CN108324742B - Sparassis crispa medicinal granules and preparation method thereof - Google Patents
Sparassis crispa medicinal granules and preparation method thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/06—Fungi, e.g. yeasts
- A61K36/07—Basidiomycota, e.g. Cryptococcus
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/385—Concentrates of non-alcoholic beverages
- A23L2/39—Dry compositions
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L31/00—Edible extracts or preparations of fungi; Preparation or treatment thereof
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/70—Carbohydrates; Sugars; Derivatives thereof
- A61K31/715—Polysaccharides, i.e. having more than five saccharide radicals attached to each other by glycosidic linkages; Derivatives thereof, e.g. ethers, esters
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
- A61K47/38—Cellulose; Derivatives thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/0087—Galenical forms not covered by A61K9/02 - A61K9/7023
- A61K9/0095—Drinks; Beverages; Syrups; Compositions for reconstitution thereof, e.g. powders or tablets to be dispersed in a glass of water; Veterinary drenches
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/141—Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers
- A61K9/146—Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers with organic macromolecular compounds
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/17—Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
Abstract
The invention discloses a sparassis crispa medicinal granules and a preparation method thereof, wherein the sparassis crispa medicinal granules comprise sparassis crispa polysaccharide micro powder and NaHCO3The sparassis crispa polysaccharide micro powder comprises sparassis crispa polysaccharide, polyvinylpyrrolidone and lactose, and NaHCO3The microcapsule comprises NaHCO3And polyethylene glycol wrapped outside; by mass, Sparassis crispa polysaccharide, polyvinylpyrrolidone, lactose, NaHCO3The polyethylene glycol, the dry powder of the hydrangea residue, the soluble starch, the citric acid and the microcrystalline cellulose respectively account for 10-12%, 5-6%, 15-18%, 2.0-2.5%, 5-6%, 40-44%, 10-12% and 0% of the hydrangea electuary.8-1.2% and 4-5%, and has water solubility.
Description
Technical Field
The invention relates to a sparassis crispa electuary and a preparation method thereof.
Background
Fungi belonging to the genus Sparassispfr are rare edible and medicinal fungi (Daiyou and Yanghua 2008; Daiyou 2010), also called as cauliflower mushroom, Sparassia crispa, Sparassidaceae belonging to the fungus kingdom. Sparassis crispa not only has delicious taste, but also has multiple nutrition and health promotion functions. Modern researches prove that the traditional Chinese medicine composition has various efficacies of resisting tumors (Ohnoetal.2000), regulating immunity (Haradaetatal.2002b), promoting wound healing (Kwontetal.2009), promoting hematopoietic function (Haradaetatal.2002a) and the like. As one of the main active ingredients, Sparassis crispa is rich in beta-glucan, and it is reported that the beta-glucan content measured by food analysis assay in Japan reaches 40% or more (Kimura 2013), which is the most important mushroom, so it is called "fantasy mushroom" in Japan.
The edible part of the sparassis crispa is sporocarp, the sparassis crispa contains rich nutrient substances, and the sparassis crispa medicinal granules are not available in the market due to the limitation of solubility.
Disclosure of Invention
The first purpose of the invention is to provide a sparassis crispa medicinal granules which has the advantage of improving water solubility.
The technical purpose of the invention is realized by the following technical scheme:
a Sparassis crispa granule comprises Sparassis crispa polysaccharide micropowder and NaHCO3The sparassis crispa polysaccharide micro powder comprises sparassis crispa polysaccharide, polyvinylpyrrolidone and lactose, and NaHCO3The microcapsule comprises NaHCO3And polyethylene glycol wrapped outside; by mass, Sparassis crispa polysaccharide, polyvinylpyrrolidone, lactose, NaHCO3The polyethylene glycol, the dry powder of the hydrangea residue, the soluble starch, the citric acid and the microcrystalline cellulose respectively account for 10-12%, 5-6%, 15-18%, 2.0-2.5%, 5-6%, 40-44%, 10-12%, 0.8-1.2% and 4-5% of the hydrangea granule.
