CN110859870A - Fig particle and preparation method thereof - Google Patents

Fig particle and preparation method thereof Download PDF

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CN110859870A
CN110859870A CN201911139994.4A CN201911139994A CN110859870A CN 110859870 A CN110859870 A CN 110859870A CN 201911139994 A CN201911139994 A CN 201911139994A CN 110859870 A CN110859870 A CN 110859870A
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freeze
dried powder
particles
granules
powder
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柯学
郭青龙
郑保安
李其彬
王省业
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Qingdao Haidekun Biotechnology Co Ltd
China Pharmaceutical University
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Qingdao Haidekun Biotechnology Co Ltd
China Pharmaceutical University
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/60Moraceae (Mulberry family), e.g. breadfruit or fig
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/385Concentrates of non-alcoholic beverages
    • A23L2/39Dry compositions
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/14Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1605Excipients; Inactive ingredients
    • A61K9/1629Organic macromolecular compounds
    • A61K9/1635Organic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polyvinyl pyrrolidone, poly(meth)acrylates
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/14Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1605Excipients; Inactive ingredients
    • A61K9/1629Organic macromolecular compounds
    • A61K9/1652Polysaccharides, e.g. alginate, cellulose derivatives; Cyclodextrin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P1/00Drugs for disorders of the alimentary tract or the digestive system
    • A61P1/14Prodigestives, e.g. acids, enzymes, appetite stimulants, antidyspeptics, tonics, antiflatulents
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

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  • Animal Behavior & Ethology (AREA)
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  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • General Chemical & Material Sciences (AREA)
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  • Food Science & Technology (AREA)
  • Alternative & Traditional Medicine (AREA)
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  • Medicinal Preparation (AREA)

Abstract

The invention discloses fig granules and a preparation method thereof. The fig particles are composed of fig freeze-dried powder and modified auxiliary materials; the modified auxiliary materials are selected from one or more of dry adhesive, suspending agent, flavoring agent and lubricating agent; the fig particles are prepared by the following method: adding modified auxiliary materials into the fig freeze-dried powder according to a certain proportion, mixing by using a mixer, adding a lubricant, continuously mixing, granulating, screening, collecting particles with the particle size of 40-80 meshes, collecting fine powder, and re-granulating to obtain the fig particles. The invention solves the contradiction among the dispersibility, the settling property and the fluidity brought by improving the moisture absorption of the fig solid particles in the prior art through the improvement of the formula and the preparation process, the moisture absorption is reduced from 22 percent moisture absorption weight gain to 11 percent, and the fluidity is as follows: from a general (38 ° angle of repose) to good (32 °).

