The method of a kind of ultrasonic wave-microwave synergistic extraction ganoderan
Technical field
The present invention relates to the edible mushrooms processing technique field, particularly ganoderan extractive technique field.
Background technology
Since the reform and opening-up, China's edible mushrooms processing development rapidly.National output was 60,000 tons in 1979, after the reform and opening-up, formed and produced and the exploitation upsurge; China's edible mushrooms annual production in 2006 has been increased to 1,400 ten thousand tons, accounts for 70% of the world, has become an important channel of increasing peasant income.And the annual demand to edible mushrooms in the whole world is also with 3%-5% speed increment.2003, edible fungi of china exported to 119 countries, and export volume reaches 43.32 ten thousand tons, and export volume has 12 in the countries and regions more than ten thousand tons. Japan, Hong Kong, Korea S, Germany, Canada, Malaysia, the U.S., Holland etc.Though China is the country of being familiar with edible mushrooms the earliest, because the industrialization starting is late, the edible mushrooms processing industry of China still has very big development space, especially in the deep processing of edible mushrooms.
Glossy ganoderma is Basidiomycetes, polyporaceae Ganoderma fungi, and the good reputation of " celestial grass " is just arranged in China from ancient times.Modern medicine study shows that glossy ganoderma is used for the treatment of liver, ephrosis, hypertension, and hyperlipidemia, neurasthenia, cardiovascular disorder and antitumor etc. all has good and clinical curative effect.Polysaccharide is one of main active principle of biologically active in the glossy ganoderma, and its nourishing function is one of focus of studying in the present protective foods and the action of drug factor.Existing result of study shows, the anti-tumor activity of glossy ganoderma is owing to have the ganoderan of ad hoc structure, and ganoderan also has significant anti-mutation except having raise immunity and suppressing the function of tumour, reducing blood-fat, blood sugar, effect such as antiviral.
At present, the ganoderan extracting method common solvent according to the available data report is water, diluted acid, diluted alkaline and dimethyl sulfoxide (DMSO) etc.Though dimethyl sulfoxide (DMSO) is a kind of good solvent that extracts polysaccharide, but cost an arm and a leg, big to the effective constituent loss, technological process is complicated, and workload is big, human factor is many, wayward, and the waste liquid that produces in producing pollutes harmful HUMAN HEALTH easily to environment, both be not suitable for suitability for industrialized production and application, do not met the trend of current industry development again; When extracting with diluted acid, seeking time short, temperature had better not be higher than 5 ℃, therefore, will consider refrigeration in the production, and this has just increased cost without doubt; Though do to extract the extraction yield that solvent can improve polysaccharide with diluted alkaline, but diluted alkaline has a significant impact to the biological activity of polysaccharide.In recent years, the scientific research personnel adopts new and high technologies such as microwave, ultrasonic wave, ultrasonic wave enzyme process that ganoderan has been carried out extracting experiment, the result shows, microwave, supersonic method and ultrasonic wave enzyme process can both shorten extraction time significantly, improve the extraction yield of polysaccharide, and extraction effect is better than conventional hot water extraction method.
In order to obtain more cost-effective ganoderan extracting method, the method for a kind of ultrasonic wave-microwave synergistic extraction ganoderan has been explored in this research.
Result of study shows, ultrasonic-microwave synergistic extraction method integrates microwave, ultrasonic extraction characteristics, both remedied ultrasonic wave and the microwave deficiency of independent extraction respectively, concentrate and kept the advantage of ultrasonic extraction or microwave extracting method simultaneously again, its outstanding advantage applies in the vibration homogenize, make each point is subjected in the sample media effect unanimity, alternative extraction solvent kind is many, the target extract is in extensive range, reduce the bonding force of target compound and sample matrices, it is big etc. that the acceleration target compound enters process, the processing sample size of solvent phase from solid phase.
Summary of the invention
The objective of the invention is: provide a kind of free from environmental pollution, production technique is simple, extraction time is short, extraction yield is high, practical more cost-effective method---ultrasonic-microwave synergistic extraction method for extracting preparation sesame polysaccharide.The method of a kind of ultrasonic wave-microwave synergistic extraction ganoderan.