The water solubility of the sparassis crispa is low, but the water solubility of the sparassis crispa polysaccharide in the sparassis crispa is high, the sparassis crispa is divided into solid residues and sparassis crispa polysaccharide, the separate treatment of different components is facilitated, and the targeted and effective treatment is facilitated; sparassis crispa polysaccharide has good water solubility but poor hygroscopicity, and can be mixed with polyvinylpyrrolidone and lactoseThe preparation method is characterized in that the preparation method comprises the steps of preparing micropowder, wherein the combined action of polyvinylpyrrolidone and lactose is beneficial to the dispersion and powdering process of the Sparassis crispa polysaccharide, and meanwhile, the Sparassis crispa polysaccharide can be wrapped and combined to greatly improve the moisture absorption of the Sparassis crispa polysaccharide; the dry powder of the hydrangea fungi residues is added into the formula, so that on one hand, materials can be fully used, the water-insoluble part is fully utilized again, the utilization rate of the materials is improved, and on the other hand, the dry powder of the hydrangea fungi residues can assist in granulating the polysaccharide micropowder of the hydrangea fungi; in addition, although the water solubility of the dry powder of the hydrangea fungi residues is low, the dry powder is obtained by citric acid and NaHCO3Mixing the microcapsules, when NaHCO is used3After the microcapsule is mixed with water, the polyethylene glycol on the surface of the microcapsule is dissolved to release NaHCO3，NaHCO3The reaction with citric acid is beneficial to the rolling and dissolution of the dry powder of the hydrangea fungi residues in water when bubbles are generated, and provides a pH system which is beneficial to the dissolution of the dry powder of the hydrangea fungi residues for a water system; the soluble starch and the microcrystalline cellulose can play a role in assisting granulation, and can balance the water solubility and the moisture absorption of the sparassis crispa granules.
More preferably: the polyvinylpyrrolidone is K15 or K30, and the average molecular weight of the polyethylene glycol is 1500-1800.
More preferably: the sparassis crispa medicinal granules further comprise a flavoring agent, wherein the flavoring agent comprises 50-55 wt% of sorbitol powder and 45-50 wt% of maltitol powder, and the influence of the flavoring agent on the moisture absorption is reduced.
More preferably: by mass, Sparassis crispa polysaccharide, polyvinylpyrrolidone, lactose, NaHCO3The polyethylene glycol, the dry powder of the hydrangea fungi residues, the soluble starch, the citric acid and the microcrystalline cellulose respectively account for 11 percent, 5.7 percent, 16 percent, 2.3 percent, 5.5 percent, 43 percent, 11 percent, 1.0 percent and 4.5 percent of the hydrangea granule.
The second purpose of the invention is to provide a preparation method of the Sparassis crispa medicinal granules.
