CN102417545B - Extracting method for active polysaccharide in higher plant or edible and medicinal fungi - Google Patents
Extracting method for active polysaccharide in higher plant or edible and medicinal fungi Download PDFInfo
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Abstract
The invention relates to an extracting method for an active polysaccharide in a higher plant or edible and medicinal fungi. The extracting method comprises the following steps: adding an organic acid or an organic or inorganic mixed acid solution in raw materials; heating the raw materials, utilizing the molecules of the organic acid to separate the active polysaccharide from the raw materials, and moderately cutting off glucosidic bonds of macromolecular active polysaccharide of the plant, thereby realizing local degradation; adopting a distilling, filtering or centrifuging method to remove most acid solution in the raw materials, and then washing with an organic solvent, thereby removing few remained acid solutions; extracting by adding water with the volume being 5-15 times that of the raw materials into the raw materials processed with the organic acid, and after concentrating an extracting solution, settling alcohol, thereby obtaining rough active polysaccharide; dissolving the rough active polysaccharide in de-ionized water with the volume being 5-15 times that of the rough active polysaccharide; adjusting pH of the solution to be neutral; and centrifuging, dialyzing or film-separating liquid supernatant, and then concentrating and drying, thereby obtaining an active polysaccharide product with low average molecular weight, narrow molecular weight distribution of the polysaccharide and excellent water solubility. Various defects, such as water consumption and energy consumption caused by technology, low yield of products, and the like, are overcome.
Description
Technical field
The present invention relates to the extraction field of active ingredient of natural product, is the highly effective extraction method of active polysaccharide in a kind of higher plant or the edible and medicinal fungi class specifically.
Background technology
Polysaccharide is by the natural macromolecular compound of a plurality of monose molecules with the glycosidic link be combined into, is one of base substance that constitutes life.Recent two decades comes, development along with molecular biology and cytobiology, it is found that polysaccharide has the various biological function, polysaccharide and conjugate thereof have participated in the various vital movements in the cell, as cell-specific identification, form the acceptor of various antigens of cell surface and medicine, immune cell activated etc., therefore, polysaccharide research has caused the great interest of people.Polysaccharide generally can be divided into fungus polysaccharide, higher plant polysaccharide, animal polysaccharide, algal polysaccharides, bacterial polysaccharides etc. by its source.Wherein edible and medicinal fungi polysaccharide and higher plant polysaccharide have long applicating history in China, and resource is very abundant, have now become the focus of paying close attention to and studying.Modern pharmacology studies show that, this two classes polysaccharide has extremely important and special physiologically active, is promoting immunity of organisms, antibiotic, antiviral, parasiticide, antitumor, radioprotective, antithrombotic, anticoagulation, anti-ageing, anti-inflammatory, blood fat reducing and improving aspect such as breeding performonce fo animals that clear and definite effect is all arranged.And most of polysaccharide do not have direct cytotoxicity, and are many even can take for a long time.Higher plant and edible and medicinal fungi class active polysaccharide have become at present one of health care resource of tool development prospect.
The biological activity of polysaccharide has determined the utility value of polysaccharide to a great extent.The water-soluble etc. of formation component, constituted mode and the space conformation of polysaccharide, the molecular weight of polysaccharide size and distribution range and polysaccharide is to influence the bioactive principal element of polysaccharide.A large amount of studies show that active polysaccharide molecular weight size is that it possesses bioactive prerequisite.The active polysaccharide molecular weight is big more, and the molecule apparent volume is big more, is unfavorable for that polysaccharide leap cell multiplex film obstacle enters performance biologic activity in the organism.And the water-soluble of polysaccharide is another essential condition of its performance biologic activity.
Because the structure of polysaccharide is very complicated, causes its resulting anomaly difficulty, active polysaccharide is all got by natural product extraction at present.Higher plant polysaccharide and edible and medicinal fungi polysaccharide are exactly extraction separation from sporophore, mycelium and the hypha fermentation liquid of the different sites of different plants or kindred plant and edible fungus and medicinal fungi.The extraction separation purifying of polysaccharide does not still have at present generally acknowledged, effective, unified method, existing processes generally can be summarized as water extraction, sour formulation, alkaline extraction, salt formulation and enzyme process assisted extraction etc.These methods are no matter in spatter property, energy consumption and the material consumption of polysaccharide extraction efficiency, production process, still exist obvious deficiency at aspects such as active polysaccharide controls, the scientific and technological content of gained polysaccharide product is not high yet, be in particular in: polysaccharide material purity is low, poorly water-soluble, molecular weight too disperses and be difficult to obtain aspects such as homogeneous component, has restricted the value added applications of polysaccharide.Specifically, existing method mainly contains following problem:
The general length consuming time of water extract method, the energy consumption height, the extraction solvent usage quantity is big, polysaccharide extract rate is low;
Soda acid extracts all bad control of used inorganic acid, alkaline consumption and reaction times, very easily destroys the activity of polysaccharide molecule, even can make polysaccharide resolve into the littler pigment molecular of molecular weight, has increased the weight of subsequent decolorization work.And, after reaction finishes, also to accomplish neutralization rapidly or dialysis rapidly, otherwise can cause product contamination acid solution alkali lye, increase the insecurity that product is used for the food and medicine healthcare products.In addition, the inorganic acid alkali that use can not be degraded causes serious environmental to pollute easily during scale operation.
