CN112006996A - Quick production method of traditional Chinese medicine formula granules - Google Patents
Quick production method of traditional Chinese medicine formula granules Download PDFInfo
- Publication number
- CN112006996A CN112006996A CN202010901836.4A CN202010901836A CN112006996A CN 112006996 A CN112006996 A CN 112006996A CN 202010901836 A CN202010901836 A CN 202010901836A CN 112006996 A CN112006996 A CN 112006996A
- Authority
- CN
- China
- Prior art keywords
- decoction
- drying
- composite particles
- inorganic composite
- ultrasonic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 239000008187 granular material Substances 0.000 title claims abstract description 46
- 239000003814 drug Substances 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- 239000011246 composite particle Substances 0.000 claims abstract description 59
- 238000001035 drying Methods 0.000 claims abstract description 34
- 239000000463 material Substances 0.000 claims abstract description 34
- 238000001704 evaporation Methods 0.000 claims abstract description 29
- 230000008020 evaporation Effects 0.000 claims abstract description 29
- 238000000926 separation method Methods 0.000 claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 23
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims description 40
- 239000000243 solution Substances 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 238000001914 filtration Methods 0.000 claims description 22
- 239000004113 Sepiolite Substances 0.000 claims description 20
- 239000011259 mixed solution Substances 0.000 claims description 20
- 229910052624 sepiolite Inorganic materials 0.000 claims description 20
- 238000005469 granulation Methods 0.000 claims description 17
- 230000003179 granulation Effects 0.000 claims description 17
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 13
- 235000019355 sepiolite Nutrition 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 13
- 238000001694 spray drying Methods 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 10
- 239000007921 spray Substances 0.000 claims description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 5
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- 238000002604 ultrasonography Methods 0.000 claims 1
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- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 6
- IVTMALDHFAHOGL-UHFFFAOYSA-N eriodictyol 7-O-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C=C3C(C(C(O)=C(O3)C=3C=C(O)C(O)=CC=3)=O)=C(O)C=2)O1 IVTMALDHFAHOGL-UHFFFAOYSA-N 0.000 description 6
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- IKGXIBQEEMLURG-BKUODXTLSA-N rutin Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@@H]1OC[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-BKUODXTLSA-N 0.000 description 6
- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 description 6
- 235000005493 rutin Nutrition 0.000 description 6
- 229960004555 rutoside Drugs 0.000 description 6
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 230000002279 cholagogic effect Effects 0.000 description 5
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- YKRGDOXKVOZESV-WRJNSLSBSA-N Paeoniflorin Chemical compound C([C@]12[C@H]3O[C@]4(O)C[C@](O3)([C@]1(C[C@@H]42)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)C)OC(=O)C1=CC=CC=C1 YKRGDOXKVOZESV-WRJNSLSBSA-N 0.000 description 3
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- 235000008216 herbs Nutrition 0.000 description 3
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- YKRGDOXKVOZESV-UHFFFAOYSA-N paeoniflorin Natural products O1C(C)(C2(CC34)OC5C(C(O)C(O)C(CO)O5)O)CC3(O)OC1C24COC(=O)C1=CC=CC=C1 YKRGDOXKVOZESV-UHFFFAOYSA-N 0.000 description 3
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- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- 235000009051 Ambrosia paniculata var. peruviana Nutrition 0.000 description 1
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- 240000001851 Artemisia dracunculus Species 0.000 description 1
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- 235000003261 Artemisia vulgaris Nutrition 0.000 description 1
- 235000006200 Glycyrrhiza glabra Nutrition 0.000 description 1
- 244000303040 Glycyrrhiza glabra Species 0.000 description 1
- 235000002598 Inula helenium Nutrition 0.000 description 1
- 244000116484 Inula helenium Species 0.000 description 1
- 241001571764 Lysimachia christinae Species 0.000 description 1
- 240000003065 Malva verticillata Species 0.000 description 1
- 235000002384 Malva verticillata Nutrition 0.000 description 1
- 240000004980 Rheum officinale Species 0.000 description 1
- 235000008081 Rheum officinale Nutrition 0.000 description 1
- 241000301400 Trogopterus Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000001138 artemisia absinthium Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 210000003038 endothelium Anatomy 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 210000003608 fece Anatomy 0.000 description 1
- LPLVUJXQOOQHMX-QWBHMCJMSA-N glycyrrhizinic acid Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@H](O[C@@H]1O[C@@H]1C([C@H]2[C@]([C@@H]3[C@@]([C@@]4(CC[C@@]5(C)CC[C@@](C)(C[C@H]5C4=CC3=O)C(O)=O)C)(C)CC2)(C)CC1)(C)C)C(O)=O)[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@H]1O LPLVUJXQOOQHMX-QWBHMCJMSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 235000011477 liquorice Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 239000012466 permeate Substances 0.000 description 1
