loss.
Description
Technical field
The present invention relates to the Ganoderma spore powder process technology, specifically a kind of method that can fully discharge the Ganoderma spore powder effective ingredient.
Background technology
Ganoderma is described as " Herba mesonae chinensis " of strengthening the body resistance by China's successive dynasties medicine scholar.Recent two decades comes, because the success of artificial culture Ganoderma technology and wideling popularize is done a lot of work to Ganoderma sporophore and mycelial research.Simultaneously, updating of Ganoderma spore powder collection technique also promoted the systematic study of people to the aspects such as pharmacological effect of spore powder greatly.Ganoderma spore powder be the Ganoderma development later stage launch the kind that discharges in, biologically claim basidiospore, be powder after putting together, the common name Ganoderma spore powder.Ganoderma spore powder has been assembled the elite of Ganoderma, and the kind of various effective ingredient and content all are higher than sporophore and mycelium.Contain compositions such as rich in amino acid, polysaccharide, polypeptide, protein, terpenoid, alkaloid, organic germanium, vitamin in the Ganoderma spore.It is in enhance immunity, and the drug effect aspect that suppresses tumor is also considerably beyond its parent Ganoderma.Clinical practice proves, Ganoderma spore powder all has the obvious treatment effect to tumor, liver cirrhosis, diabetes, coronary heart disease, hyperlipidemia, neurasthenia, leukemia, thrombocytopenia etc., and these effects are mainly derived from effective ingredient such as polysaccharide in the Ganoderma spore powder, triterpene, nucleoside.Since to human body nontoxic, harmless, have no side effect, Ganoderma spore powder enters the domestic and international market as a class special health product or nutraceutical, and obtains the extensive approval of consumer.
But, the double-deck sporoderm structure that is made of inorganic elementss such as lignin, cellulose, chitin, colloid and Si and Ca is not only very hard, also have extremely strong resistance to oxidation and acid and alkali resistance corrosive power, both limited the absorption of human body to effective ingredient in the spore powder, particularly to the absorption of polysaccharide, also restricted the high efficiency extraction of effective ingredient in the spore powder, made with the Ganoderma spore powder that to be that raw material carries out related drugs (as the ganoderma spore polysaccharide injection) production cost high.
The experimental results shows that the two-way immunoregulation effect of ganoderan is the material base of Ganoderma series products strengthening the body resistance.For this reason, the deep working method of searching Ganoderma spore becomes the research focus of developing Ganoderma spore powder in recent years.At present, the research of the processing method of Ganoderma spore focused mostly on (break the hard outer wall of spore at breaking cellular wall, destroy the globality of spore) on, now formed comprise biologic enzymolysis method, ultrasonic disruption method, supersonic airstream comminuting method etc. multiple lucidium spore powder wall breaking method.Because the supersonic airstream comminuting method has working (machining) efficiency height, breaking cellular wall efficient height advantages such as (can surpass 90%), is extensive use of aborning.Now, the Ganoderma spore powder product that occurs multiple brand on the market is handled through the supersonic airstream wall-breaking method mostly.
The supersonic airstream wall-breaking method can make that the extraction ratio of lipid and terpenoid obviously improves in the spore powder, but the extraction ratio of polysaccharide is not seen and is significantly improved, even reach the sporoderm-broken rate more than 90%, the dissolution rate of ganoderma spore polysaccharide in aqueous solution only doubles than former powder, and the polysaccharide in the spore powder more than 80% still is present in the spore powder with crushed sporoderm and can not dissolves in the water.This may be present in the hard double wall shell with ganoderan more direct relation.More bad is, theory and practice has proved that all easily caking is rotten behind the complete breaking cellular wall of spore powder, have a strong impact on activity and taste, think that this mainly is because its interior effective ingredient of the spore powder behind the breaking cellular wall, especially some oil substances are easy to oxidation deterioration owing to being exposed to fully in the air, are unfavorable for storing.Adopt the antioxidation measure so have to during preservation and packaging,, bring a series of problems such as cost rising as adding antioxidant, filling measures such as nitrogen inner packing, low temperature storage, employing processed with honey type and microcapsule-type.Therefore, for the quality, the exploitation of accelerating Ganoderma spore class medicine that improve spirit skill spore powder product, reduce production costs, be necessary to seek new processing method, can increase substantially the releasability of effective ingredient in the Ganoderma spore powder (particularly polysaccharide), can guarantee that again effective ingredient keeps its original biological activity in the preservation process of spore powder.