Shortcomings such as there is easy inactivation in the enzyme price general charged costliness in the enzyme process assisted extraction toward contact, and the life-span is short, and purity is not enough.The optimum temps of enzyme is often in a very little scope in enzymolysis process, the minor fluctuations of reaction conditions, the activity of enzyme is reduced greatly, so Enzymatic Extraction is higher to requirement for experiment condition, even requires to carry out the ten minutes complicated pretreatment extracting raw material.The Enzymatic Extraction technology will be used for industrialized polysaccharide to be extracted, the further further investigation of still needing.
Cause these difficult reasons to have a lot.In general, higher plant, fungi activity polysaccharide molecular weight are all very big, and be water-soluble also relatively poor.Its content in plant material is lower, and distribution and distribution situation complexity, and some is unbound state, and other polymers such as some and protein, hemicellulose are combined into complicated conjugate, and some is present in the tenuigenin, and some wrapped folder is in cell walls.The main component of plant cell wall is a Mierocrystalline cellulose, also comprises materials such as hemicellulose, pectin substance, xylogen in addition.Mierocrystalline cellulose has the supramolecule rock steady structure in highly crystalline district, is difficult to hydrolysis.Extraction method commonly used can only be flooded for a long time by a large amount of solvents, and it is swollen that plant cell wall is fully expanded, and its dense construction becomes loose, reduce effective constituent in the born of the same parents to the resistance to mass transfer of extracting Medium Diffusion.Therefore traditional extracting method needs a large amount of solvents and long time.Simple solvent impregnated can only the stripping born of the same parents in the free polysaccharide, powerless for cell wall polysaccharide, so extraction yield is generally not high.
If in the extraction of higher plant or edible medicinal fungus active polysaccharide, use the moderate organic acid system of acidity, just might pass through the CONTROL PROCESS condition, make materials such as Mierocrystalline cellulose in the raw material, hemicellulose, pectin substance that the part degraded take place, thereby change the structural sheet of plant cell wall, when making the rapid stripping of intracellular polyse, cell wall polysaccharides is also discharged as early as possible.
Summary of the invention
The present invention is just relating to the method for a kind of like this high efficiency extraction higher plant, edible and medicinal fungi class active polysaccharide, promptly by the control reaction conditions, utilize of the effect of organic acid system to polymer substances such as higher plant, edible and medicinal fungi cell walls Mierocrystalline cellulose, hemicellulose, pectin substances, realize the high efficiency extraction of intracellular polyse and cell wall polysaccharide, and appropriateness is cut off the glycosidic link in the target polysaccharide molecule, the active polysaccharide product of obtained performance, structure uniqueness is realized the water saving of technological process, energy-conservation purpose simultaneously.
In order to realize above-mentioned purpose, the technical solution used in the present invention is as follows:
The extracting method of active polysaccharide in a kind of higher plant or the edible and medicinal fungi class adopts the organic acid system that higher plant, edible and medicinal fungi class raw material are handled, and then adopts aqueous extraction-alcohol precipitation technology, obtains the water-soluble active polysaccharide; Be specially:
1) pretreated raw material is inserted in the extraction vessel, add organic acid or organic inorganic mixed acid solution, fully stir make evenly wetting;
2) add thermal material, the weight of material proportioning is that raw material/organic acid soln or organic and inorganic mixed acid solution are 5/1-1/5, Heating temperature is 50～150 ℃, soaking time is 10-180min, the extraction vessel operating pressure is 20mmHg-760mmHg, utilizes the effect between organic acid molecule and higher plant, the edible and medicinal fungi cell walls organic polymer material, and active polysaccharide is separated from raw material, and the glycosidic link of appropriateness cut-out macromolecule polysaccharide, realize its part degraded;
3) adopt organic solvent washing to remove the acid solution of small portion of residual, finish the organic acid of raw material and handle;
4) through organic acid-treated raw material, adding about 5-15 times of volume water extracts, extracting solution concentrates the back alcohol precipitation, promptly add ethanol in the extracting solution after concentrating, make water-soluble but be insoluble to the alcoholic acid polysaccharide precipitation, the alcoholic acid add-on is to make polysaccharide precipitation complete, is generally 3 to 6 times of aqueous solution volume, and the collecting precipitation part can obtain active Crude polysaccharides;
5) active Crude polysaccharides is dissolved in the deionized water of 5-15 times of volume, and the pH of regulator solution is extremely neutral, centrifugal treating, and supernatant liquor concentrates behind dialysis or membrane sepn, and drying obtains active polysaccharide.Semi-permeable membranes is adopted in dialysis, and the selection of semi-permeable membranes is decided according to the molecular weight size of polysaccharide product.