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- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 208000011580 syndromic disease Diseases 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 0.000 description 1
Classifications
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- 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
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Abstract
The invention provides a rapid production method of traditional Chinese medicine formula granules, which comprises the following steps: 1) ultrasonic decoction: putting the raw medicinal materials, the inorganic composite particles and the solvent into a container, and carrying out ultrasonic decoction to obtain a decoction liquid; 2) separation: carrying out solid-liquid separation on the decoction obtained in the step 1) to obtain an extracting solution; 3) flash evaporation and concentration: carrying out flash evaporation concentration on the extracting solution to obtain an extract; 4) drying and granulating: drying and granulating the extract obtained in the step 2) to obtain the traditional Chinese medicine formula granules. The invention adopts ultrasonic waves and inorganic composite particles to assist the solvent for decoction, can obtain high extraction rate by one-time decoction, effectively shortens the extraction time and greatly improves the extraction rate of the active ingredients of the medicinal materials.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicines, in particular to a rapid production method of traditional Chinese medicine formula granules.
Background
The Chinese medicine prescription granule is a pure Chinese medicine product series which is prepared by using traditional Chinese medicine decoction pieces which meet the processing specifications as raw materials and carrying out extraction, concentration, separation, drying, granulation and packaging refining by modern pharmaceutical technology. The traditional Chinese medicine decoction pieces have the advantages of ensuring all characteristics of the original traditional Chinese medicine decoction pieces, satisfying the requirements of doctors for treatment based on syndrome differentiation, having strong medicine property and high medicine effect when added or subtracted according to the symptoms, having no need of decoction, direct taking with water, small dosage, rapid action, complete components, exact curative effect, safety, sanitation, convenient carrying and storage, easy modulation, suitability for industrial production and the like.
In the existing preparation method, the extraction step generally adopts a heating reflux method, and the effective components in the medicinal materials can be extracted by multiple times of reflux, so that the preparation time is long; the used drying granulation process has the phenomenon of wall sticking, so that medicinal materials are wasted, and the drying granulation effect is poor, so that the traditional Chinese medicine particles are poor in forming. The whole manufacturing process is long in time consumption and cannot meet the requirements of modern industrial production.
Disclosure of Invention
The invention aims to solve the problems and provides a preparation method of a traditional Chinese medicine formula granule with rapidness and good product quality.
The invention provides a rapid production method of traditional Chinese medicine formula granules, which comprises the following steps:
1) ultrasonic decoction: putting the raw medicinal materials, the inorganic composite particles and the solvent into a container, and carrying out ultrasonic decoction to obtain a decoction liquid;
2) separation: carrying out solid-liquid separation on the decoction obtained in the step 1) to obtain an extracting solution;
3) flash evaporation and concentration: carrying out flash evaporation concentration on the extracting solution to obtain an extract;
4) drying and granulating: drying and granulating the extract obtained in the step 2) to obtain the traditional Chinese medicine formula granules.
The invention utilizes the high-speed and strong cavitation effect and stirring action generated by sound waves to destroy the cells of the plant medicinal materials and ensure that the solvent permeates into the medicinal material cells; the auxiliary materials are inorganic composite particles, and the inorganic composite particles collide with the traditional Chinese medicinal materials strongly and disorderly in the ultrasonic decoction process, so that the crushing of the plant medicinal materials is accelerated, the plant medicinal materials are crushed to a nano level with smaller particle size, and the extraction of effective components in the medicinal materials is facilitated. The medicinal materials do not need to be pretreated before decoction, and the high extraction rate can be obtained by one-time decoction. In addition, flash evaporation concentration is adopted, so that the drug effect is greatly kept; the drying and granulating method is simple, and the prepared granules are well formed.
Further, the inorganic composite particles in step 1) are: the aluminum oxide-sepiolite powder composite particle comprises the following components in percentage by mass: 0.1 to 1.