Description

Fig particle and preparation method thereof
Technical Field
The invention belongs to the field of pharmaceutical preparations, and relates to fig granules and a preparation method thereof.
Background
Fig (Ficus carica Linn.) is a flowering plant belonging to the genus Ficus of the family moriaceae, mainly growing in some tropical and temperate areas, and belonging to the subtropical deciduous small trees. At present, eight hundred varieties of figs are known, most of the figs are evergreen, and the fig is a fallen leaf variety only in places with the length longer than temperate regions. The fruit is bulbous, the tail has a small hole, and pollen is spread by wasp.
The edible probability of the fig is very high, the edible place of the fresh fig is as high as 97%, the edible part of the fig made into dry fruits and preserved fruits can be as high as 100%, the acid content is very low, no hard fruits exist, and the fig is suitable for being eaten by old people and children. The fig contains rich amino acid, the fresh fruit accounts for 1.0 percent, and the dry fruit accounts for 5.3 percent; at present, 18 species have been found. Not only has higher utilization value due to the fact that 8 kinds of amino acid necessary for human bodies are available, but also has the highest content of aspartic acid (1.9 percent of dry weight) and has good effects of resisting leukemia, recovering physical strength and eliminating fatigue. Therefore, the fig drink is taken as a 'carborphine substitute' abroad. The dry matter content of the fig is high, the fresh fruit is 14-20%, and the dry fruit is more than 70%. Among them, glucose content, fructose content and sucrose content, which can be directly absorbed and utilized by human body, are 34.3% (dry weight), 31.2% (dry weight) and only 7.82% (dry weight). The caloric value is low and is called a low-calorie food in japan. The domestic medical research proves that the health food is a weight-losing health food. Fig contains polysaccharides, accounting for 6.49% (dry weight), mainly arabinose and galactose, and has a certain effect on resisting aging. The fig contains various vitamins, especially contains more carotene, the fresh fruit is 30mg/100g, the dry fruit is 70mg/100g, and the fresh fruit is above peach, grape, plum, pear, orange and sweet persimmon. Besides fresh food and medicine, the fig can also be processed into dried fruit, preserved fruit, jam, fruit juice, fruit tea, fruit wine, beverage, can, etc. However, there are few reports on the absence of pollen. CN 109527468A discloses a fig powder and its preparation method, the preparation process of the fig powder comprises the steps of material selection, three-stage countercurrent cleaning, cutting, heat pump drying, primary grinding, fine grinding, packaging and the like. However, the method has complex preparation process, puts high requirements on equipment, has high production cost, and is not suitable for popularization in industrial mass production. Some reports have been made on the production of fig powder by extracting fig juice after cooking and then spray-drying, but this method also results in loss of some of the nutrients due to high-temperature cooking. At present, no related report of solid beverage taking fig powder as main ingredient is found.
The traditional fig powder is difficult to store due to extremely easy hygroscopicity, and although the hygroscopicity can be improved to a certain extent by increasing the particle size of the fig powder, the suspension speed in water is slow, the sedimentation is fast, and the taste and the appearance of the fig powder are poor; although the reduction of the particle size can slow down the sedimentation rate and accelerate the suspension molding, the dispersion in water is poor and the wetting is difficult, and the powder flowability is poor, and the difference of the loading in industrial production is large, which is unfavorable for mass production.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the fig granules which have the advantages of good dispersibility in water, high suspension speed, low sedimentation speed, good fluidity and low hygroscopicity, and are suitable for industrial production.
The invention also aims to provide a preparation method of the fig granules.
The purpose of the invention can be realized by the following technical scheme:
a fig granule is prepared from fructus fici lyophilized powder and modified adjuvant; the modified auxiliary materials are selected from one or more of dry adhesive, suspending agent, flavoring agent and lubricating agent; the fig particles are prepared by the following method: adding modified auxiliary materials into the fig freeze-dried powder according to a certain proportion, mixing by using a mixer, adding a lubricant, continuously mixing, granulating, screening, collecting particles with the particle size of 40-80 meshes, collecting fine powder, and re-granulating to obtain the fig particles; the dry adhesive is selected from one or more of microcrystalline cellulose, starch, spray-dried lactose, polyvidone K30 and hypromellose; the suspending agent is selected from one or more of acacia, tragacanth, peach gum, sodium alginate, agar, starch slurry, methylcellulose, sodium carboxymethylcellulose, hydroxypropyl cellulose, carbopol, polyvidone, dextran, dextrin, and poloxamer; the flavoring agent is one or more selected from sucrose, synthetic essence, oleum Menthae Dementholatum, mucilage, effervescent, and mannitol; the lubricant is selected from one or more of magnesium stearate, colloidal silicon dioxide, talcum powder, hydrogenated vegetable oil and polyethylene glycol.
The fig freeze-dried powder is preferably prepared by freeze-drying fig, crushing and sieving through a 80-mesh sieve.
The suspending agent is preferably dextrin, and the dosage of the suspending agent is 1-10% by total mass of the raw materials, and is further preferably 5%.
The flavoring agent is preferably mannitol, and the dosage of the flavoring agent is 5-30% by total mass of the raw materials, and is more preferably 15%.
The lubricant is preferably magnesium stearate, and the dosage of the magnesium stearate is 0.5-3% by mass of the total mass of the raw materials, and the dosage of the magnesium stearate is more preferably 1%.
The fig granules further comprise one or two of fig freeze-dried powder, magnesium stearate, mannitol and dextrin; still further preferably, the fig freeze-dried powder consists of fig freeze-dried powder, magnesium stearate and mannitol, wherein the fig freeze-dried powder: the mass ratio of mannitol is 4: 1; or even more preferably comprises fig freeze-dried powder, magnesium stearate and dextrin, wherein the fig freeze-dried powder: the mass ratio of dextrin is 4: 1; or even more preferably comprises fig freeze-dried powder, magnesium stearate, dextrin and mannitol, wherein the fig freeze-dried powder: mannitol: the mass ratio of dextrin is 8:1: 1.
The preparation method of the fig granules comprises the steps of mixing the fig freeze-dried powder and other modified auxiliary materials except the lubricant in proportion, adding the lubricant, continuously mixing, granulating by using a dry method granulator, and collecting granules of 40-80 meshes to obtain the fig granules.
And preferably, mixing the fig freeze-dried powder and other modified auxiliary materials except the lubricant by adopting a rotary mixer under the conditions of 20-25 rpm and 3-5 min, adding magnesium stearate serving as the lubricant, and continuously mixing for 3-5 min.
The preferable feeding speed of the dry granulating machine is 10-30RPM, the pressure of the extrusion roller is 4-14KN/cm, and the rotating speed of the extrusion roller is 5-30 RPM.
The feed rate for dry granulation is further preferably 20RPM, the pressure of the squeeze rolls is further preferably 10KN/cm, and the rotational speed of the pressure wheels is further preferably 25 RPM.
The environmental humidity is controlled within RH 50% during the granulation process.
Has the advantages that:
the invention solves the contradiction among the dispersibility, the settling property and the fluidity brought by improving the moisture absorption of the fig solid particles in the prior art through the improvement of the formula and the preparation process, the moisture absorption is reduced from 22 percent moisture absorption weight gain to 11 percent, and the fluidity is as follows: increasing from normal (38 ° angle of repose) to good (32 °), the settling time increased from 10min to 2 h.
The invention provides a novel fig solid beverage, which retains the nutrient components to the maximum extent, has simple preparation process and low requirement on equipment and is suitable for industrial production. The fig solid beverage can improve the compliance of clinical patients, particularly inappetence and elderly patients, is convenient to store and transport, and is convenient to take with water quantitatively.
Drawings
FIG. 1 measurement principle of natural angle of repose injection method
Detailed Description
Example 1:
crushing the fig freeze-dried tablets by a crusher, screening particles with certain granularity by a stainless steel screen (80 meshes), and preparing the fig freeze-dried powder according to the following steps: adding auxiliary materials according to the ratio of mannitol to 4:1, mixing by using a mixer (20rpm, 3min), adding 1% of magnesium stearate as a lubricant, continuously mixing for 3min, granulating by using a dry granulating machine (the feeding speed is 20rpm, the pressure of an extrusion roller is 10KN/cm, the speed of a pressing wheel is 25rpm, the mesh size is 40 meshes), and collecting particles of 40-80 meshes to obtain fig particles; collecting fine powder, and granulating again. And controlling the ambient humidity within 50% in the granulating process.