Organic acid soln is selected from the propionic acid aqueous solution that oxalic acid that mass percent concentration is 5%-50%, formic acid that mass percent concentration is 10%-99%, acetate that mass percent concentration is 10%-99% and mass percent concentration be 10%-99% a kind of.
Mineral acid is selected from a kind of in hydrochloric acid, sulfuric acid, nitric acid and the phosphoric acid.The add-on of mineral acid is to make the mass percent concentration of mineral acid in the organic and inorganic nitration mixture reach 0.1%-15%.
When organic acid is a organic acid in oxalic acid or the organic and inorganic nitration mixture when being oxalic acid, handle the back in the step 3) and adopt organic solvent washing to remove residual oxalic acid or nitration mixture; Organic acid is that the organic acid in formic acid, acetate, propionic acid solution or the organic and inorganic nitration mixture is when being formic acid, acetate, propionic acid solution, handle the back and adopt distillation, pumping rate or centrifugation to remove most acid solution earlier, adopt organic solvent to carry out the acid that thorough washing is removed small portion of residual then.
Described organic solvent is selected from alcohol, acetone a kind of of C1-C3.
Pretreated method described in the step 1) can be with after raw material drying, removal of impurities, the mechanical disintegration, adopt alcohol or the ethyl acetate of ethanol, sherwood oil, C1-C3 to carry out extracting, obtain wherein volatile oil, flavonoid, triterpenes, saponins fat-soluble active substance, the extracting residue is after drying as going on foot raw material down.
Pretreatment process can also be with after raw material drying, removal of impurities, the mechanical disintegration as following step raw material.Order number to mechanical disintegration does not require, adopt this method after, the fat-soluble active substance in the raw material can obtain when the organic solvent of step 3) is handled.
Higher plant comprises the Radix Astragali among the present invention, matrimony vine, Ginkgo Leaf, pawpaw, Japanese Honeysuckle, Radix Angelicae Sinensis, dried orange peel, ephedra sinica, rhizome of chuanxiong, Rhizome of Grass leaf Sweelflag, garlic, Sharpleaf Galangal Fruit, the root of Dahurain angelica, tarragon, the root of Chinese wild ginger, Herba Cistanches, arrow-leaved oleaster, folium eucalypti, Herba Houttuyniae, Glossy Privet Fruit, notopterygium root, genseng, pseudo-ginseng, Herba Pileae Scriptae, Semen Plantaginis, Princes-feather Fruit, lilac daphne, Buddha's hand, White Mulberry Root-bark, loranthus parasiticus, the root of large-flowered skullcap, Herba Epimedii, tealeaves, Root of Kirilow Rhodiola, aloe, oat, konjaku, Chinese yam, rhizoma Gastrodiae, radix bupleuri, the flower of Radix Et Caulis Acanthopanacis Senticosi etc., leaf, seed, skin, fruit, root, stem class raw material; Described edible and medicinal fungi is selected from the fungus sporophore of glossy ganoderma, auricularia auriculajudae, mushroom, umbellate pore furgus, white fungus, Grifola frondosa, Poria cocos, rainbow conk, Hericium erinaceus (Bull. Ex Fr.) Pers., Cordyceps sinensis or mycelium etc.The present invention has enumerated above-mentioned plant, but is not limited to listed plant, and for other higher plants, method of the present invention still is suitable for, and can obtain the obtained effect of the present invention.
Except containing active polysaccharide, also contain many other class active substances, in higher plant, the edible and medicinal fungi as triterpenes, flavonoid, saponins etc.In present method implementation process, tailor-make processing step targetedly, i.e. difference on solvability according to these activeconstituentss and polysaccharide, use the different solvent extraction of polarity respectively before organic acid is handled or after the organic acid processing, organic solvent of for example selecting for use in pre-treatment such as sherwood oil, ethyl acetate or low-molecular-weight alcohol all have dissimilar polarity respectively.As extracting volatile oil with the little sherwood oil of polarity among the embodiment, the alcohol big slightly with polarity extracts flavones etc., extracts polysaccharide with the water of polarity maximum, thereby realizes the comprehensive utilization of higher plant activeconstituents.