Further, the preparation method of the inorganic composite particles in the step 1) comprises the following steps:
s1, adding sepiolite powder into the mixed solution of 1, 4-butanediol and acetone, and uniformly mixing to obtain a mixed solution; adding aluminum oxide into the mixed solution, stirring for a period of time, centrifuging, and filtering to obtain filter residue;
and S2, adding the filter residue into an ethanol/water mixed solution of a silane coupling agent, stirring for a period of time, filtering, drying, and calcining at 1150-1300 ℃ for 2 hours to obtain the aluminum oxide-sepiolite powder composite particles.
The aluminum oxide has weak hydrophilicity, the surface of the aluminum oxide has strong hydrophilicity after being modified in the steps S1 and S2, the aluminum oxide strongly collides with the traditional Chinese medicinal materials under the ultrasonic condition, active ingredients contained in the traditional Chinese medicinal materials are released by utilizing the hydrophilicity of the aluminum oxide, the function of a bridge between the traditional Chinese medicinal materials and water is realized, and the extraction of the active ingredients is accelerated.
Further, the ultrasonic decoction in the step 1) is as follows: the ultrasonic frequency is 2-10 kHz, and the decoction time is 0.5-2 h.
Further, the solid-liquid separation in the step 2) is filtration separation, and/or centrifugal separation, and/or membrane separation.
Further, the temperature of flash evaporation concentration in the step 3) is 40-70 ℃, and the vacuum degree is as follows: -0.10 to 0.05 MPa.
Further, the relative density of the extract in the step 3) is 1.0-1.5.
Further, the drying and granulating in the step 4) specifically comprises the following steps: adding adjuvants into the extract, mixing, spray drying, and granulating; the spray drying granulation specifically comprises the following steps: and drying by adopting a spray dryer, wherein the air inlet temperature is 150-200 ℃, the air outlet temperature is 75-90 ℃, the liquid inlet temperature is 90-100 ℃, and the rotation speed of an atomizer is 1000-1500 r/min.
Further, the drying and granulating in the step 4) is specifically fluidized bed drying and granulating, and the temperature is 50-90 ℃.
Further, the adding amount of the solvent for ultrasonic decoction in the step 1) is 6-15 times of the weight of the raw medicinal materials.
The invention can obtain at least one of the following beneficial effects:
1. the invention adopts ultrasonic waves and inorganic composite particles to assist the solvent for decoction, can obtain high extraction rate by one-time decoction, effectively shortens the extraction time and greatly improves the extraction rate of the active ingredients of the medicinal materials.
2. The inorganic composite particles adopted by the invention do not influence the components of the traditional Chinese medicine formula particles and the drug effect; and can promote extraction of active ingredients of Chinese medicinal materials and shorten extraction time.
3. The production method of the invention does not affect the active ingredients of the Chinese medicinal materials, and greatly maintains the drug effect.
4. The production method of the invention has high powder yield and good molding of the prepared particles.
5. The whole production process flow is short in time consumption, and the obtained traditional Chinese medicine formula granules are accurate in formula amount and can be applied to industrial production.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A preparation method of granule for removing calculus and promoting gallbladder function is provided.
Example 1:
the calculus-removing and gallbladder-benefiting granule comprises the following raw material medicines in parts by weight: 10 parts of radix bupleuri, 8 parts of elecampane, 15 parts of radix curcumae, 17 parts of lysimachia christinae hance, 11 parts of oriental wormwood, 7 parts of radix scutellariae, 5 parts of trogopterus dung, 5 parts of pollen typhae, 7 parts of fructus toosendan, 13 parts of radix paeoniae rubra, 11 parts of malva verticillata, 12 parts of talcum powder, 11 parts of rheum officinale, 5 parts of fructus aurantii, 9 parts of semen raphani, 6 parts of rhizoma atractylodis macrocephalae, 15 parts of semen coicis, 6 parts of endothelium corneum gigeriae galli, 7 parts of liquorice, 6 parts of pyr.
The preparation method of the inorganic composite particles comprises the following steps:
s1, adding sepiolite powder into a mixed solution of 1, 4-butanediol and acetone (mass ratio is 1: 10), and uniformly mixing to obtain a mixed solution; adding aluminum oxide with the mass of 80 times that of the sepiolite powder into the mixed solution, stirring for 15min, centrifuging, and filtering to obtain filter residue;
and S2, adding the filter residue into an ethanol/water mixed solution (mass ratio is 2: 8: 1) of a silane coupling agent, stirring for 30min, filtering, drying in vacuum at 80 ℃, and calcining at 1250 ℃ for 2h to obtain the aluminum oxide-sepiolite powder composite particles.