To achieve these goals, concrete technical scheme of the present invention is:
The method of a kind of ultrasonic wave-microwave synergistic extraction ganoderan is characterized in that key step is followed successively by:
1), with Ganoderma sporophore oven dry, pulverize, sieve, the Ganoderma sporophore powder;
2), in the Ganoderma sporophore powder, add entry;
3) utilize ultrasonic wave-microwave synergistic extraction machine to extract;
4) after extraction is finished,, obtain containing the supernatant liquor of ganoderan through overcooling, centrifugation;
5) with this supernatant concentration to 1/2~1/3 of original volume, add dehydrated alcohol, make in the liquid alcohol volume content 70%~85%, under 4 ℃ of conditions, leave standstill to precipitation fully, filter then, filter gained solid phase vacuum lyophilization, promptly obtain ganoderan.
The method steps 1 of above-mentioned ultrasonic wave-microwave synergistic extraction ganoderan) in, after Ganoderma sporophore is dried in 50~60 ℃ of baking ovens, pulverizes, cross 20 orders~60 mesh sieves.
The method steps 2 of above-mentioned ultrasonic wave-microwave synergistic extraction ganoderan) in, add moisture in the Ganoderma sporophore powder after sieving, making the feed liquid weight ratio is 1:20~1:50.
The method steps 3 of above-mentioned ultrasonic wave-microwave synergistic extraction ganoderan) in, the processing parameter of ultrasonic wave-microwave synergistic extraction machine extraction is: ultrasonic wave 50W, microwave 10~400W, 60~80 ℃ of temperature, 10~60 minutes time.
The invention has the beneficial effects as follows: ultrasonic wave and microwave are organically combined, make full use of the high energy effect of cavitation effect of ultrasonic waves and microwave, proposed under the low-temperature atmosphere-pressure condition, to carry out the microwave-ultrasonic synergy and extracted ganoderan.In whole operating process that ganoderan extracts, except that using distilled water, pure water and food grade ethanol, do not add any harmful chemical reagent and carry out assisted extraction, free from environmental pollution, extraction process is simple, operating time short (only need 10~50 minutes), extraction efficiency height, is easy to industrialization.In addition, the by product in the ganoderan leaching process can be produced healthy complementary food such as functional type wine slightly through processing, and its major-minor product all is useful product, can bring into play productivity effect to greatest extent.
Embodiment
Further specify technology contents of the present invention and effect below by example.
Embodiment 1
Ganoderma sporophore is dried under 50 ℃ of conditions with baking oven, adopt Universalpulverizer that it is pulverized, cross 20 mesh sieves; Accurately take by weighing REISH 4g, add 80ml distilled water, in ultrasonic wave-microwave synergistic extraction machine, extract, ultrasonic wave 50w, (10~400W) regulate 80 ℃ of constant temperature, 20 minutes time to microwave power automatically; After extraction was finished, cooling was carried out centrifugation 20 minutes, and centrifugal speed 4000r/min filters, and obtains containing the supernatant liquor of ganoderan; Adopt Rotary Evaporators to be concentrated into 1/3 of original volume this supernatant liquor, add dehydrated alcohol, make that alcohol volume content left standstill 24 hours at 75%, 4 ℃ in the liquid, filter, filter gained solid phase vacuum lyophilization, obtain ganoderan 0.102g.Polysaccharide extract rate is 0.102/4=2.55%.
Embodiment 2
Use baking oven 50 ℃ of oven dry Ganoderma sporophore, adopt Universalpulverizer that it is pulverized, cross 30 mesh sieves; Accurately take by weighing REISH 3g, add 90ml distilled water, in ultrasonic wave-microwave synergistic extraction machine, extract, ultrasonic wave 50w, (10~400W) regulate 70 ℃ of constant temperature, 30 minutes time to microwave power automatically; After extraction was finished, cooling was carried out centrifugation 25 minutes, and centrifugal speed 4000r/min filters, and obtains containing the supernatant liquor of ganoderan; Adopt Rotary Evaporators to be concentrated into 1/3 of original volume this supernatant liquor, add dehydrated alcohol, make that alcohol volume content left standstill 24 hours at 80%, 4 ℃ in the liquid, filter, filter gained solid phase vacuum lyophilization, obtain ganoderan 0.084g.Polysaccharide extract rate is 0.084/3=2.8%.