The efficient rapid extraction that microwave heating technique is applied to the natural drug effective ingredient is the natural drug extractive technique that grows up in the world over past ten years.This technology abbreviates microwave extraction as, its principle is: the moisture microwave and the effect of cell interior, vaporization is rapidly heated, cell interior pressure is increased sharply, until " implosion " takes place, cause cell wall rupture, the interior effective ingredient of cell can directly be dissolved in extract in the medium, realize the efficient rapid extraction of effective ingredient.Generally speaking, " implosion " phenomenon often can be finished in the extremely short time (10-1 second～10 second), thereby can not cause the destruction of the not too strong effective ingredient of thermal sensitivity.
But water content is low excessively in cell, and raw material is difficult to obtain Fast Heating because of can not fully absorbing microwave energy, or the obdurability of cell wall is when enough high, and " implosion " phenomenon or be difficult to take place perhaps takes place also can not cause cell wall rupture; In this case, microwave extraction not only can not be brought into play efficiently effect fast, can make effective ingredient cause loss because of heat damage on the contrary.Because the water content in the Ganoderma spore powder generally is no more than 10%, cell wall is extremely tough and tensile again, is difficult to utilize " implosion " effect that spore powder is carried out broken wall treatment, thereby also is difficult to significantly improve with the microwave extraction technology extraction efficiency of effective ingredient in the spore powder.
Summary of the invention
In order to overcome above-mentioned deficiency, the purpose of this invention is to provide a kind of method that can fully discharge the Ganoderma spore powder effective ingredient, it utilizes the microwave softened technology, both improved the releasability of effective ingredient in the spore powder (particularly polysaccharide), guarantee the integrity of spore powder bulk shape again, avoided easy oxidation loss of active ingredients.
To achieve these goals, technical scheme of the present invention is as follows:
Adopt the microwave softened processing mode, be specially: 1) the Ganoderma spore powder raw material is inserted in the microwave reaction chamber, add organic acid soln, fully stir and make even moistening; 2) microwave treatment applies microwave power, utilizes chitin and gelationus reaction in microwave reinforced organic acid soln and the sporoderm structure, and it is partly dissolved, and produces the nanoscale hole or the crackle of dense distribution on sporoderm; 3) distilling under reduced pressure, get rid of organic acid soln:
Wherein: it is that continuous microwave combines with pulse microwave that described microwave power applies mode, and using earlier continuous microwave irradiation, time is to reflux to organic acid soln, is converted to pulse microwave then, irradiation 5min～100min; Its reaction condition is as follows:
1) the quality power density of microwave power is 10 kilowatts of 1 kilowatt～every kilogram materials of every kilogram of material;
2) the reaction chamber operating pressure is 20mmHg～760mmHg;
3) the weight of material proportioning is a spore powder: organic acid soln=5/1～1/5;
The quality power density is 5 kilowatts of 1 kilowatt～every kilogram materials of every kilogram of material under the described continuous microwave situation; The quality power density is 10 kilowatts of 2 kilowatts～every kilogram materials of every kilogram of material under the pulse microwave situation, and dutycycle is A/B, A=1 second～100 second wherein, B=1 second～100 second; Described material is the mixture of spore powder and organic acid soln; Described organic acid soln is respectively that concentration is 5%～50% oxalic acid, 20%～99% formic acid, 20%～99% acetic acid or 20%～99% propanoic acid aqueous solution; Described microwave cavity both can be the travelling-wave-type microwave cavity, also can be the resonant mode microwave cavity; When the organic acid soln of described adding was oxalic acid solution, the removal that softening back adopts calcium ion to carry out oxalic acid was handled.