A method for quickly producing calculus-removing and gallbladder-benefiting granules comprises the following steps:
1) ultrasonic decoction: placing the raw medicinal materials, the inorganic composite particles and water in a container, and carrying out ultrasonic decoction, wherein the adding amount of the inorganic composite particles and the water is 1/8 times and 10 times of the weight of the raw medicinal materials respectively, the ultrasonic frequency is 5kHz, and the decoction time is 1.5h, so as to obtain a decoction;
2) separation: filtering the decoction obtained in the step 1), and removing filter residues to obtain an extracting solution;
3) flash evaporation and concentration: flash evaporation concentration is carried out on the extracting solution, the temperature is 50 ℃, and the vacuum degree is as follows: concentrating the extracting solution to the relative density of 1.25 under the pressure of-0.10 MPa to obtain an extract;
4) drying and granulating: and (3) spray-drying the extract obtained in the step 2), wherein the air inlet temperature of a spray dryer is 180 ℃, the air outlet temperature is 80 ℃, the liquid inlet temperature is 90 ℃, and the rotation speed of an atomizer is 1200r/min to obtain fine powder, and then carrying out dry extrusion granulation on the fine powder to obtain the calculus-removing and cholagogic granules.
Example 2:
the composition of the raw material materials and the inorganic composite particles in this example were the same as those in example 1.
A method for quickly producing calculus-removing and gallbladder-benefiting granules comprises the following steps:
1) ultrasonic decoction: placing the raw medicinal materials, the inorganic composite particles and water in a container, and carrying out ultrasonic decoction, wherein the adding amount of the inorganic composite particles and the water is 1/5 and 10 times of the weight of the raw medicinal materials respectively, the ultrasonic frequency is 8kHz, and the decoction time is 0.5h, so as to obtain a decoction;
2) separation: filtering the decoction obtained in the step 1), and removing filter residues to obtain an extracting solution;
3) flash evaporation and concentration: flash evaporation concentration is carried out on the extracting solution, the temperature is 70 ℃, and the vacuum degree is as follows: concentrating the extracting solution to the relative density of 1.2 under the pressure of-0.06 MPa to obtain an extract;
4) drying and granulating: drying the extract obtained in the step 2) by a fluidized bed at the temperature of 80 ℃, and then carrying out dry extrusion granulation to obtain the calculus removing and cholagogic granules.
Example 3:
the composition of the raw material herbs in this example is the same as that in example 1.
The preparation method of the inorganic composite particles comprises the following steps:
s1, adding sepiolite powder into a mixed solution of 1, 4-butanediol and acetone (mass ratio is 1.5: 10), and uniformly mixing to obtain a mixed solution; adding aluminum oxide 50 times the mass of sepiolite powder into the mixed solution, stirring for 15min, centrifuging, and filtering to obtain filter residue;
and S2, adding the filter residue into an ethanol/water mixed solution (mass ratio is 2: 8: 1) of a silane coupling agent, stirring for 30min, filtering, drying in vacuum at 80 ℃, and calcining at 1200 ℃ for 2h to obtain the aluminum oxide-sepiolite powder composite particles.
A method for quickly producing calculus-removing and gallbladder-benefiting granules comprises the following steps:
1) ultrasonic decoction: placing the raw medicinal materials, the inorganic composite particles and water in a container, and carrying out ultrasonic decoction, wherein the adding amount of the inorganic composite particles and the water is respectively 1 time and 12 times of the weight of the raw medicinal materials, the ultrasonic frequency is 6kHz, and the decoction time is 2 hours, so as to obtain a decoction;
2) separation: filtering the decoction obtained in the step 1), and removing filter residues to obtain an extracting solution;
3) flash evaporation and concentration: flash evaporation concentration is carried out on the extracting solution, the temperature is 60 ℃, and the vacuum degree is as follows: concentrating the extracting solution to the relative density of 1.3 under the pressure of-0.08 MPa to obtain an extract;
4) drying and granulating: and (3) spray-drying the extract obtained in the step 2), wherein the air inlet temperature of a spray dryer is 170 ℃, the air outlet temperature is 90 ℃, the liquid inlet temperature is 90 ℃, and the rotation speed of an atomizer is 1400r/min to obtain fine powder, and then carrying out dry extrusion granulation on the fine powder to obtain the calculus-removing and cholagogic granules.