The principle of the invention is: under certain processing condition, suitable organic acid system can and the organic macromolecule material (comprising Mierocrystalline cellulose, hemicellulose and pectin) of flower, leaf, fruit, seed, skin, tubers and the medicinal fungi sporophore of higher plant or mycelium raw material cell wall between the generation effect, target polysaccharide and plant material matrix are separated, utilized water that water-soluble polysaccharide is extracted again.In addition, utilize the organic acid system, can also be under gentle relatively condition, glycosidic link in the fracture polysaccharide molecule of appropriateness, the molecular structure of excessive, the water-soluble relatively poor target polysaccharide of those molecular weight is suitably degraded, improve its inherent structure and physico-chemical property, obtain the high added value active polysaccharide.Simultaneously, because the raw material cell wall structural sheet changes, extract water loss and significantly reduce.Like this, not only significantly improved the extraction yield of vegetable polysaccharides, and reduced the extraction water, the energy consumption when having reduced concentrated extracting solution has been simplified technological process.Use organic acid system replaces inorganic strong acid solution and the inorganic strong alkali solution in the original technology in the novel process, makes reaction conditions become gentle, handy, has reduced the destruction to the macromolecule polysaccharide active fragments.Used organic solution is easily from feed separation and can use repeatedly, reduced to the polysaccharide product and to the pollution of surrounding environment.Simultaneously, the controlled reduction of molecular weight of product, favourable its bioactive expression.Therefore, the invention provides the highly effective extraction method of active polysaccharide in a kind of higher plant or the edible and medicinal fungi class.
Compared with prior art, the present invention has more following advantage:
1. water saving, reduction of discharging, energy-saving effect are remarkable; Use organic acid system replaces inorganic strong acid solution and the inorganic strong alkali solution in the original technology, and is little to the active fragments destruction of polysaccharide molecule, and solvent recuperation is simple, and environmental pollution is little.
2. be compared to traditional technology, novel process polysaccharide product yield is significantly improved, and polysaccharide content also is significantly improved.
3. directly realize the degraded of polysaccharide molecule appropriateness in the leaching process, obtain that molecular-weight average is low, the polysaccharide product of polysaccharide molecular weight narrowly distributing, good water solubility.Novel process polysaccharide product has special advantages as medicine and healthcare product exploitation.
Description of drawings
Fig. 1 is the technological process synoptic diagram of the embodiment of the invention 1.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment 1
Shown in the technological process synoptic diagram as shown in Figure 1, detailed process is as follows:
1) Radix Astragali of getting after 1.5kg drying, removal of impurities, the mechanical disintegration places the Chinese herbal medicine extracting container, adds 10L ethanol, and heating and refluxing extraction 1 hour repeats said process once;
2) filter, merge twice filtrate and underpressure distillation and reclaim ethanol, must be rich in the pure medicinal extract of fat-soluble active ingredients such as flavones, saponin(e, tonka bean camphor, the filter residue partially desiccated is standby;
3) get step 2) in the oven dry after filter residue partly place extraction vessel;
4) get oxalic acid 180g, add water 2.0L and be made into oxalic acid solution;
5) get above-mentioned steps 4) in oxalic acid solution 2L, be added in the extraction vessel in the step 3), fully stir and make the evenly wetting mixture that obtains of filter residue;
6) mixture of step 5) is heated to 100 ℃, behind the insulation 20min, carries out underpressure distillation, absence of liquid to the extraction vessel.
7) add dehydrated alcohol 5L in the step 6) in the extraction vessel, fully stir, filter.Ethanol and oxalic acid are reclaimed in the filtrate distillation, are organic acid after the filter residue and drying and handle the Radix Astragali.
8) get the organic acid processing Radix Astragali 100 grams in the step 7), put into the beaker of 1L, add 500ml distilled water, in 70 ℃ hot water bath, extract 40min, filter, repeat said process 1 time, merge filtrate twice.
9) filtrate concentrates the back alcohol precipitation in the step 8), adds ethanol to precipitation and separates out fully, carries out drying after the precipitate and separate, obtains active Crude polysaccharides product.
10) the active Crude polysaccharides product of step 9) adds distilled water 1L dissolving, regulates pH to neutral with sodium hydroxide solution, is that 1000 semi-permeable membranes is dialysed with molecular weight cut-off.
11) dialysis back polysaccharide soln lyophilize in the step 10) gets the active polysaccharide product.
The calculated activity polysaccharide extract rate is also measured polysaccharide content.Polysaccharide extract rate is the percentage ratio of the mass ratio of product and higher plant raw material, and polysaccharide content adopts sulfuric acid-phynol method to measure.Polysaccharide molecular weight distributes and adopts gel chromatograph to measure.Data such as polysaccharide extract rate, polysaccharide content, polysaccharide molecular weight distribution and extraction water consumption see Table 1.
Embodiment 2
Difference from Example 1 is:
1) pawpaw places extraction vessel after 1.5kg drying, removal of impurities, the mechanical disintegration;
2) get anhydrous acetic acid 0.8L, add water 0.15L, add mass percent concentration and be 5% dilute hydrochloric acid 0.05L, be made into acetate hydrochloric acid mixed acid solution 1L;
3) get step 2) middle mixed acid solution 1L, be added in the extraction vessel of step 1), fully stir and make the evenly wetting mixture that obtains;
4) mixture with step 3) is heated to 80 ℃, behind the insulation 60min, carries out underpressure distillation, absence of liquid to the extraction vessel.