The technical purpose of the invention is realized by the following technical scheme:
a preparation method of sparassis crispa granules comprises the following steps:
(1) preparation of sparassis crispa polysaccharide and sparassis crispa residue dry powder
Taking a fresh sparassis crispa sporocarp, blowing and drying for 4-5 hours at the temperature of 30-32 ℃, and then drying for 24-26 hours in a vacuum freeze dryer with the cold trap temperature of-60 to-55 ℃ to obtain a dried sparassis crispa sporocarp;
crushing the dried sparassis crispa sporocarp, and sieving the crushed sparassis crispa sporocarp with a 60-100-mesh sieve; putting the crushed dry sparassis crispa sporocarp into a reaction container, adding water, carrying out ultrasonic treatment for 21-24 min at 40-45 ℃ according to the ultrasonic frequency of 80000-100000 Hz, and carrying out ultrasonic treatment for 30-32 min at 54-58 ℃ according to the ultrasonic frequency of 120000-150000 Hz to obtain an extracting solution, wherein the mass ratio of the dry sparassis crispa sporocarp to the water is 1: 5-7;
centrifuging the extract to obtain solid residue and supernatant; drying the solid residues at 40-45 ℃ by air blast until the weight is constant to obtain dry powder of hydrangea fungi residues; the supernatant is concentrated to 1/3-1/2 of the original volume by nitrogen blowing, 1.5-2.0 times of ethanol is added into the concentrated supernatant, precipitate is separated out under stirring at 4-8 ℃, 5.0-6.0 times of ethanol is added after stirring for 1-2 hours, the precipitate is filtered after stirring for 12-14 hours, and the precipitate is dried by air blowing at 30-35 ℃ to obtain the Sparassis crispa polysaccharide;
(2) preparation of sparassis crispa polysaccharide micropowder
Respectively crushing polyvinylpyrrolidone and lactose, sieving with a 60-100-mesh sieve, adding the Sparassis crispa polysaccharide prepared in the step (1), mixing according to the formula amount, uniformly mixing, crushing, and sieving with a 150-200-mesh sieve to obtain Sparassis crispa polysaccharide micropowder;
（3）NaHCO3preparation of microcapsules
Preparing acetone solution of polyethylene glycol, spraying on NaHCO3Externally, blowing and drying at the temperature of 60-70 ℃ to obtain NaHCO3Micro-capsules;
(4) preparation of Sparassis crispa medicinal granules
The sparassis crispa polysaccharide micro powder prepared in the step (2) and NaHCO prepared in the step (3)3And (2) uniformly mixing the microcapsules, the dry powder of the Sparassis crispa dregs prepared in the step (1), soluble starch, citric acid and microcrystalline cellulose according to the formula amount to obtain the Sparassis crispa medicinal granules.
In conclusion, the invention has the following beneficial effects:
the water solubility of the sparassis crispa is improved to 25-50 mg/ml from indissolvable, so that the water solubility of the product is greatly improved, and the product absorption is facilitated;
the hydroscopic property of the sparassis crispa is improved, the sparassis crispa medicinal granules are low in hydroscopic rate and stable in product, and the hydroscopic rate can be kept even after the sparassis crispa is placed at a high temperature;
compare sparassis crispa dry goods, the absorptivity of sparassis crispa dissolved medicine of this application is better, performance effect that can be better, and it deposits the convenience simultaneously, and the security is high.
Detailed Description
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the present invention.
Examples 1 to 3: a sparassis crispa electuary is prepared by the following method:
(1) preparation of sparassis crispa polysaccharide and sparassis crispa residue dry powder
Taking fresh Sparassis crispa fruiting body, air-drying at 30 deg.C for 5hr, and drying in vacuum freeze-drying machine at-60 deg.C for 26hr to obtain Sparassis crispa fruiting body dry product;
pulverizing dried Sparassis crispa fruiting body, and sieving with 60 mesh sieve; putting the crushed dry sparassis crispa sporocarp into a reaction container, adding water, performing ultrasonic treatment at 40 ℃ for 24min according to the ultrasonic frequency of 10000Hz, and performing ultrasonic treatment at 54 ℃ for 32min according to the ultrasonic frequency of 150000Hz to obtain an extracting solution, wherein the mass ratio of the dry sparassis crispa sporocarp to the water is 1: 5;
centrifuging the extract to obtain solid residue and supernatant; drying the solid residue at 40 deg.C by air blast to constant weight to obtain dry powder of hydrangea fungi residue; concentrating the supernatant with nitrogen until the volume of the supernatant is 1/3, adding 1.5 times of ethanol into the concentrated supernatant, stirring at 4 deg.C to precipitate, stirring for 2hr, adding 5.0 times of ethanol, stirring for 14hr, filtering to obtain precipitate, and air drying at 30 deg.C to obtain Sparassis crispa polysaccharide;
(2) preparation of sparassis crispa polysaccharide micropowder
Respectively crushing polyvinylpyrrolidone and lactose, sieving with a 60-mesh sieve, adding the sparassis crispa polysaccharide prepared in the step (1), mixing according to the formula amount, uniformly mixing, crushing, and sieving with a 150-mesh sieve to obtain sparassis crispa polysaccharide micropowder;
（3）NaHCO3preparation of microcapsules
Preparing acetone solution of polyethylene glycol, spraying on NaHCO3Further, forced air drying at 60 ℃ to obtain NaHCO3Micro-capsules;
(4) preparation of Sparassis crispa medicinal granules
The sparassis crispa polysaccharide micro powder prepared in the step (2) and NaHCO prepared in the step (3)3Uniformly mixing the microcapsules, the dry powder of the Sparassis crispa dregs prepared in the step (1), soluble starch, citric acid and microcrystalline cellulose according to the formula amount to obtain Sparassis crispa granules;
the formulations of examples 1-3 are shown in Table 1.