Example 4:
the composition of the raw material herbs in this example is the same as that in example 1.
The preparation method of the inorganic composite particles comprises the following steps:
s1, adding sepiolite powder into a mixed solution of 1, 4-butanediol and acetone (mass ratio is 1: 5), and uniformly mixing to obtain a mixed solution; adding aluminum oxide with the mass being 10 times that of the sepiolite powder into the mixed solution, stirring for 15min, centrifuging, and filtering to obtain filter residue;
and S2, adding the filter residue into an ethanol/water mixed solution (mass ratio is 2: 7: 1) of a silane coupling agent, stirring for 30min, filtering, drying in vacuum at 80 ℃, and calcining at 1250 ℃ for 2h to obtain the aluminum oxide-sepiolite powder composite particles.
A method for quickly producing calculus-removing and gallbladder-benefiting granules comprises the following steps:
1) ultrasonic decoction: placing the raw medicinal materials, the inorganic composite particles and water in a container, and carrying out ultrasonic decoction, wherein the adding amount of the inorganic composite particles and the water is 1/3 times and 8 times of the weight of the raw medicinal materials respectively, the ultrasonic frequency is 6.5kHz, and the decoction time is 1.5h, so as to obtain a decoction;
2) separation: filtering the decoction obtained in the step 1), and removing filter residues to obtain an extracting solution;
3) flash evaporation and concentration: flash evaporation concentration is carried out on the extracting solution, the temperature is 40 ℃, and the vacuum degree is as follows: concentrating the extracting solution to the relative density of 1.35 under the pressure of-0.08 MPa to obtain an extract;
4) drying and granulating: and (3) spray-drying the extract obtained in the step 2), wherein the air inlet temperature of a spray dryer is 160 ℃, the air outlet temperature is 80 ℃, the liquid inlet temperature is 95 ℃, and the rotation speed of an atomizer is 1300r/min to obtain fine powder, and then carrying out dry extrusion granulation on the fine powder to obtain the calculus-removing and cholagogic granules.
Example 5:
the composition of the raw material herbs in this example is the same as that in example 1.
In the preparation method of the inorganic composite particle, the amount of the added alumina is 20 times of the weight of the sepiolite powder, and the rest is the same as that of the embodiment 4.
A method for quickly producing calculus-removing and gallbladder-benefiting granules comprises the following steps:
1) ultrasonic decoction: placing the raw medicinal materials, the inorganic composite particles and water in a container, and carrying out ultrasonic decoction, wherein the adding amount of the inorganic composite particles and the water is 1/2 and 10 times of the weight of the raw medicinal materials respectively, the ultrasonic frequency is 7kHz, and the decoction time is 1h, so as to obtain a decoction;
2) separation: filtering the decoction obtained in the step 1), and removing filter residues to obtain an extracting solution;
3) flash evaporation and concentration: flash evaporation concentration is carried out on the extracting solution, the temperature is 60 ℃, and the vacuum degree is as follows: concentrating the extracting solution to the relative density of 1.25 under the pressure of-0.10 MPa to obtain an extract;
4) drying and granulating: and (3) spray-drying the extract obtained in the step 2), wherein the air inlet temperature of a spray dryer is 160 ℃, the air outlet temperature is 80 ℃, the liquid inlet temperature is 95 ℃, and the rotation speed of an atomizer is 1200r/min to obtain fine powder, and then carrying out dry extrusion granulation on the fine powder to obtain the calculus-removing and cholagogic granules.
The inorganic composite particles can be repeatedly used, and are separated by utilizing the density difference between the inorganic composite particles and the traditional Chinese medicinal materials.
Comparative example 1:
the procedure of example 5 was repeated except that the inorganic composite particles were not added.
Comparative example 2:
the decoction was carried out while stirring without sonication, and the rest of the procedure was the same as in example 5.
Comparative example 3:
the inorganic composite particles were replaced with alumina and sepiolite powder, and the remaining steps were the same as in example 5.
Comparative example 4:
the inorganic composite particles were replaced with alumina, and the remaining procedure was the same as in example 5.