5) be 95% ethanolic soln with the mass percent concentration that adds 5L in the extraction vessel in the step 4), fully stir that filter, the pure medicinal extract that ethanol can be rich in the pawpaw flavones is reclaimed in the filtrate distillation, is organic acid after the filter residue part drying and handles pawpaw.
6) get organic acid pre-treatment pawpaw 100 grams, put into the beaker of 1L, add 500ml distilled water, in 70 ℃ hot water bath, extract 40min, filter, repeat said process 1 time, merge filtrate twice.
7) filtrate concentrates the back alcohol precipitation in the step 6), adds ethanol to precipitation and separates out fully, carries out drying after the precipitate and separate, obtains active Crude polysaccharides product.
8) the active Crude polysaccharides product of step 7) adds distilled water 1L dissolving, regulates pH to neutral with sodium hydroxide solution, is that 3000 semi-permeable membranes is dialysed with molecular weight cut-off.
9) dialysis back polysaccharide soln lyophilize in the step 8) gets the active polysaccharide product.
The calculated activity polysaccharide extract rate is also measured polysaccharide content.Polysaccharide extract rate is the percentage ratio of the mass ratio of product and higher plant raw material, and polysaccharide content adopts sulfuric acid-phynol method to measure.Polysaccharide molecular weight distributes and adopts gel chromatograph to measure.Data such as polysaccharide extract rate, polysaccharide content, polysaccharide molecular weight distribution and extraction water consumption see Table 1.
Embodiment 3
Difference from Example 1 is:
1) Radix Angelicae Sinensis after 1.5kg drying, removal of impurities, the pulverizing places extraction vessel, adds the 7L sherwood oil, and heating and refluxing extraction 1 hour repeats said process once;
2) filter, merge twice filtrate and underpressure distillation and reclaim sherwood oil, can get Radix Angelicae Sinensis volatile oil, standby behind the Radix Angelicae Sinensis filter residue partially desiccated;
3) dried Radix Angelicae Sinensis filter residue partly places extraction vessel step 2), adds 10L ethanol, and heating and refluxing extraction 1 hour repeats said process once;
4) filter, merge twice filtrate and underpressure distillation and reclaim ethanol, must be rich in the pure medicinal extract of Radix Angelicae Sinensis flavones, the filter residue partially desiccated is standby;
5) get the Radix Angelicae Sinensis filter residue of drying in the step 4) and place extraction vessel;
6) get anhydrous propionic acid 0.85L, add water 0.15L and be made into propionic acid solution 1L;
7) get propionic acid solution 1L in the step 6), be added in the extraction vessel of step 5), fully stir and make even wetting formation mixture;
8) the mixture heat to 130 of step 7) ℃, behind the insulation 100min, the cooling material is to room temperature, the most of propionic acid solution of centrifugal removal, solid part is put back in the extraction vessel.
9) adding mass percent concentration in the extraction vessel in the step 8) is 90% ethanolic soln 5L, and fully agitator treating filters, and filtrate recycling ethanol is organic acid and handles Radix Angelicae Sinensis after the filter residue part drying.
10) get organic acid processing Radix Angelicae Sinensis 100 grams in the step 9), put into the beaker of 1L, add 500ml distilled water, in 70 ℃ hot water bath, extract 40min, filter, repeat said process 1 time, merge filtrate twice.
11) filtrate concentrates the back alcohol precipitation in the step 10), adds ethanol to precipitation and separates out fully, carries out drying after the precipitate and separate, obtains active Crude polysaccharides product.
12) the active Crude polysaccharides product of step 11) adds distilled water 1L dissolving, regulates pH to neutral with sodium hydroxide solution, is that 3000 semi-permeable membranes is dialysed with molecular weight cut-off.
13) dialysis back polysaccharide soln lyophilize in the step 12) gets the active polysaccharide product.
The calculated activity polysaccharide extract rate is also measured polysaccharide content.Polysaccharide extract rate is the percentage ratio of the mass ratio of product and higher plant raw material, and polysaccharide content adopts sulfuric acid-phynol method to measure.Polysaccharide molecular weight distributes and adopts gel chromatograph to measure.Data such as polysaccharide extract rate, polysaccharide content, polysaccharide molecular weight distribution and extraction water consumption see Table 1.