Example 2
Crushing fig freeze-dried tablets by a crusher, screening particles with certain granularity by a stainless steel screen (50 meshes), and according to fig freeze-dried powder: adding auxiliary materials into dextrin at a ratio of 4:1, mixing by using a mixer (20rpm for 3min), adding 0.5% of magnesium stearate as a lubricant in mass fraction, adding 0.2% of strawberry essence as a flavoring agent, continuously mixing for 3min, granulating by using a dry granulating machine (feeding speed is 20rpm, extrusion roller pressure is 10KN/cm, pressing wheel speed is 25rpm, and the mesh number of whole granules is 40), and collecting granules of 40-60 meshes to obtain fig granules; collecting fine powder, and granulating again. And controlling the ambient humidity within 50% in the granulating process.
And controlling the ambient humidity within 50% in the granulating process.
Example 3
Crushing fig freeze-dried tablets by a crusher, screening particles with certain granularity by a stainless steel screen (50 meshes), and according to fig freeze-dried powder: mannitol: adding auxiliary materials into dextrin at a ratio of 8:1:1, mixing by using a mixer (20rpm, 3min), adding 1% of magnesium stearate as a lubricant, 5% of sucrose and 0.01% of vanillin as a flavoring agent, continuously mixing for 3min, granulating by using a dry granulating machine (the feeding speed is 20rpm, the extrusion roller pressure is 10KN/cm, the pressing wheel speed is 25rpm, and the mesh number of the whole granules is 40 meshes), and collecting the granules of 40-60 meshes to obtain fig granules; collecting fine powder, and granulating again. And controlling the ambient humidity within 50% in the granulating process.
And controlling the ambient humidity within 50% in the granulating process.
Effects of the embodiment
The index-related index was measured in the following manner, and the results are shown in Table 1.
1. Fluidity, using angle of repose as an index
The angle of repose was determined by the injection method, the cone diameter d (mm) was determined, the funnel height h (mm) and the cone radius r (mm) (r ═ d/2) were used as tangent tan θ, the angle of repose θ was calculated, and the average was repeated 3 times.
The principle of the injection method is shown in fig. 1, and the height of the cone piled up by the wheat seeds for experiments is measured by using a fixed horizontal bottom surface diameter and can be obtained according to the formula (1).
Figure BDA0002280657390000041
Wherein θ is an angle of repose; h is the height of the species cone, and R is the radius of the horizontal bottom surface of the species cone.
2. Hygroscopicity, weight gain due to moisture absorption as an indicator
The test article is placed in a suitable open container (such as a weighing bottle or a petri dish), spread into a thick thin layer, placed under the condition of relative humidity of 75% for 24 hours, and accurately weighed before and after the test to examine the moisture absorption deliquescence of the test article. Rating according to the following criteria
Has the characteristics of moisture absorption: the moisture-drawing weight gain is not less than 15%.
Moisture absorption: the moisture-inducing weight gain is less than 15% but not less than 2%.
Slightly hygroscopic: the moisture-inducing weight gain is less than 2% but not less than 0.2%.
No or almost no hygroscopicity: the moisture-drawing weight gain is less than 0.2 percent.
3. Water dispersability solids (m) are dispersed in a volume (v) of a dispersion medium, which may be water at different temperatures, with a certain mass. The level of agglomeration of the material to be dispersed during the dispersion was examined for ease of dispersion.
4. The settling time is such that a certain mass of solids (m) is dispersed in a certain volume (v) of dispersion medium, i.e. the settling volume ratio should be uniform. The time (t) from uniform dispersion to the time at which significant solid-liquid demixing occurred was recorded.
The starting height H of the suspension is noted. Standing until the solid-liquid interface is not changed any more, recording the final high-degree of the suspension, and calculating according to the following formula:
volume ratio of sedimentation H/H
TABLE 1
Figure BDA0002280657390000051
Remarking: settling time was tested under conditions in which 10g of the solid was dispersed in 100mL of water