Comparative example 5:
the invention patent CN 111388627A: the preparation method of the calculus removing and gallbladder promoting granule comprises the step of preparing the calculus removing and gallbladder promoting granule by the method of example 10.
The powder yield test of the fine powders of examples 1 to 5 and comparative examples 1 to 5 and the test of the effective components of paeoniflorin were carried out, and the extraction rate was used as an index, and the specific test methods are shown in comparative example 5: patent CN 111388627A.
TABLE 1
| Yield (%) | Extraction ratio of paeoniflorin (%) | |
| Example 1 | 79.3 | 7.5 |
| Example 2 | 78.6 | 7.8 |
| Example 3 | 80.2 | 7.2 |
| Example 4 | 79.5 | 8.1 |
| Example 5 | 85.5 | 8.0 |
| Comparative example 1 | 62.6 | 6.8 |
| Comparative example 2 | 63.4 | 6.2 |
| Comparative example 3 | 66.8 | 6.5 |
| Comparative example 4 | 67.1 | 6.1 |
| Comparative example 5 | 69 | 6.1 |
As can be seen from the data in Table 1, the data in Table 2 show that the product quality of the granules is greatly influenced by adding no inorganic composite granules (comparative example 1), adding no aluminum oxide or sepiolite powder directly (comparative example 3) or adding only aluminum oxide (comparative example 4), and the total flavone content and the rutin content are far lower than those of the example 10. The total flavone content and rutin content of the product obtained by multiple reflux extraction (comparative example 5) are far lower than those of the product obtained in example 5, but the method only carries out one-time short-time decoction, and the powder obtaining rate and the paeoniflorin extraction rate can reach 85.5 percent and 8.0 percent, and the results show that the method has the advantages of rapidness, high efficiency and high extraction rate.
Example 6:
the inorganic composite particles were prepared in the same manner as in example 1.
A rapid production method of fried sophora flower formula granules comprises the following steps:
1) ultrasonic decoction: putting the fried sophora japonica decoction pieces, the inorganic composite particles and water into a container, and carrying out ultrasonic decoction, wherein the adding amount of the inorganic composite particles and the water is 1/8 times and 12 times of the weight of the fried sophora japonica decoction pieces respectively, the ultrasonic frequency is 10kHz, and the decoction time is 0.5h, so as to obtain decoction liquid;
2) separation: filtering the decoction obtained in the step 1), and removing filter residues to obtain an extracting solution;
3) flash evaporation and concentration: flash evaporation concentration is carried out on the extracting solution, the temperature is 50 ℃, and the vacuum degree is as follows: concentrating the extracting solution to the relative density of 1.2 under the pressure of-0.08 MPa to obtain an extract;
4) drying and granulating: and (3) spray-drying the extract obtained in the step 2), wherein the air inlet temperature of a spray dryer is 180 ℃, the air outlet temperature is 80 ℃, the liquid inlet temperature is 90 ℃, and the rotation speed of an atomizer is 1200r/min to obtain fine powder, and then carrying out dry extrusion granulation on the fine powder to obtain the fried sophora flower formula particles.
Example 7:
the preparation method of the inorganic composite particles was the same as in example 2.
A rapid production method of fried sophora flower formula granules comprises the following steps:
1) ultrasonic decoction: putting the fried sophora japonica decoction pieces, the inorganic composite particles and water into a container, and carrying out ultrasonic decoction, wherein the adding amount of the inorganic composite particles and the water is 1/5 times and 10 times of the weight of the fried sophora japonica decoction pieces respectively, the ultrasonic frequency is 6kHz, and the decoction time is 0.75h, so as to obtain decoction liquid;
2) separation: filtering the decoction obtained in the step 1), and removing filter residues to obtain an extracting solution;
3) flash evaporation and concentration: flash evaporation concentration is carried out on the extracting solution, the temperature is 70 ℃, and the vacuum degree is as follows: concentrating the extracting solution to the relative density of 1.2 under the pressure of-0.06 MPa to obtain an extract;
4) drying and granulating: drying the extract obtained in the step 2) by a fluidized bed at the temperature of 60 ℃, and then carrying out dry extrusion granulation to obtain the fried sophora flower formula particles.
Example 8:
the inorganic composite particles were prepared in the same manner as in example 3.