Embodiment 4
1) Ganoderma sporophore of getting after the dry removal of impurities of 1.5kg, the mechanical disintegration places extraction vessel, adds the 10L dehydrated alcohol, and heating and refluxing extraction 1 hour repeats said process once;
2) filter, merge twice filtrate and underpressure distillation and reclaim ethanol, must be rich in the pure medicinal extract of Ganoderma triterpenoids, the filter residue partially desiccated is standby;
3) get oxalic acid 100g, add water 2.0L and be made into oxalic acid solution;
4) get oxalic acid solution 2L, be added in the extraction vessel, fully stir and make the even wetting formation material of filter residue;
5) material of step 4) is heated to 100 ℃, behind the insulation 20min, carries out underpressure distillation, and absence of liquid to the extraction vessel is finished the organic acid pre-treatment of Ganoderma sporophore.
6) through adding dehydrated alcohol 5L among the pretreated Ganoderma sporophore 1.5kg, fully stir, filter.Ethanol and oxalic acid are reclaimed in the filtrate distillation, are organic acid after the filter residue and drying and handle Ganoderma sporophore.
7) get organic acid processing Ganoderma sporophore 100 grams in the step 6), put into the beaker of 1L, add 500ml distilled water, in 70 ℃ hot water bath, extract 40min, filter, repeat said process 1 time, merge filtrate twice.
8) filtrate concentrates the back alcohol precipitation in the step 7), specifically is to add ethanol, adds alcoholic acid amount polysaccharide precipitation to the solution and separates out fully, carries out drying after the precipitate and separate, obtains active Crude polysaccharides product.
9) the active Crude polysaccharides product of step 10) adds distilled water 1L dissolving, regulates pH to neutral with sodium hydroxide solution, is that 2000 semi-permeable membranes is dialysed with molecular weight cut-off.
10) dialysis back polysaccharide soln lyophilize in the step 9) gets the active polysaccharide product.
The calculated activity polysaccharide extract rate is also measured polysaccharide content.Polysaccharide extract rate is the percentage ratio of the mass ratio of product and higher plant raw material, and polysaccharide content adopts sulfuric acid-phynol method to measure.Polysaccharide molecular weight distributes and adopts gel chromatograph to measure.Data such as polysaccharide extract rate, polysaccharide content, polysaccharide molecular weight distribution and extraction water consumption see Table 1.
Embodiment 5
Difference from Example 1 is:
1) get the removal of impurities of 1.5kg drying, the black fungus sporophore after pulverizing places extraction vessel;
2) get anhydrous formic acid 1L, add water 0.45L, add mass percent concentration and be 10% sulphuric acid soln and be made into formic acid-sulfuric acid mixed acid solution 1.5L;
3) get above-mentioned solution 1.5L, be added in the said extracted container, fully stirring makes evenly wetting;
4) above-mentioned material is heated to 110 ℃, behind the insulation 20min, carries out underpressure distillation, gets rid of organic acid soln, and absence of liquid to the extraction vessel is finished the organic acid pre-treatment of black fungus sporophore.
5) through adding dehydrated alcohol 5L among the pretreated black fungus sporophore 1.5kg, fully stir, filter.Ethanol and oxalic acid are reclaimed in the filtrate distillation, are organic acid pre-treatment black fungus sporophore after the filter residue and drying.
6) get above-mentioned pre-treatment black fungus sporophore 100 grams, put into the beaker of 1L, add 500ml distilled water, in 70 ℃ hot water bath, extract 40min, filter, repeat said process 1 time, merge filtrate twice.
7) filtrate concentrates the back alcohol precipitation in the step 6), adds ethanol to precipitation and separates out fully, carries out drying after the precipitate and separate, obtains active Crude polysaccharides product.
8) the active Crude polysaccharides product of step 7) adds distilled water 1L dissolving, regulates pH to neutral with sodium hydroxide solution, is that 15000 semi-permeable membranes is dialysed with molecular weight cut-off.
9) dialysis back polysaccharide soln lyophilize in the step 8) gets the active polysaccharide product.
The calculated activity polysaccharide extract rate is also measured polysaccharide content.Polysaccharide extract rate is the percentage ratio of the mass ratio of product and higher plant raw material, and polysaccharide content adopts sulfuric acid-phynol method to measure.Polysaccharide molecular weight distributes and adopts gel chromatograph to measure.Data such as polysaccharide extract rate, polysaccharide content, polysaccharide molecular weight distribution and extraction water consumption see Table 1.
Embodiment 6
Difference from Example 1 is:
1) get the removal of impurities of 1.5kg drying, the mushroom fruiting body after pulverizing places extraction vessel;
2) get anhydrous acetic acid 0.8L, add water 0.2L and be made into acetic acid solution 1L;
3) get step 2) acetic acid solution 1L, be added in the extraction vessel of step 1), fully stir and make material evenly wetting;
4) material with step 3) is heated to 80 ℃, behind the insulation 60min, carries out underpressure distillation, gets rid of organic acid soln, and absence of liquid to the extraction vessel is finished the organic acid pre-treatment of mushroom fruiting body.