The principle of the invention is: significantly strengthen the acidolysis reaction of organic acid to organic macromolecules such as chitin, colloids by microwave, make microwave when acting on Ganoderma spore powder and organic acid mixed system, chitin and the colloid that is filled in lignin and the cellulose network can be dissolved in the acid solution, make sporoderm be transformed into loose structure by compact texture, for the abundant release of the effective ingredient in the spore powder provides a large amount of passages, spore powder still is kept perfectly simultaneously.Therefore, course of reaction of the present invention is different from the spore powder shattering process, be the process that makes sporoderm " expanded " or claim " softening ", microwave softened processing method then of the present invention provides a kind of and has not destroyed the technology path that only makes sporoderm " expanded " or " softening " under the spore powder overall structure prerequisite.
Compared with prior art, the present invention has more following advantage:
1. effective component extraction rate height.The present invention utilizes chitin and gelationus reaction in organic acid reagents such as microwave reinforced oxalic acid, formic acid, acetic acid, propanoic acid and the sporoderm structure, it is partly dissolved, thereby on sporoderm, produce the nanoscale hole or the crackle of dense distribution, the profile of the Ganoderma spore powder after the processing keeps the integrity of primospore powder, dense distribution the hole or the crackle of many nanoscales on the sporoderm, can improve effective ingredient release rate in the Ganoderma spore powder greatly.Extraction especially for effective ingredient such as polysaccharide, can significantly improve extraction ratio, as: polyoses content of the present invention can reach 5%～16%, far above in be untreated spore powder and the prior art the wall-breaking method that adopts handle the polyoses content (2%～4%) of back spore powder, the crude polysaccharides content in the Ganoderma spore aqueous extract after microwave softened is handled be untreated or the spore powder water extract after supersonic airstream breaking cellular wall (90% above sporoderm-broken rate) is handled in 3～7 times of polyoses content raisings.Utilization ratio of raw materials is significantly improved, and the later stage separation and purification cost of extracting solution is able to remarkable reduction.
2. convenient the storage.The deficiency of activity and taste is gone bad, had a strong impact on to easy the caking after product of the present invention had been avoided the complete breaking cellular wall of prior art miospore powder, its interior effective ingredient of spore powder after softening, especially be not exposed in the air not can oxidation deterioration for some oil substances, is beneficial to storage.Reduced cost.
3. effective ingredient absorbance height.Adopt the spore powder of the present invention after microwave softened is handled to be directly used in human body and take, can increase substantially the abundant absorption of human body effective ingredient such as polysaccharide, Ganodenic acid, nucleoside in the spore powder.
Description of drawings
Fig. 1 is the atomic force microscope photo of one embodiment of the invention spore powder raw material without the spore powder of microwave softened processing.
Fig. 2 is the atomic force microscope photo of one embodiment of the invention spore powder raw material spore powder after microwave softened is handled.
Concrete embodiment
Below in conjunction with drawings and Examples the present invention is described in further detail.
Embodiment 1
1. the 1.5kg Ganoderma spore powder places the travelling-wave-type microwave cavity;
2. get oxalic acid 180g, add water 2.0L and be made into oxalic acid solution;
3. get above-mentioned solution 2L, be added in the above-mentioned microwave cavity, fully stir and make even moistening;
4. above-mentioned material has been irradiated to liquid return under 5KW continuous microwave power, it is the organic acid soln vaporization, change pulse microwave power working method into, dutycycle is 5 seconds/5 seconds, peak power 10KW, behind the maintenance 20min, evacuation (the reaction chamber operating pressure is 20mmHg), no liquid to the microwave cavity is finished the microwave softened of spore powder and is handled.
5. add distilled water 5L among the Ganoderma spore powder 1.5kg after softening, fully stir, filter, add full aqua calcis in the filtrate, complete to oxalic acid precipitation, the filtering precipitation.Filtrate is added in the above-mentioned 1.5kg spore powder, and 60 ℃ of evaporated under reduced pressure get finished product.