TABLE 1 formulations of examples 1-3 (unit: parts by mass)
Example 4: a sparassis crispa electuary is prepared by the following method:
(1) preparation of sparassis crispa polysaccharide and sparassis crispa residue dry powder
Taking fresh Sparassis crispa fruiting body, air-drying at 32 deg.C for 4hr, and drying in vacuum freeze-drying machine with cold trap temperature of-55 deg.C for 24hr to obtain Sparassis crispa fruiting body dry product;
pulverizing dried Sparassis crispa fruiting body, and sieving with 100 mesh sieve; putting the crushed dry sparassis crispa sporocarp into a reaction container, adding water, carrying out ultrasonic treatment for 21min at 45 ℃ according to the ultrasonic frequency of 80000Hz, and then carrying out ultrasonic treatment for 30min at 58 ℃ according to the ultrasonic frequency of 120000Hz to obtain an extracting solution, wherein the mass ratio of the dry sparassis crispa sporocarp to the water is 1: 7;
centrifuging the extract to obtain solid residue and supernatant; drying the solid residue at 45 deg.C by air blast to constant weight to obtain dry powder of hydrangea fungi residue; concentrating the supernatant with nitrogen until the volume of the supernatant is 1/2, adding 2.0 times of ethanol into the concentrated supernatant, stirring at 8 deg.C to precipitate, stirring for 1hr, adding 6.0 times of ethanol, stirring for 12hr, filtering to obtain precipitate, and air drying at 35 deg.C to obtain Sparassis crispa polysaccharide;
(2) preparation of sparassis crispa polysaccharide micropowder
Respectively crushing polyvinylpyrrolidone and lactose, sieving with a 100-mesh sieve, adding the Sparassis crispa polysaccharide prepared in the step (1), mixing according to the formula amount, uniformly mixing, crushing, and sieving with a 200-mesh sieve to obtain Sparassis crispa polysaccharide micropowder;
（3）NaHCO3preparation of microcapsules
Preparing acetone solution of polyethylene glycol, spraying on NaHCO3Further, forced air drying at 70 ℃ to obtain NaHCO3Micro-capsules;
(4) preparation of Sparassis crispa medicinal granules
The sparassis crispa polysaccharide micro powder prepared in the step (2) and NaHCO prepared in the step (3)3Uniformly mixing the microcapsules, the dry powder of the Sparassis crispa dregs prepared in the step (1), soluble starch, citric acid and microcrystalline cellulose according to the formula amount to obtain Sparassis crispa granules;
wherein Sparassis crispa polysaccharide, polyvinylpyrrolidone, lactose, NaHCO3The amounts of polyethylene glycol, dry powder of hydrangea residue, soluble starch, citric acid and microcrystalline cellulose were the same as in example 1.
Example 5: a Sparassis crispa granule is prepared by adding 2g correctant into 100g Sparassis crispa granule prepared in example 1, wherein the correctant comprises 50wt% sorbitol powder and 50wt% maltitol powder.
