CN110772573A - Cold granules and preparation method thereof - Google Patents

Cold granules and preparation method thereof Download PDF

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Publication number
CN110772573A
CN110772573A CN201910889808.2A CN201910889808A CN110772573A CN 110772573 A CN110772573 A CN 110772573A CN 201910889808 A CN201910889808 A CN 201910889808A CN 110772573 A CN110772573 A CN 110772573A
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parts
solid residue
filtrate
water
mixing
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戴源发
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Guangdong Kangqili Pharmaceutical Ltd By Share Ltd
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Guangdong Kangqili Pharmaceutical Ltd By Share Ltd
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    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/73Rosaceae (Rose family), e.g. strawberry, chokeberry, blackberry, pear or firethorn
    • A61K36/736Prunus, e.g. plum, cherry, peach, apricot or almond
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/50Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates
    • A61K47/69Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit
    • A61K47/6949Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit inclusion complexes, e.g. clathrates, cavitates or fullerenes
    • A61K47/6951Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit inclusion complexes, e.g. clathrates, cavitates or fullerenes using cyclodextrin
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    • A61K9/00Medicinal preparations characterised by special physical form
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    • A61K9/16Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
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    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331Extraction 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
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    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying

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Abstract

The cold granules are prepared from the following raw material medicines in parts by weight: 25-45 parts of wild chrysanthemum; 20-40 parts of holly; 20-40 parts of houttuynia cordata; 15-25 parts of bitter apricot seeds; 30-60 parts of fructus forsythiae; 60-180 parts of golden pomelo peel; the preparation method comprises the following steps: distilling herba Houttuyniae and golden pomelo peel to obtain volatile oil, filtrate A and solid residue A, concentrating the volatile oil under reduced pressure, vacuum freeze drying, and clathrating with BETA-cyclodextrin to obtain clathrate A; freeze-drying flos Chrysanthemi Indici, flos Ilicis Asprellae and fructus forsythiae under vacuum, and ultrasonically extracting to obtain filtrate B and solid residue B; distilling bitter almond powder to obtain almond water and solid residue C; mixing the solid residue A, B, C, adding the filtrate A and B, decocting in water, and concentrating under reduced pressure to obtain soft extract; mixing the clathrate A with the soft extract, adding dextrin and sucralose, spraying almond water, mixing, and granulating; simple and feasible process, controllable quality, stable curative effect, high content of effective components, high curative effect, homogeneous granularity and high stability.

Description

Cold granules and preparation method thereof
Technical Field
The invention relates to the technical field of pharmaceutical compositions and preparation methods thereof, in particular to cold granules and a preparation method thereof.
Background
The symptoms of cold are generally aching pain all over the body, nasal obstruction, nasal discharge and cough with phlegm. In recent years, although the treatment method for the wind-cold type common cold is improved by a lot of progress, the treatment method still adopts western medicines, the cost is high, side effects are caused, and the health of patients is seriously influenced.
The cold granules taking traditional Chinese medicines as main components take the cold granules prescription recorded in the pharmacopoeia of the people's republic of China 2015 as an example: 100g of radix bupleuri, 75g of lonicera confusa, 100g of radix puerariae, 75g of sweet wormwood, 75g of fructus forsythiae, 75g of radix scutellariae, 50 g of platycodon grandiflorum, 50 g of bitter almond and 0.15g of menthol. The preparation method comprises the following steps: decocting the above nine materials except Mentholum and the other eight materials such as bupleuri radix with water twice each for 4 hr, filtering the decoction, mixing filtrates, concentrating to appropriate amount, adding sucrose and dextrin, granulating, drying, dissolving Mentholum in ethanol, spraying into the granule, and mixing to obtain 1000 g; or spray drying the concentrated solution to obtain fine powder, adding appropriate amount of dextrin and Mentholum (encapsulated with appropriate amount of BETA-cyclodextrin), mixing, and dry granulating to obtain 300g (without sucrose). Therefore, the following steps are carried out:
the prior art is mostly used for researching the components of the Chinese medicinal composition, and the preparation methods of the Chinese medicinal composition in the technical dictionary are mostly prepared by adopting the traditional methods of decoction, impregnation and the like, so that the active ingredients in the medicament can not be effectively extracted, and the curative effect of the medicament is influenced.
Disclosure of Invention
The invention aims to provide cold granules which are simple, convenient and feasible, have controllable quality, stable curative effect, high content of active ingredients of finished products, good drug effect, uniform granules and good stability aiming at the defects of the prior art, and also provides a preparation method thereof.