As shown in Figure 1, 2, very smooth, fine and close without the spore powder material powder surface that microwave softened is handled, and after microwave softened of the present invention was handled, the spore powder surface had formed numerous nanoscale hole and crackle, but spore powder has kept the integrity of overall geometry.
Because polysaccharide is the topmost active component of spore powder, thereby the present invention is with the method for the dissolve in amount of polysaccharide in water as effective ingredient releasability in the evaluation spore powder.Concrete grammar is: weigh up 10 gram spore powder raw materials, supersonic airstream breaking cellular wall (90% above sporoderm-broken rate) spore powder and microwave softened spore powder respectively, put into the conical flask of three 500ml, each adds the 100ml distilled water, carries out water and carry in 80 ℃ hot bath, 1 hour extraction time.After water is proposed end, take out all materials, the centrifuge tube of packing into carries out high speed centrifugation.Then, each takes out supernatant 50ml, adds the 300ml dehydrated alcohol respectively and carries out precipitate with ethanol, behind high speed centrifugation, removes supernatant, and pure hypostasis is carried out vacuum drying, obtains not moisture and alcoholic acid dried crude polysaccharides.At last, with analytical balance weighing crude polysaccharides.Crude polysaccharides weight with the spore powder raw material is divisor, and the crude polysaccharides of spore powder with crushed sporoderm and microwave softened spore powder is a dividend, and ratio is represented spore powder its effective ingredient releasability after the different disposal method is handled.Measurement result shows: under the extraction process by water condition of identical extraction, the crude polysaccharides content in the Ganoderma spore aqueous extract after microwave softened is handled be untreated or the spore powder water extract after supersonic airstream breaking cellular wall (90% above sporoderm-broken rate) processing in polyoses content improve respectively more than 6～8 times and 3～4 times.This result shows that microwave softened method of the present invention can increase substantially the solvability of ganoderan in aqueous solution, and its polysaccharide releasability sees Table 1.
Embodiment 2
Difference from Example 1 is:
1. the 1.5kg Ganoderma spore powder places the travelling-wave-type microwave cavity;
2. get anhydrous formic acid 1.8L, add water 1.2L and be made into formic acid solution 3L;
3. get above-mentioned solution 3L, be added in the above-mentioned microwave cavity, fully stir and make even moistening;
4. above-mentioned material has been irradiated to liquid return under 3KW continuous microwave power, it is the organic acid soln vaporization, change pulse microwave power working method into, dutycycle is 5 seconds/15 seconds, and peak power 8KW is behind the maintenance 40min, evacuation (the reaction chamber operating pressure is 100mmHg) distilling under reduced pressure, get rid of organic acid soln, no liquid to the microwave cavity is finished the microwave softened of spore powder and is handled.Its polysaccharide releasability sees Table 1.
Embodiment 3
Difference from Example 1 is:
1. the 1.5kg Ganoderma spore powder places the resonant mode microwave cavity;
2. get anhydrous acetic acid 2.8L, add water 1.2L and be made into acetic acid solution 4L;
3. get above-mentioned solution 4L, be added in the above-mentioned microwave cavity, fully stir and make even moistening;
3. above-mentioned material has been irradiated to liquid return under 1KW continuous microwave power, it is the organic acid soln vaporization, change pulse microwave power working method into, dutycycle is 15/5 second, and peak power 5KW is behind the maintenance 60min, evacuation (the reaction chamber operating pressure is 200mmHg) distilling under reduced pressure, get rid of organic acid soln, no liquid to the microwave cavity is finished the microwave softened of spore powder and is handled.Its polysaccharide releasability sees Table 1.