A rapid production method of fried sophora flower formula granules comprises the following steps:
1) ultrasonic decoction: putting the fried sophora japonica decoction pieces, the inorganic composite particles and water into a container, and carrying out ultrasonic decoction, wherein the adding amount of the inorganic composite particles and the water is respectively 1 time and 15 times of the weight of the fried sophora japonica decoction pieces, the ultrasonic frequency is 8kHz, and the decoction time is 0.5h, so as to obtain decoction liquid;
2) separation: filtering the decoction obtained in the step 1), and removing filter residues to obtain an extracting solution;
3) flash evaporation and concentration: flash evaporation concentration is carried out on the extracting solution, the temperature is 60 ℃, and the vacuum degree is as follows: concentrating the extracting solution to the relative density of 1.3 under the pressure of-0.08 MPa to obtain an extract;
4) drying and granulating: and (3) spray-drying the extract obtained in the step 2), wherein the air inlet temperature of a spray dryer is 170 ℃, the air outlet temperature is 90 ℃, the liquid inlet temperature is 90 ℃, and the rotation speed of an atomizer is 1400r/min to obtain fine powder, and then carrying out dry extrusion granulation on the fine powder to obtain the fried sophora flower formula particles.
Example 9:
the inorganic composite particles were prepared in the same manner as in example 4.
A rapid production method of fried sophora flower formula granules comprises the following steps:
1) ultrasonic decoction: putting the fried sophora japonica decoction pieces, the inorganic composite particles and water into a container, and carrying out ultrasonic decoction, wherein the adding amount of the inorganic composite particles and the water is 1/3 times and 9 times of the weight of the fried sophora japonica decoction pieces respectively, the ultrasonic frequency is 3.5kHz, and the decoction time is 1.25h, so as to obtain a decoction liquid;
2) separation: filtering the decoction obtained in the step 1), and removing filter residues to obtain an extracting solution;
3) flash evaporation and concentration: flash evaporation concentration is carried out on the extracting solution, the temperature is 40 ℃, and the vacuum degree is as follows: concentrating the extracting solution to the relative density of 1.35 under the pressure of-0.08 MPa to obtain an extract;
4) drying and granulating: and (3) spray-drying the extract obtained in the step 2), wherein the air inlet temperature of a spray dryer is 160 ℃, the air outlet temperature is 80 ℃, the liquid inlet temperature is 95 ℃, and the rotation speed of an atomizer is 1300r/min to obtain fine powder, and then carrying out dry extrusion granulation on the fine powder to obtain the fried sophora flower formula particles.
Example 10:
the inorganic composite particles were prepared in the same manner as in example 5.
A rapid production method of fried sophora flower formula granules comprises the following steps:
1) ultrasonic decoction: putting the fried sophora japonica decoction pieces, the inorganic composite particles and water into a container, and carrying out ultrasonic decoction, wherein the adding amount of the inorganic composite particles and the water is 1/2 times and 10 times of the weight of the fried sophora japonica decoction pieces respectively, the ultrasonic frequency is 7kHz, and the decoction time is 1h, so as to obtain a decoction liquid;
2) separation: filtering the decoction obtained in the step 1), and removing filter residues to obtain an extracting solution;
3) flash evaporation and concentration: flash evaporation concentration is carried out on the extracting solution, the temperature is 60 ℃, and the vacuum degree is as follows: concentrating the extracting solution to the relative density of 1.25 under the pressure of-0.10 MPa to obtain an extract;
4) drying and granulating: and (3) spray-drying the extract obtained in the step 2), wherein the air inlet temperature of a spray dryer is 160 ℃, the air outlet temperature is 80 ℃, the liquid inlet temperature is 95 ℃, and the rotation speed of an atomizer is 1200r/min to obtain fine powder, and then carrying out dry extrusion granulation on the fine powder to obtain the fried sophora flower formula particles.
The inorganic composite particles can be repeatedly used, and are separated by utilizing the density difference between the inorganic composite particles and the traditional Chinese medicinal materials.
Comparative example 6:
the procedure of example 5 was repeated except that the inorganic composite particles were not added.
Comparative example 7:
the decoction was carried out while stirring without sonication, and the rest of the procedure was the same as in example 5.
Comparative example 8:
the inorganic composite particles were replaced with alumina and sepiolite powder, and the remaining steps were the same as in example 5.
Comparative example 9:
the inorganic composite particles were replaced with alumina, and the remaining procedure was the same as in example 5.