5) through adding anhydrous methanol 5L among the pretreated mushroom fruiting body 1.5kg, fully stir, filter.Methyl alcohol is reclaimed in the filtrate distillation, is organic acid pre-treatment Ganoderma sporophore after the filter residue and drying.
6) get step 5) organic acid pre-treatment mushroom fruiting body 100 grams, put into the beaker of 1L, add 500ml distilled water, in 70 ℃ hot water bath, extract 40min, filter, repeat said process 1 time, merge filtrate twice.
7) filtrate concentrates the back alcohol precipitation in the step 6), adds ethanol to precipitation and separates out fully, carries out drying after the precipitate and separate, obtains active Crude polysaccharides product.
8) the active Crude polysaccharides product of step 7) adds distilled water 1L dissolving, regulates pH to neutral with sodium hydroxide solution, is that 8000 semi-permeable membranes is dialysed with molecular weight cut-off.
9) dialysis back polysaccharide soln lyophilize in the step 8) gets the active polysaccharide product.
The calculated activity polysaccharide extract rate is also measured polysaccharide content.Polysaccharide extract rate is the percentage ratio of the mass ratio of product and higher plant raw material, and polysaccharide content adopts sulfuric acid-phynol method to measure.Polysaccharide molecular weight distributes and adopts gel chromatograph to measure.Data such as polysaccharide extract rate, polysaccharide content and extraction water consumption see Table 1.
Embodiment 7
Difference from Example 1 is:
1) the umbellate pore furgus sporophore after 1.5kg drying removal of impurities, the pulverizing places extraction vessel;
2) get anhydrous formic acid 0.85L, add water 0.15L and be made into formic acid solution 1L;
3) get step 2) formic acid solution 1L, be added in the step 1) extraction vessel, fully stir and make even wetting material;
5) the step 3) material is heated to 130 ℃, behind the insulation 100min, stops heating, and is cooled to room temperature, and organic acid soln is got rid of in press filtration, and solid part is put back in the extraction vessel, finishes the organic acid pre-treatment of umbellate pore furgus sporophore.
6) through adding dehydrated alcohol 5L among the umbellate pore furgus sporophore 1.5kg of step 5), fully stir, filter.Ethanol is reclaimed in the filtrate distillation, is organic acid pre-treatment umbellate pore furgus sporophore after the filter residue and drying.
7) get organic acid pre-treatment umbellate pore furgus sporophore 100 gram of step 6), put into the beaker of 1L, add 500ml distilled water, in 70 ℃ hot water bath, extract 40min, filter, repeat said process 1 time, merge filtrate twice.
8) filtrate concentrates the back alcohol precipitation in the step 7), adds ethanol to precipitation and separates out fully, carries out drying after the precipitate and separate, obtains active Crude polysaccharides product.
9) the active Crude polysaccharides product of step 7) adds distilled water 1L dissolving, regulates pH to neutral with sodium hydroxide solution, is that 3000 semi-permeable membranes is dialysed with molecular weight cut-off.
10) dialysis back polysaccharide soln lyophilize in the step 9) gets the active polysaccharide product.
The calculated activity polysaccharide extract rate is also measured polysaccharide content.Polysaccharide extract rate is the percentage ratio of the mass ratio of product and higher plant raw material, and polysaccharide content adopts sulfuric acid-phynol method to measure.Polysaccharide molecular weight distributes and adopts gel chromatograph to measure.Polysaccharide extract rate, polysaccharide content (purity of resulting solid polysaccharide) and extraction water consumption data such as (mass ratioes of material and institute's water) see Table 1.
Table 1 is polysaccharide product extraction yield among the embodiment 1-5, polysaccharide content, polysaccharide molecular weight distributes and polysaccharide extracts the water loss comparable situation
Result and analysis
According to existing data and our control experiment result in the past, when higher plant and edible and medicinal fungi class active polysaccharide adopt conventional water extracting method, the extraction yield of general polysaccharides product is below 4wt%, that have even lower, such as Auricularia polycose, its polysaccharide extract rate＜1wt% during water extraction, extract water loss generally about 30 times even bigger, the black fungus water loss will reach 50 times, and the molecular weight of polysaccharide product does not generally wait from several ten thousand to hundreds of thousands of, such as lentinan, when adopting conventional water extracting method, the molecular weight of products obtained therefrom is at 60000-110000, and the astragalus polysaccharides molecular weight is at 10000-80000, and the molecular weight of Auricularia polycose is also about 100000, in addition, the polysaccharide degree of purity of production is also lower, and when adopting conventional water extraction such as ganoderan, polysaccharide content only is 30-40%.And can find out that from this patent the foregoing description extracting water loss by method of the present invention is reduced greatly, play the purpose of energy-saving and emission-reduction; Polysaccharide product molecular-weight average is low, molecular weight distribution is narrower, and the polysaccharide product yield is significantly improved, and polysaccharide content also is significantly improved.