The aim of the invention is achieved by the following technical measures:
the cold treating granule consists of the following raw material medicines in parts by weight:
25-45 parts of wild chrysanthemum;
20-40 parts of holly;
20-40 parts of houttuynia cordata;
15-25 parts of bitter apricot seeds;
30-60 parts of fructus forsythiae;
60-180 parts of golden pomelo peel.
In one embodiment, the traditional Chinese medicine composition is prepared from the following raw material medicines in parts by weight:
25 parts of wild chrysanthemum;
30 parts of holly;
30 parts of houttuynia cordata;
25 parts of bitter almond;
60 parts of fructus forsythiae;
80 parts of golden pomelo peel.
In one embodiment, the traditional Chinese medicine composition is prepared from the following raw material medicines in parts by weight:
35 parts of wild chrysanthemum;
40 parts of holly;
40 parts of houttuynia cordata;
20 parts of bitter almond;
50 parts of fructus forsythiae;
120 parts of golden pomelo peel.
In one embodiment, the traditional Chinese medicine composition is prepared from the following raw material medicines in parts by weight:
45 parts of wild chrysanthemum;
20 parts of holly;
20 parts of houttuynia cordata;
15 parts of bitter almond;
40 parts of fructus forsythiae;
140 parts of golden pomelo peel.
In one embodiment, the traditional Chinese medicine composition is prepared from the following raw material medicines in parts by weight:
25 parts of wild chrysanthemum;
30 parts of holly;
30 parts of houttuynia cordata;
15 parts of bitter almond;
30 parts of fructus forsythiae;
180 parts of golden pomelo peel.
A preparation method of cold granules comprises the following steps:
s110, pulverizing and mixing houttuynia cordata and golden pomelo peel, sieving, introducing steam for distillation to obtain volatile oil, filtrate A and solid residue A, concentrating the volatile oil under reduced pressure, freeze-drying in vacuum, and clathrating with beta-cyclodextrin to obtain clathrate A;
vacuum freeze drying flos Chrysanthemi Indici, flos Ilicis Asprellae and fructus forsythiae, removing water, pulverizing, sieving, adding ethanol solution, soaking, and ultrasonic extracting to obtain filtrate B and solid residue B;
pulverizing semen Armeniacae amarum, sieving, soaking in ethanol, and distilling with steam to obtain semen Armeniacae amarum water and solid residue C;
s120, mixing the solid residue A, the solid residue B and the solid residue C, adding the filtrate A and the filtrate B, adding water, decocting, filtering, centrifuging and clarifying the filtrate, and concentrating under reduced pressure to obtain thick paste;
s130, mixing the inclusion A obtained in the step S110 with the thick paste obtained in the step S120, adding dextrin and sucralose, spraying the almond juice obtained in the step S110, uniformly mixing, and granulating.
In one embodiment, in step S110, the preparation of the clathrate a specifically includes:
pulverizing herba Houttuyniae and pericarpium Citri Grandis, mixing, sieving, adding 6-8 times of water, soaking at room temperature for 4-5 hr, and distilling under heating for 4-6 hr to obtain volatile oil, filtrate A and solid residue A; concentrating volatile oil under reduced pressure, vacuum freeze drying, and dissolving the dried product in 2-3 times of 75-95% ethanol to obtain solution A; dissolving BETA-cyclodextrin in 4-5 times of 60-75 deg.C water to obtain solution B; mixing solution A and solution B, stirring for 2-4h, and vacuum freeze drying to obtain white powder, i.e. clathrate A.
In one embodiment, in step S110, the preparing of the filtrate B and the solid residue B specifically includes:
slicing and dishing wild chrysanthemum, holly and fructus forsythiae respectively, and freezing at-38 to-35 ℃ for 4 to 5 hours;
keeping the frozen wild chrysanthemum, holly and forsythia slices at the pressure of 70-110 Pa and the temperature of 50-85 ℃ for 15-18 hours for vacuum drying to obtain mixed dry slices, wherein the water content of the mixed dry slices is 3-5%;
adding 5 times of 20-25% ethanol solution into the mixed dry tablet, keeping the temperature at 35-40 deg.C, introducing reverse current and forward current alternately for three times respectively, and performing ultrasonic extraction for 5-10min to obtain filtrate B and solid residue B.
In one embodiment, in step S110, the preparation of the almond water specifically includes:
pulverizing semen Armeniacae amarum, sieving, soaking in 1-2 times volume of 50-60% ethanol for 30-45min, adding 5-7 times volume of water solution, and heating and distilling to obtain semen Armeniacae amarum water and solid residue C.