Embodiment 4
Difference from Example 1 is:
1. the 1.5kg Ganoderma spore powder places the resonant mode microwave cavity;
2. get anhydrous propanoic acid 0.85L, add water 0.15L and be made into propanoic acid solution 1L;
3. get above-mentioned solution 1L, be added in the above-mentioned microwave cavity, fully stir and make even moistening;
4. above-mentioned material has been irradiated to liquid return under 1KW continuous microwave power, it is the organic acid soln vaporization, change pulse microwave power working method into, dutycycle is 5/40 second, and peak power 2KW is behind the maintenance 100min, evacuation (the reaction chamber operating pressure is 400mmHg) distilling under reduced pressure, get rid of organic acid soln, no liquid to the microwave cavity is finished the microwave softened of spore powder and is handled.Its polysaccharide releasability sees Table 1.
Table 1 is the polysaccharide releasability comparable situation of microwave softened spore powder and unprocessed raw material among existing wall breaking technology and the embodiment 1～4:
| Raw material | Spore powder with crushed sporoderm | Embodiment 1 spore powder | Embodiment 2 spore powders | Embodiment 3 spore powders | Embodiment 4 spore powders | |
| Polysaccharide releasability (doubly) | 1 | 2.1 | 6.1 | 8.5 | 6.4 | 7.8 |
Claims (5)
1. the method that can discharge the Ganoderma spore powder effective ingredient is characterized in that: adopt the microwave softened processing mode, be specially: 1) the Ganoderma spore powder raw material is inserted in the microwave reaction chamber, add organic acid soln, fully stir and make even moistening; 2) microwave treatment applies microwave power, utilizes chitin and gelationus reaction in microwave reinforced organic acid soln and the sporoderm structure, and it is partly dissolved, and produces the nanoscale hole or the crackle of dense distribution on sporoderm; 3) organic acid soln is got rid of in distilling under reduced pressure;
It is that continuous microwave combines with pulse microwave that described microwave power applies mode, and using earlier continuous microwave irradiation, time is to reflux to organic acid soln, is converted to pulse microwave then, irradiation 5min～100min; Its reaction condition is as follows:
1) the quality power density of microwave power is 10 kilowatts of 1 kilowatt～every kilogram materials of every kilogram of material;
2) the reaction chamber operating pressure is 20mmHg～760mmHg;
3) the weight of material proportioning is a spore powder: organic acid soln=5/1～1/5;
Described organic acid soln is respectively that concentration is 5%～50% oxalic acid, 20%～99% formic acid, 20%～99% acetic acid or 20%～99% propanoic acid aqueous solution.
2. by the described method that can discharge the Ganoderma spore powder effective ingredient of claim 1, it is characterized in that: the quality power density is 5 kilowatts of 1 kilowatt～every kilogram materials of every kilogram of material under the described continuous microwave situation; The quality power density is 10 kilowatts of 2 kilowatts～every kilogram materials of every kilogram of material under the pulse microwave situation, and dutycycle is A/B, A=1 second～100 second wherein, B=1 second～100 second.
3. by claim 1 or the 2 described methods that can discharge the Ganoderma spore powder effective ingredient, it is characterized in that: described material is the mixture of Ganoderma spore powder and organic acid soln.
4. by the described method that can discharge the Ganoderma spore powder effective ingredient of claim 1, it is characterized in that: when the organic acid soln of described adding was oxalic acid solution, the removal that softening back adopts calcium ion to carry out oxalic acid was handled.
5. by the described method that can discharge the Ganoderma spore powder effective ingredient of claim 1, it is characterized in that: described microwave cavity can be travelling-wave-type microwave cavity or resonant mode microwave cavity.
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| CN102417545B (en) * | 2011-11-03 | 2013-07-24 | 沈阳科思高科技有限公司 | Extracting method for active polysaccharide in higher plant or edible and medicinal fungi |
| CN102391387B (en) * | 2011-11-07 | 2013-02-27 | 沈阳科思高科技有限公司 | Microwave chemical extraction method of active polysaccharide in higher plants or edible and medicinal fungi |
| CN110521837B (en) * | 2019-06-05 | 2022-12-02 | 吉林农业大学 | Functional chocolate tablet containing ganoderma lucidum spore powder and preparation method of functional chocolate tablet |
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