Claims (10)

1. The fig granules are characterized by consisting of fig freeze-dried powder and modified auxiliary materials; the modified auxiliary materials are selected from one or more of dry adhesive, suspending agent, flavoring agent and lubricating agent; the fig particles are prepared by the following method: adding modified auxiliary materials into the fig freeze-dried powder according to a certain proportion, mixing by using a mixer, adding a lubricant, continuously mixing, granulating, collecting particles with the particle size of 40-80 meshes, re-granulating if redundant fine powder exists, obtaining particles with the particle size of 40-80 meshes again, and mixing all the particles with the particle size of 40-80 meshes to obtain the fig particles; the dry adhesive is selected from one or more of microcrystalline cellulose, starch, spray-dried lactose, polyvidone K30 and hypromellose; the suspending agent is selected from one or more of acacia, tragacanth, peach gum, sodium alginate, agar, starch slurry, methylcellulose, sodium carboxymethylcellulose, hydroxypropyl cellulose, carbopol, polyvidone, dextran, dextrin, and poloxamer; the flavoring agent is one or more selected from sucrose, synthetic essence, oleum Menthae Dementholatum, mucilage, effervescent, and mannitol; the lubricant is selected from one or more of magnesium stearate, colloidal silicon dioxide, talcum powder, hydrogenated vegetable oil and polyethylene glycol.
2. The fig granule as claimed in claim 1, wherein the fig lyophilized powder is prepared by lyophilizing whole fig, pulverizing, and sieving with 80 mesh sieve.
3. Fig granules according to claim 1, wherein the suspending agent is dextrin, in an amount of 1-10%, preferably 5%.
4. Fig granules according to claim 1, characterized in that said flavoring agent is mannitol in an amount of 5-30%, preferably 15%.
5. Fig granules according to claim 1, wherein the lubricant is magnesium stearate in an amount of 0.5-3%, preferably 1%.
6. The fig granules according to any one of claims 1-5, wherein the fig granules are composed of one or two of fig lyophilized powder, magnesium stearate, mannitol and dextrin; the fig freeze-dried powder is preferably composed of fig freeze-dried powder, magnesium stearate and mannitol, wherein the fig freeze-dried powder: the mass ratio of mannitol is 4: 1; or preferably consists of fig freeze-dried powder, magnesium stearate and dextrin, wherein the fig freeze-dried powder comprises the following components in percentage by weight: the mass ratio of dextrin is 4: 1; or preferably comprises fig freeze-dried powder, magnesium stearate, dextrin and mannitol, wherein the fig freeze-dried powder: mannitol: the mass ratio of dextrin is 8:1: 1.
7. The method for preparing fig granules according to any one of claims 1 to 5, wherein the fig granules are obtained by mixing freeze-dried fig powder with other modified auxiliary materials except lubricant in proportion, adding the lubricant, continuing mixing, granulating by a dry granulation machine, and collecting granules of 40-80 meshes.
8. The preparation method according to claim 7, wherein the fig freeze-dried powder and other modified auxiliary materials except the lubricant are mixed by a mixer under the conditions of 20-25 rpm and 3-5 min, magnesium stearate is added as the lubricant, and the mixture is continuously mixed for 3-5 min.
9. The process according to claim 7, wherein the dry granulator is fed at a feed rate of 10-30RPM, the compression roller is pressed at a pressure of 4-14KN/cm, and the compression roller is rotated at a speed of 5-30 RPM.
10. The process according to claim 7, wherein the dry granulation is carried out at a feed rate of 20RPM, a compression roller pressure of 10KN/cm and a compression roller speed of 25 RPM.
CN201911139994.4A 2019-11-20 2019-11-20 Fig particle and preparation method thereof Pending CN110859870A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20110089893A (en) * 2010-02-02 2011-08-10 주식회사 머슈빌 Composition for preventing or treating atopic dermatitis and allergy-related diseases comprising fermented phellinus linteus extract
CN107772330A (en) * 2016-08-29 2018-03-09 朱玉龙 A kind of compound fig freeze-dried powder lozenge
CN110024986A (en) * 2019-05-05 2019-07-19 四川农业大学 A kind of fig functionality chewable tablets and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20110089893A (en) * 2010-02-02 2011-08-10 주식회사 머슈빌 Composition for preventing or treating atopic dermatitis and allergy-related diseases comprising fermented phellinus linteus extract
CN107772330A (en) * 2016-08-29 2018-03-09 朱玉龙 A kind of compound fig freeze-dried powder lozenge
CN110024986A (en) * 2019-05-05 2019-07-19 四川农业大学 A kind of fig functionality chewable tablets and preparation method thereof

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Application publication date: 20200306