In one embodiment, the step S120 specifically includes:
mixing the solid residue A, the solid residue B and the solid residue C, adding the filtrate A and the filtrate B, adding water to 4-6 times of volume, decocting for 2-3 times, each time for 1-2h, filtering, concentrating the filtrate with a vacuum concentration tank to obtain a concentrated solution with a relative density of 1.03, and centrifuging at a super high speed of 15000 r/min until the concentrated solution is clear; concentrating the separated liquid to obtain soft extract with relative density of 1.20-1.30.
The common cold granules and the preparation method thereof utilize the golden pomelo which is produced in Guangdong Meizhou province and the like mostly, the pomelo peel has the effects of reducing phlegm and relieving cough and regulating qi to alleviate pain due to pungent, bitter and warm natures, and the traditional Chinese medicine theory is used as guidance, and distillation extraction and vacuum drying processes are carried out on the natures and the tastes of the raw material medicines; effectively extracts the active ingredients in the medicine and improves the curative effect of the medicine. Simple and feasible process, controllable quality, stable curative effect, high content of effective components, high curative effect, homogeneous granularity and high stability.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clear, the present invention is further described in detail below with reference to examples. It should be understood that the specific embodiments described herein are only for better understanding of the technical solutions of the present invention, and are not intended to limit the present invention.
The cold treating granule consists of the following raw material medicines in parts by weight:
25-45 parts of wild chrysanthemum;
20-40 parts of holly;
20-40 parts of houttuynia cordata;
15-25 parts of bitter apricot seeds;
30-60 parts of fructus forsythiae;
60-180 parts of golden pomelo peel.
A preparation method of cold granules comprises the following steps:
step S110, pulverizing and mixing the houttuynia cordata and the golden pomelo peel, sieving, introducing steam for distillation to obtain volatile oil, filtrate A and solid residue A, concentrating the volatile oil under reduced pressure, freeze-drying in vacuum, and encapsulating with beta-cyclodextrin to obtain the clathrate A.
Vacuum freeze drying flos Chrysanthemi Indici, flos Ilicis Asprellae and fructus forsythiae, removing water, pulverizing, sieving, adding ethanol solution, soaking, and ultrasonic extracting to obtain filtrate B and solid residue B;
pulverizing semen Armeniacae amarum, sieving, soaking in ethanol, and distilling with steam to obtain semen Armeniacae amarum water and solid residue C.
Golden pomelo is mostly produced in Meizhou, Guangdong, etc., and the compendium of materia Medica records: the pomelo peel is pungent, bitter and warm in taste, has the functions of eliminating phlegm and stopping cough, and regulating qi to alleviate pain, so the pomelo peel can be used as a medicine, and the contained naringenin has the effect of spasmolysis, which is consistent with the fact that the Li Shizhen says that the pomelo peel has the effect of' dispersing anger. In recent years, scientific and technical personnel further research the golden pomelos by using modern science and technology, and the golden pomelos contain various amino acids required by human bodies, abundant vitamins C, B1, carotene and the like, contain more abundant naringin and belong to natural plant flavone. Fructus Citri Grandis flavone has antiinflammatory, blood lipid reducing and blood viscosity lowering effects.
According to the method, the volatile oil is extracted from the golden pomelos in a steam distillation mode, and the remaining filtrate and residue are recycled, so that the extraction degree of the effective components is high, and the activity is well maintained.
The wild chrysanthemum flower, the roughhaired holly root and the weeping forsythia are subjected to vacuum freeze drying for dewatering, then are soaked and are subjected to ultrasonic extraction, and the cell walls of the plant components can be embrittled by the treatment process, so that the wall breaking ratio is high, and the extraction degree of the effective components is high.
And step S120, mixing the solid residue A, the solid residue B and the solid residue C, adding the filtrate A and the filtrate B, adding water, decocting, filtering, centrifuging and clarifying the filtrate, and concentrating under reduced pressure to obtain thick paste.
And S130, mixing the inclusion A obtained in the step S110 with the thick paste obtained in the step S120, adding dextrin and sucralose, spraying the almond juice obtained in the step S110, uniformly mixing, and granulating.
The common cold granules and the preparation method thereof utilize the golden pomelo which is produced in Guangdong Meizhou province and the like mostly, the pomelo peel has the effects of reducing phlegm and relieving cough and regulating qi to alleviate pain due to pungent, bitter and warm natures, and the traditional Chinese medicine theory is used as guidance, and distillation extraction and vacuum drying processes are carried out on the natures and the tastes of the raw material medicines; effectively extracts the active ingredients in the medicine and improves the curative effect of the medicine. Simple and feasible process, controllable quality, stable curative effect, high content of effective components, high curative effect, homogeneous granularity and high stability.