Comparative example 10:
the invention patent CN 111467387A: a fried flos Sophorae Immaturus formula particle, and its preparation method and quality standard detection method are provided, wherein the fried flos Sophorae Immaturus formula particle is prepared by the method of trial study number 1 in the embodiment section.
Meanwhile, the effective components of the sophora japonica stir-fried formula granules in the examples 6-10 and the comparative examples 4-6 are tested, and the total flavone and the rutin are index components of the sophora japonica stir-fried formula granules, and the specific test method is shown in the comparative example 10: patent CN 111467387A.
TABLE 2
As can be seen from the data in Table 2, the product quality of the granules is greatly affected by adding no inorganic composite granules (comparative example 6), adding no aluminum oxide or sepiolite powder directly (comparative example 8) or adding only aluminum oxide (comparative example 9), and the total flavone content and the rutin content are far lower than those of the example 10. The content of total flavone and the content of rutin in the product obtained by multiple reflux extraction (comparative example 10) are far lower than those in example 10, but the method only carries out one-time decoction for a short time, and the content of total flavone and the content of rutin can reach 29.5 percent and 21.2 percent, and the result shows that the method has the advantages of rapidness, high efficiency and high extraction rate.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (10)
1. A rapid production method of traditional Chinese medicine formula granules is characterized by comprising the following steps:
1) ultrasonic decoction: putting the raw medicinal materials, the inorganic composite particles and the solvent into a container, and carrying out ultrasonic decoction to obtain a decoction liquid;
2) separation: carrying out solid-liquid separation on the decoction obtained in the step 1) to obtain an extracting solution;
3) flash evaporation and concentration: carrying out flash evaporation concentration on the extracting solution to obtain an extract;
4) drying and granulating: drying and granulating the extract obtained in the step 2) to obtain the traditional Chinese medicine formula granules.
2. The method for rapidly producing a granule formulation of Chinese traditional medicine according to claim 1, wherein the inorganic composite particles in step 1) are: the aluminum oxide-sepiolite powder composite particle comprises the following components in percentage by mass: 0.01 to 0.5.
3. The method for rapidly producing a Chinese medicinal granule according to claim 2, wherein the method for preparing the inorganic composite particles in step 1) comprises:
s1, adding sepiolite powder into the mixed solution of 1, 4-butanediol and acetone, and uniformly mixing to obtain a mixed solution; adding aluminum oxide into the mixed solution, stirring for a period of time, centrifuging, and filtering to obtain filter residue;
and S2, adding the filter residue into an ethanol/water mixed solution of a silane coupling agent, stirring for a period of time, filtering, drying, and calcining at 1150-1300 ℃ for 2 hours to obtain the aluminum oxide-sepiolite powder composite particles.
4. The method for rapid production of a granule formulation of Chinese traditional medicine according to claim 1, wherein the ultrasound decoction in step 1) is: the ultrasonic frequency is 2-10 kHz, and the decoction time is 0.5-2 h.
5. The method of claim 1, wherein the solid-liquid separation in step 2) is filtration separation, and/or centrifugation separation, and/or membrane separation.
6. The rapid production method of a traditional Chinese medicine formula granule as claimed in claim 1, wherein the temperature of flash evaporation concentration in step 3) is 40-70 ℃, and the vacuum degree is as follows: -0.10 to 0.05 MPa.
7. The rapid production method of a traditional Chinese medicine formula granule as claimed in claim 1, wherein the relative density of the extract in step 3) is 1.0-1.5.
8. The method for rapidly producing a granule of a Chinese medicinal formulation according to claim 1, wherein the dry granulation in step 4) is specifically: adding adjuvants into the extract, mixing, spray drying, and granulating; the spray drying granulation specifically comprises the following steps: and drying by adopting a spray dryer, wherein the air inlet temperature is 150-200 ℃, the air outlet temperature is 75-90 ℃, the liquid inlet temperature is 90-100 ℃, and the rotation speed of an atomizer is 1000-1500 r/min.
9. The method for rapidly producing the Chinese medicinal granule according to claim 1, wherein the drying granulation in the step 4) is fluidized bed drying granulation at a temperature of 50-90 ℃.
10. The method for rapidly producing a Chinese medicinal granule as claimed in claim 1, wherein the amount of the solvent for the ultrasonic decoction in step 1) is 6-15 times of the weight of the raw materials.
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