Embodiment 3
Use baking oven 60 ℃ of oven dry Ganoderma sporophore, adopt Universalpulverizer that it is pulverized, cross 20 mesh sieves; Accurately take by weighing REISH 4g, add 160ml distilled water, in ultrasonic wave-microwave synergistic extraction machine, extract, ultrasonic wave 50w, (10~400W) regulate 60 ℃ of constant temperature, 40 minutes time to microwave power automatically; After extraction was finished, cooling was carried out centrifugation 20 minutes, and centrifugal speed 4000r/min filters, and obtains containing the supernatant liquor of ganoderan; Adopt Rotary Evaporators to be concentrated into 1/2 of original volume this supernatant liquor, add dehydrated alcohol, make that alcohol volume content left standstill 24 hours at 75%, 4 ℃ in the liquid, filter, filter gained solid phase vacuum lyophilization, obtain ganoderan 0.111g.Polysaccharide extract rate is 0.111/4=2.78%.
Embodiment 4
Use baking oven 50 ℃ of oven dry Ganoderma sporophore, adopt Universalpulverizer that it is pulverized, cross 40 mesh sieves; Accurately take by weighing REISH 4g, add 80ml distilled water, in ultrasonic wave-microwave synergistic extraction machine, extract, ultrasonic wave 50w, (10~400W) regulate 60 ℃ of constant temperature, 50 minutes time to microwave power automatically; After extraction was finished, cooling was carried out centrifugation 20 minutes, centrifugal speed 4000r/min,, filter, obtain containing the supernatant liquor of ganoderan; Adopt Rotary Evaporators to be concentrated into 1/3 of original volume this supernatant liquor, add dehydrated alcohol, make that alcohol volume content left standstill 24 hours at 85%, 4 ℃ in the liquid, filter, filter gained solid phase vacuum lyophilization, obtain ganoderan 0.115g.Polysaccharide extract rate is 0.115/4=2.88%.
Embodiment 5
Use baking oven 55 ℃ of oven dry Ganoderma sporophore, adopt Universalpulverizer that it is pulverized, cross 40 mesh sieves; Accurately take by weighing REISH 3g, add 90ml distilled water, in ultrasonic wave-microwave synergistic extraction machine, extract, ultrasonic wave 50w, (10~400W) regulate 80 ℃ of constant temperature, 50 minutes time to microwave power automatically; After extraction was finished, cooling was carried out centrifugation 20 minutes, centrifugal speed 4000r/min,, filter, obtain containing the supernatant liquor of ganoderan; Adopt Rotary Evaporators to be concentrated into 1/3 of original volume this supernatant liquor, add dehydrated alcohol, make that alcohol volume content left standstill 24 hours at 70%, 4 ℃ in the liquid, filter, filter gained solid phase vacuum lyophilization, obtain ganoderan 0.086g.Polysaccharide extract rate is 0.086/3=2.87%.
Embodiment 6
Use baking oven 55 ℃ of oven dry Ganoderma sporophore, adopt Universalpulverizer that it is pulverized, cross 60 mesh sieves; Accurately take by weighing REISH 3g, add 150ml distilled water, in ultrasonic wave-microwave synergistic extraction machine, extract, ultrasonic wave 50w, (10~400W) regulate 70 ℃ of constant temperature, 60 minutes time to microwave power automatically; After extraction was finished, cooling was carried out centrifugation 20 minutes, centrifugal speed 4000r/min,, filter, obtain containing the supernatant liquor of ganoderan; Adopt Rotary Evaporators to be concentrated into 1/3 of original volume this supernatant liquor, add dehydrated alcohol, make that alcohol volume content left standstill 24 hours at 70%, 4 ℃ in the liquid, filter, filter gained solid phase vacuum lyophilization, obtain ganoderan 0.088g.Polysaccharide extract rate is 0.088/3=2.93%.