In one embodiment, in step S110, the preparation of the clathrate a specifically includes:
pulverizing herba Houttuyniae and pericarpium Citri Grandis, mixing, sieving, adding 6-8 times of water, soaking at room temperature for 4-5 hr, and distilling under heating for 4-6 hr to obtain volatile oil, filtrate A and solid residue A; concentrating volatile oil under reduced pressure, vacuum freeze drying, and dissolving the dried product in 2-3 times of 75-95% ethanol to obtain solution A; dissolving BETA-cyclodextrin in 4-5 times of 60-75 deg.C water to obtain solution B; mixing solution A and solution B, stirring for 2-4h, and vacuum freeze drying to obtain white powder, i.e. clathrate A.
In one embodiment, in step S110, the preparing of the filtrate B and the solid residue B specifically includes:
slicing and dishing wild chrysanthemum, holly and fructus forsythiae respectively, and freezing at-38 to-35 ℃ for 4 to 5 hours;
keeping the frozen wild chrysanthemum, holly and forsythia slices at the pressure of 70-110 Pa and the temperature of 50-85 ℃ for 15-18 hours for vacuum drying to obtain mixed dry slices, wherein the water content of the mixed dry slices is 3-5%;
adding 5 times of 20-25% ethanol solution into the mixed dry tablet, keeping the temperature at 35-40 deg.C, introducing reverse current and forward current alternately for three times respectively, and performing ultrasonic extraction for 5-10min to obtain filtrate B and solid residue B.
In one embodiment, in step S110, the preparation of the almond water specifically includes:
pulverizing semen Armeniacae amarum, sieving, soaking in 1-2 times volume of 50-60% ethanol for 30-45min, adding 5-7 times volume of water solution, and heating and distilling to obtain semen Armeniacae amarum water and solid residue C.
In one embodiment, the step S120 specifically includes:
mixing the solid residue A, the solid residue B and the solid residue C, adding the filtrate A and the filtrate B, adding water to 4-6 times of volume, decocting for 2-3 times, each time for 1-2h, filtering, concentrating the filtrate with a vacuum concentration tank to obtain a concentrated solution with a relative density of 1.03, and centrifuging at a super high speed of 15000 r/min until the concentrated solution is clear; concentrating the separated liquid to obtain soft extract with relative density of 1.20-1.30.
In one embodiment, the traditional Chinese medicine composition is prepared from the following raw material medicines in parts by weight:
25 parts of wild chrysanthemum;
30 parts of holly;
30 parts of houttuynia cordata;
25 parts of bitter almond;
60 parts of fructus forsythiae;
80 parts of golden pomelo peel.
In one embodiment, the traditional Chinese medicine composition is prepared from the following raw material medicines in parts by weight:
35 parts of wild chrysanthemum;
40 parts of holly;
40 parts of houttuynia cordata;
20 parts of bitter almond;
50 parts of fructus forsythiae;
120 parts of golden pomelo peel.
In one embodiment, the traditional Chinese medicine composition is prepared from the following raw material medicines in parts by weight:
45 parts of wild chrysanthemum;
20 parts of holly;
20 parts of houttuynia cordata;
15 parts of bitter almond;
40 parts of fructus forsythiae;
140 parts of golden pomelo peel.
In one embodiment, the traditional Chinese medicine composition is prepared from the following raw material medicines in parts by weight:
25 parts of wild chrysanthemum;
30 parts of holly;
30 parts of houttuynia cordata;
15 parts of bitter almond;
30 parts of fructus forsythiae;
180 parts of golden pomelo peel.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims (10)

1. The cold treating granule is characterized by comprising the following raw material medicines in parts by weight:
25-45 parts of wild chrysanthemum;
20-40 parts of holly;
20-40 parts of houttuynia cordata;
15-25 parts of bitter apricot seeds;
30-60 parts of fructus forsythiae;
60-180 parts of golden pomelo peel.
2. The cold granules of claim 1, wherein the cold granules comprise the following raw material medicines in parts by weight:
25 parts of wild chrysanthemum;
30 parts of holly;
30 parts of houttuynia cordata;
25 parts of bitter almond;
60 parts of fructus forsythiae;
80 parts of golden pomelo peel.
3. The cold granules of claim 1, wherein the cold granules comprise the following raw material medicines in parts by weight:
35 parts of wild chrysanthemum;
40 parts of holly;
40 parts of houttuynia cordata;
20 parts of bitter almond;
50 parts of fructus forsythiae;
120 parts of golden pomelo peel.
