CN116270770A - Preparation method of drynaria rhizome formula particles - Google Patents
Preparation method of drynaria rhizome formula particles Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 13
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- 229940035034 maltodextrin Drugs 0.000 claims abstract description 14
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- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 description 2
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- 206010012735 Diarrhoea Diseases 0.000 description 1
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- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/11—Pteridophyta or Filicophyta (ferns)
- A61K36/12—Filicopsida or Pteridopsida
- A61K36/126—Drynaria
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
- A61K9/1605—Excipients; Inactive ingredients
- A61K9/1629—Organic macromolecular compounds
- A61K9/1652—Polysaccharides, e.g. alginate, cellulose derivatives; Cyclodextrin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
- A61K9/1682—Processes
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P1/00—Drugs for disorders of the alimentary tract or the digestive system
- A61P1/12—Antidiarrhoeals
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P13/00—Drugs for disorders of the urinary system
- A61P13/12—Drugs for disorders of the urinary system of the kidneys
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P19/00—Drugs for skeletal disorders
- A61P19/04—Drugs for skeletal disorders for non-specific disorders of the connective tissue
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P19/00—Drugs for skeletal disorders
- A61P19/08—Drugs for skeletal disorders for bone diseases, e.g. rachitism, Paget's disease
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P27/00—Drugs for disorders of the senses
- A61P27/16—Otologicals
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P29/00—Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention discloses a preparation method of drynaria rhizome formula particles, and belongs to the technical field of traditional Chinese medicine processing. The method comprises the following steps: soaking rhizoma Drynariae decoction pieces in water, reflux-extracting, filtering, concentrating, adding adjuvants, mixing, spray-drying to obtain dry extract powder, adding adjuvants, and dry granulating to obtain rhizoma Drynariae granule. The water adding amount for soaking is 3-12 times, and the soaking time is not less than 30 minutes; reflux extraction time is not less than 30 minutes, and extraction times are not less than 2 times; when filtering, the mesh number of the filter screen is not less than 300 meshes; vacuum concentrating at a heating temperature not higher than 65deg.C and vacuum degree of not less than-0.08 mpa to relative density of 1.15-1.20; the auxiliary material is selected from corn starch, dextrin or maltodextrin; the air inlet temperature of spray drying is 135-180deg.C, and the optimal temperature is 140-150deg.C. The drynaria rhizome formula particles obtained by adopting the scheme are packaged by adopting a composite aluminum film.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicine processing, in particular to a preparation method of drynaria rhizome formula particles.
Background
Rhizoma drynariae is a traditional Chinese medicine, also called as arborvitae or rhizoma drynariae, is the rhizome of wild plant drynaria fortunei, can be eaten as health-care food after harvesting, and can be used as medicine after sun drying. Rhizoma Drynariae is usually rhizome of Dryopteris fern, which is grown on tree, wall or stone wall, and is mainly distributed in Yunnan, taiwan, zhejiang, guangxi, jiangxi, fujian and other places in China, and is picked in spring and winter, and dried in the sun, fried or used for life after removing sediment and impurities. Sex flavor meridian tropism: warm nature and bitter taste; it enters liver and kidney meridians. The efficacy mainly treats: promoting blood circulation, tonifying kidney and strengthening bone, and is suitable for treating traumatic injury, soreness and weakness of waist and knees, deafness, tinnitus, chronic diarrhea and the like caused by bone and muscle injury and kidney deficiency.
The traditional processing method of the drynaria rhizome comprises the following steps: digging the medicinal materials, removing silt, drying or singeing to remove fuzz, packaging, and storing. After the decoction pieces are processed, washing, softening, slicing, drying and packaging are carried out. The prepared rhizoma drynariae decoction pieces have large volume and standard deviation in hygiene, are not beneficial to storage and have high storage and transportation costs. In addition, the quality stability of the decoction pieces is poor, the clinical curative effect is difficult to ensure, the administration of patients is inconvenient, and the onset of action is slow. The traditional decoction pieces are added into the rhizoma drynariae decoction pieces in the market at present, but the traditional decoction pieces are taken as raw materials, the quality of the traditional decoction pieces is determined, and the problem of medicinal material pollution cannot be solved by the superfine decoction pieces; the concentrated granules only extract water soluble components.