Example 6: a Sparassis crispa granule is prepared by adding 5g correctant into 100g Sparassis crispa granule prepared in example 1, wherein the correctant comprises 55wt% sorbitol powder and 45wt% maltitol powder.
Example 7: a Sparassis crispa granule is prepared by adding 2g correctant (sucrose) into 100g Sparassis crispa granule prepared in example 1.
Example 8: a Sparassis crispa granule is prepared by adding 2g correctant into 100g Sparassis crispa granule prepared in example 1, wherein the correctant is sorbitol powder.
Example 9: a Sparassis crispa granule is prepared by adding 2g correctant into 100g Sparassis crispa granule prepared in example 1, wherein the correctant is maltitol powder.
Example 10: a sparassis crispa granule differing from example 1 in that K30 is selected as polyvinylpyrrolidone and the polyethylene glycol has an average molecular weight of 1800.
Example 11: a sparassis crispa granule differing from example 1 in that K80 is selected as polyvinylpyrrolidone and the polyethylene glycol has an average molecular weight of 5000.
Solubility test
1. Preparation of control
Control 1: the dried sparassis crispa sporocarp sold in the market is crushed and sieved by a 100-mesh sieve.
Control 2: referring to the preparation of CN102919832A, the preparation method specifically comprises the steps of weighing 1g of pine needles, cleaning, adding 100ml of water, soaking for 3 hours, boiling for 20 minutes, filtering, and adding water into the filtrate to 100ml to obtain a pine needle decoction. Adding 1g of soluble starch, 1g of maltose, 0.3g of yeast extract, 0.2g of peptone, 0.2g of monopotassium phosphate, 0.1g of magnesium sulfate and 0.005g of zinc sulfate into 100ml of pine needle decoction, uniformly stirring, sterilizing at 121 ℃ for 30 minutes, cooling to 25 ℃, inoculating Sparassis crispa seeds, culturing at 25 ℃, rotating a shaking table at 150rpm, and culturing for 9 days under the condition of natural illumination. Filtering the fermentation liquor after the culture is finished to obtain the sparassis crispa mycelium, and then drying the sparassis crispa mycelium at the temperature of 55 ℃ until the water content is below 10 percent to obtain the sparassis crispa dry mycelium. Pulverizing dried Sparassis crispa mycelium, and sieving with 100 mesh sieve.
2. Content of test
The solubility test was carried out using the Sparassis crispa granules of examples 1 to 4 as test samples and using control 1 and control 2 as reference samples. Respectively crushing the test sample and the reference sample, sieving by a 100-mesh sieve, taking 20mg of the sample in a reaction bottle, adding a magnetic stirrer, putting the reaction bottle in a 37-DEG C constant-temperature water bath kettle, and gradually adding 37-DEG C pure water into the reaction bottle until the sample in the reaction bottle is just completely dissolved or added to 200ml (200 mu l is dropwise added for the first time, and then the addition amount of each time is the sum of the previous dropwise addition amounts). Each sample was run in 5 replicates and the average was taken.
3. The test results are shown in table 2. Table 2 shows that the solubility in water is lower for controls 1 and 2, while the water solubility is significantly improved for examples 1-4.
Table 2 solubility test results statistics
4. Further determination of solubility
The solubility of the test samples was tested by placing 100mg of the test samples at 0 ℃/20% RH, 25 ℃/60% RH and 40 ℃/75% RH for 30d, 90d and 360d respectively. Each sample was run in 5 replicates and the average was taken.
The solubility of the samples 1-4 is still kept between 25-50 mg/ml, and the appearance (solid form and color) of the samples 1-4 is not obviously changed.