4. The cold granules of claim 1, wherein the cold granules comprise the following raw material medicines in parts by weight:
45 parts of wild chrysanthemum;
20 parts of holly;
20 parts of houttuynia cordata;
15 parts of bitter almond;
40 parts of fructus forsythiae;
140 parts of golden pomelo peel.
5. The cold granules of claim 1, wherein the cold granules comprise the following raw material medicines in parts by weight:
25 parts of wild chrysanthemum;
30 parts of holly;
30 parts of houttuynia cordata;
15 parts of bitter almond;
30 parts of fructus forsythiae;
180 parts of golden pomelo peel.
6. A method for preparing cold granules according to any one of claims 1 to 5, comprising the steps of:
s110, pulverizing and mixing houttuynia cordata and golden pomelo peel, sieving, introducing steam for distillation to obtain volatile oil, filtrate A and solid residue A, concentrating the volatile oil under reduced pressure, freeze-drying in vacuum, and clathrating with beta-cyclodextrin to obtain clathrate A;
vacuum freeze drying flos Chrysanthemi Indici, flos Ilicis Asprellae and fructus forsythiae, removing water, pulverizing, sieving, adding ethanol solution, soaking, and ultrasonic extracting to obtain filtrate B and solid residue B;
pulverizing semen Armeniacae amarum, sieving, soaking in ethanol, and distilling with steam to obtain semen Armeniacae amarum water and solid residue C;
s120, mixing the solid residue A, the solid residue B and the solid residue C, adding the filtrate A and the filtrate B, adding water, decocting, filtering, centrifuging and clarifying the filtrate, and concentrating under reduced pressure to obtain thick paste;
s130, mixing the inclusion A obtained in the step S110 with the thick paste obtained in the step S120, adding dextrin and sucralose, spraying the almond juice obtained in the step S110, uniformly mixing, and granulating.
7. The method for preparing cold granules according to claim 6, wherein in the step S110, the preparation of the clathrate A specifically comprises:
pulverizing herba Houttuyniae and pericarpium Citri Grandis, mixing, sieving, adding 6-8 times of water, soaking at room temperature for 4-5 hr, and distilling under heating for 4-6 hr to obtain volatile oil, filtrate A and solid residue A; concentrating volatile oil under reduced pressure, vacuum freeze drying, and dissolving the dried product in 2-3 times of 75-95% ethanol to obtain solution A; dissolving BETA-cyclodextrin in 4-5 times of 60-75 deg.C water to obtain solution B; mixing solution A and solution B, stirring for 2-4h, and vacuum freeze drying to obtain white powder, i.e. clathrate A.
8. The method of claim 6, wherein the step S110 of preparing the filtrate B and the solid residue B specifically comprises:
slicing and dishing wild chrysanthemum, holly and fructus forsythiae respectively, and freezing at-38 to-35 ℃ for 4 to 5 hours;
keeping the frozen wild chrysanthemum, holly and forsythia slices at the pressure of 70-110 Pa and the temperature of 50-85 ℃ for 15-18 hours for vacuum drying to obtain mixed dry slices, wherein the water content of the mixed dry slices is 3-5%;
adding 5 times of 20-25% ethanol solution into the mixed dry tablet, keeping the temperature at 35-40 deg.C, introducing reverse current and forward current alternately for three times respectively, and performing ultrasonic extraction for 5-10min to obtain filtrate B and solid residue B.
9. The method for preparing cold granules according to claim 8, wherein in step S110, the preparation of the almond water specifically comprises:
pulverizing semen Armeniacae amarum, sieving, soaking in 1-2 times volume of 50-60% ethanol for 30-45min, adding 5-7 times volume of water solution, and heating and distilling to obtain semen Armeniacae amarum water and solid residue C.
10. The method for preparing cold granules according to any one of claims 6 to 9, wherein the step S120 specifically comprises:
mixing the solid residue A, the solid residue B and the solid residue C, adding the filtrate A and the filtrate B, adding water to 4-6 times of volume, decocting for 2-3 times, each time for 1-2h, filtering, concentrating the filtrate with a vacuum concentration tank to obtain a concentrated solution with a relative density of 1.03, and centrifuging at a super high speed of 15000 r/min until the concentrated solution is clear; concentrating the separated liquid to obtain soft extract with relative density of 1.20-1.30.
CN201910889808.2A 2019-09-20 2019-09-20 Cold granules and preparation method thereof Pending CN110772573A (en)

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Application publication date: 20200211