Claims (5)
1. the extracting method of active polysaccharide in higher plant or the edible and medicinal fungi class is characterized in that: adopt the organic acid system that higher plant, edible and medicinal fungi class raw material are handled, and then adopt aqueous extraction-alcohol precipitation technology, obtain the water-soluble active polysaccharide; Be specially:
1) pretreated raw material is inserted in the extraction vessel, add organic acid or organic inorganic mixed acid solution, fully stir make evenly wetting;
The mass percent concentration of mineral acid is 0.1%-15% in the described organic and inorganic nitration mixture;
Described mineral acid is selected from a kind of in hydrochloric acid, sulfuric acid, nitric acid and the phosphoric acid;
Described organic acid soln is selected from a kind of in the propionic acid aqueous solution that oxalic acid that mass percent concentration is 5%-50%, formic acid that mass percent concentration is 10%-99%, acetate that mass percent concentration is 10%-99% and mass percent concentration be 10%-99%;
When organic acid is oxalic acid solution, handles the back and adopt organic solvent washing to remove residual oxalic acid or nitration mixture; When described organic acid is formic acid, acetate, propionic acid solution, handles the back and adopt distillation, suction filtration or centrifugation to remove most acid solution, adopt organic solvent to carry out the acid that thorough washing is removed small portion of residual then;
2) add thermal material, the weight of material proportioning is that raw material/organic acid soln or organic and inorganic mixed acid solution are 5/1-1/5, Heating temperature is 50-150 ℃, soaking time is 10-180min, utilize the effect between organic acid molecule and higher plant, the edible and medicinal fungi cell walls organic polymer material, active polysaccharide is separated from raw material, and cut off the glycosidic link of macromolecule polysaccharide, realize its part degraded;
3) organic solvent washing is removed remaining acid solution, finishes the organic acid of raw material and handles;
4) through organic acid-treated raw material, add 5-15 times of volume water and extract, extracting solution concentrates the back alcohol precipitation, separates settling and can obtain active Crude polysaccharides;
5) active Crude polysaccharides is dissolved in the 5-15 times of volumes of deionized water, and the pH of regulator solution is extremely neutral, centrifugal treating, and supernatant liquor concentrates behind dialysis or membrane sepn, and drying obtains active polysaccharide.
2. by the extracting method of active polysaccharide in described higher plant of claim 1 or the edible and medicinal fungi class, it is characterized in that described organic solvent is selected from alcohol or the acetone of C1-C3.
3. press the extracting method of active polysaccharide in described higher plant of claim 1 or the edible and medicinal fungi class, it is characterized in that: described pretreatment process is with raw material drying, removal of impurities, mechanical disintegration, adopt alcohol or the ethyl acetate of sherwood oil, C1-C3 to carry out extracting, obtain wherein volatile oil, flavonoid, triterpenes, saponins fat-soluble active substance, the extracting residue is after drying as going on foot raw material down.
4. press the extracting method of active polysaccharide in described higher plant of claim 1 or the edible and medicinal fungi class, it is characterized in that: described pretreatment process for raw material drying, removal of impurities, mechanical disintegration as step raw material down, fat-soluble active substance can be in step 3) obtains during organic solvent washing at this moment.
5. by the extracting method of active polysaccharide in described higher plant of claim 1 or the edible and medicinal fungi class, it is characterized in that: described higher plant is selected the Radix Astragali for use, matrimony vine, Ginkgo Leaf, pawpaw, Japanese Honeysuckle, Radix Angelicae Sinensis, dried orange peel, ephedra sinica, rhizome of chuanxiong, Rhizome of Grass leaf Sweelflag, garlic, Sharpleaf Galangal Fruit, the root of Dahurain angelica, tarragon, the root of Chinese wild ginger, Herba Cistanches, arrow-leaved oleaster, folium eucalypti, Herba Houttuyniae, Glossy Privet Fruit, notopterygium root, genseng, pseudo-ginseng, Herba Pileae Scriptae, Semen Plantaginis, Princes-feather Fruit, lilac daphne, Buddha's hand, White Mulberry Root-bark, loranthus parasiticus, the root of large-flowered skullcap, Herba Epimedii, tealeaves, Root of Kirilow Rhodiola, aloe, oat, konjaku, Chinese yam, rhizoma Gastrodiae, radix bupleuri, the flower of Radix Et Caulis Acanthopanacis Senticosi, leaf, seed, skin, fruit, root, the stem class is as raw material; Described edible and medicinal fungi selects for use the fungus sporophore of glossy ganoderma, auricularia auriculajudae, mushroom, umbellate pore furgus, white fungus, Grifola frondosa, Poria cocos, rainbow conk, Hericium erinaceus (Bull. Ex Fr.) Pers., Cordyceps sinensis or mycelium as raw material.
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