Moisture absorption test
1. Control 3: sparassis crispa polysaccharide is commercially available.
2. Dynamic method
Dynamic moisture sorption analysis (DVS) data was taken from TA Instruments Q5000 TGA, typically a 5mg sample was laid in a platinum crucible and the weight change of the sample during the change from 20% to 80% to 20% relative humidity (ambient humidity 21% RH, ambient temperature 25 ℃) was recorded with TA software (self-contained) and an isothermal sorption curve was plotted, provided that the conditions were set to increase or decrease at a rate of 10% and held at each point for 180 min.
The change in mass during the moisture absorption process (20% RH → 80% RH) was recorded, and the relative change in mass was taken as the moisture absorption value. Each sample was run in 5 replicates and the average was taken.
3. Static method
The surface moisture in the test sample was measured by TGA at 100mg, 5mg, 25 ℃/60% RH, 25 ℃/75% RH for 90d, and 5mg, again using TGA. Each sample was run in 5 replicates and the average was taken.
Thermogravimetric analysis (TGA) data was taken from TA Instruments Q5000 TGA, typically 5mg samples were laid in a platinum crucible and N was dried at a temperature rise rate of 10 ℃/min at 40ml/min by means of stepwise high resolution detection2The samples were warmed from room temperature to 200 ℃ and the weight change during the sample was recorded using TA software (self contained).
4. The test results are shown in table 3. Table 3 shows that reference substance 3 absorbs moisture significantly and has poor moisture absorption, and examples 1 to 11 of the present application have small moisture absorption and significantly better moisture absorption than reference substance 3, can be placed for a long time, solve the problem of significant moisture absorption of Sparassis crispa polysaccharide, and reduce the potential safety hazard caused by moisture absorption, wherein examples 1, 4, 5, 6, and 10 have almost negligible moisture absorption under the test conditions of the present application, and have a high development value.
TABLE 3 statistics of hygroscopicity test results
5. Further testing of moisture absorption
100mg of the test sample was placed at 50 ℃/20% RH for 90d and then at 25 ℃/75% RH for 90d, respectively, and 5mg of the surface moisture in the test sample was tested by TGA. Each sample was run in 5 replicates and the average was taken.
The moisture absorption rates of examples 1 to 11 and comparative example 3 were: 0.1%, 1.3%, 1.1%, 0.1%, 0.2%, 0.1%, 10.3%, 4.0%, 4.7%, 0.2%, 4.9%, and 23.1%. The moisture absorption rates of examples 1, 4, 5, 6 and 10 are substantially the same as the results obtained without placing the samples at 50 ℃/20% RH for 90 days, and the other samples have certain changes, particularly the change rate of the reference 3 is most obvious, which shows that the retention of the moisture absorption rate of the samples of the application after placing the samples at high temperature is better than that of the sparassis crispa polysaccharide.
Claims (4)
1. A sparassis crispa granule is characterized by comprising sparassis crispa polysaccharide micro powder and NaHCO3Microcapsule, dry powder of hydrangea fungus residue, soluble starch, citric acid and microcrystalCellulose, wherein the sparassis crispa polysaccharide micropowder comprises sparassis crispa polysaccharide, polyvinylpyrrolidone, lactose and NaHCO3The microcapsule comprises NaHCO3And polyethylene glycol wrapped outside; by mass, Sparassis crispa polysaccharide, polyvinylpyrrolidone, lactose, NaHCO3The polyethylene glycol, the dry powder of the hydrangea residue, the soluble starch, the citric acid and the microcrystalline cellulose respectively account for 10-12%, 5-6%, 15-18%, 2.0-2.5%, 5-6%, 40-44%, 10-12%, 0.8-1.2% and 4-5% of the hydrangea granule;
the preparation method of the sparassis crispa electuary comprises the following steps:
(1) preparation of sparassis crispa polysaccharide and sparassis crispa residue dry powder
Taking a fresh sparassis crispa sporocarp, blowing and drying for 4-5 hours at the temperature of 30-32 ℃, and then drying for 24-26 hours in a vacuum freeze dryer with the cold trap temperature of-60-55 ℃ to obtain a dry sparassis crispa sporocarp;
crushing the dried sparassis crispa sporocarp, and sieving the crushed sparassis crispa sporocarp with a 60-100-mesh sieve; putting the crushed dry sparassis crispa sporocarp into a reaction container, adding water, carrying out ultrasonic treatment for 21-24 min at 40-45 ℃ according to the ultrasonic frequency of 80000-100000 Hz, and carrying out ultrasonic treatment for 30-32 min at 54-58 ℃ according to the ultrasonic frequency of 120000-150000 Hz to obtain an extracting solution, wherein the mass ratio of the dry sparassis crispa sporocarp to the water is 1: 5-7;
centrifuging the extract to obtain solid residue and supernatant; drying the solid residues at 40-45 ℃ by air blast until the weight is constant to obtain dry powder of hydrangea fungi residues; the supernatant is concentrated to 1/3-1/2 of the original volume by nitrogen blowing, 1.5-2.0 times of ethanol is added into the concentrated supernatant, precipitate is separated out under stirring at 4-8 ℃, 5.0-6.0 times of ethanol is added after stirring for 1-2 hours, the precipitate is filtered after stirring for 12-14 hours, and the precipitate is dried by air blowing at 30-35 ℃ to obtain the Sparassis crispa polysaccharide;
(2) preparation of sparassis crispa polysaccharide micropowder
Respectively crushing polyvinylpyrrolidone and lactose, sieving with a 60-100-mesh sieve, adding the Sparassis crispa polysaccharide prepared in the step (1), mixing according to the formula amount, uniformly mixing, crushing, and sieving with a 150-200-mesh sieve to obtain Sparassis crispa polysaccharide micropowder;
(3)NaHCO3preparation of microcapsules
Preparing acetone solution of polyethylene glycol, spraying on NaHCO3Externally, blowing and drying at the temperature of 60-70 ℃ to obtain NaHCO3Micro-capsules;
(4) preparation of Sparassis crispa medicinal granules
The sparassis crispa polysaccharide micro powder prepared in the step (2) and NaHCO prepared in the step (3)3And (2) uniformly mixing the microcapsules, the dry powder of the Sparassis crispa dregs prepared in the step (1), soluble starch, citric acid and microcrystalline cellulose according to the formula amount to obtain the Sparassis crispa medicinal granules.
2. The sparassis crispa granules according to claim 1, wherein the polyvinylpyrrolidone is K15 or K30, and the polyethylene glycol has an average molecular weight of 1500-1800.
3. The sparassis crispa granules according to claim 1, further comprising a flavoring agent, wherein the flavoring agent comprises 50-55 wt% of sorbitol powder and 45-50 wt% of maltitol powder.
4. The Sparassis crispa granule according to claim 1, wherein Sparassis crispa polysaccharide, polyvinylpyrrolidone, lactose, NaHCO by mass3The polyethylene glycol, the dry powder of the hydrangea fungi residues, the soluble starch, the citric acid and the microcrystalline cellulose respectively account for 11 percent, 5.7 percent, 16 percent, 2.3 percent, 5.5 percent, 43 percent, 11 percent, 1.0 percent and 4.5 percent of the hydrangea granule.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105343012A (en) * | 2015-11-19 | 2016-02-24 | 泰山医学院 | Eucommia polysaccharide effervescent granule and preparation method thereof |
| CN106562404A (en) * | 2016-10-30 | 2017-04-19 | 福建容益菌业科技研发有限公司 | Sparassis crispa lozenges |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105343012A (en) * | 2015-11-19 | 2016-02-24 | 泰山医学院 | Eucommia polysaccharide effervescent granule and preparation method thereof |
| CN106562404A (en) * | 2016-10-30 | 2017-04-19 | 福建容益菌业科技研发有限公司 | Sparassis crispa lozenges |
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