In order to better utilize the effective components in the drynaria rhizome, the development of decoction pieces into formula granules is also a necessary trend, which is beneficial to the utilization of various forms of resources of the traditional Chinese medicine and the convenience of patients to take.
Disclosure of Invention
In order to overcome the technical defects, the invention discloses a preparation method of drynaria rhizome formula particles, and belongs to the technical field of traditional Chinese medicine processing. The method comprises the following steps: soaking rhizoma Drynariae decoction pieces in water, reflux-extracting, filtering, concentrating, adding adjuvants, mixing, spray-drying, and dry granulating to obtain rhizoma Drynariae granule. The water adding amount for soaking is 3-12 times, and the soaking time is not less than 30 minutes; reflux extraction time is not less than 30 minutes, and extraction times are not less than 2 times; when filtering, the mesh number of the filter screen is not less than 300 meshes; vacuum concentrating at a heating temperature not higher than 65deg.C and vacuum degree of not less than-0.08 mpa to relative density of 1.15-1.20; the auxiliary material is selected from corn starch, dextrin or maltodextrin; the air inlet temperature of spray drying is 135-180deg.C, and the optimal temperature is 140-150deg.C. The drynaria rhizome formula particles obtained by adopting the scheme are packaged by adopting a composite aluminum film.
The preparation method of the drynaria rhizome formula particles comprises the following steps: soaking rhizoma Drynariae decoction pieces in water, reflux extracting, filtering, concentrating, adding adjuvant A, mixing, spray drying to obtain dry extract powder, adding adjuvant B, and dry granulating to obtain rhizoma Drynariae granule.
Further, in the technical scheme, the water adding amount for soaking is 3-12 times, and the soaking time is not less than 30 minutes.
Further, in the above technical solution, the reflux extraction time is not less than 30 minutes, and the extraction times are not less than 2 times.
Further, in the above technical solution, the mesh number of the filter screen is not less than 300 mesh during the filtering.
Further, in the technical scheme, the concentration is vacuum concentration, the heating temperature is not higher than 65 ℃, the vacuum degree is more than or equal to-0.08 mpa, and the concentration is carried out until the relative density is 1.15-1.20.
Further, in the above technical scheme, the auxiliary materials a and B are both selected from corn starch, dextrin or maltodextrin.
Further, in the technical scheme, the auxiliary material A is selected from maltodextrin, and the dosage of the auxiliary material is 14-15%; the auxiliary material B is selected from dextrin.
Further, in the technical scheme, the air inlet temperature of the spray drying is 135-180 ℃, and the optimal temperature is 140-150 ℃.
Further, in the above technical scheme, the drynaria rhizome formula particles are packaged by adopting a composite aluminum film.
Detailed Description
In the preparation process of the formula granule, the following national standard of medicines is referred to: [1] the general rule 2201 for measuring extract of the Chinese pharmacopoeia, the 2020 edition (one part) [ S ]. Beijing: chinese medical science and technology press 2020:267 ] [2] the national pharmacopoeia, the 2020 edition (four parts) general rule 2201 for measuring extract of the Chinese pharmacopoeia [ S ]. Beijing: chinese medical science and technology press 2020:232 ] [3] the national pharmacopoeia committee, the 9103 guidelines for moisture-induced test of the medicine [ S ]. Beijing: chinese medical science and technology press 2020:485 ] [4] the national pharmacopoeia, the 2020 edition (four parts) general rule 0982 for measuring particle size and particle size distribution [ S ]. Beijing: chinese medical science and technology press 2020:145 ] [5] the national pharmacopoeia, the 4 parts (four parts) general rule 0923 for measuring the degree of friability of tablets, the Chinese medical science and technology press [ S ]. The liquid medicine, and the liquid medicine, are carried out by the national medical science and technology press [ S ]. 2020:131 ] [6] YBZ-20210538-Qigold national medical science and technology press [ GmbH.7-5 GB 7.: fluidity index measurement [ S ].
Example 1 comprehensive investigation of extraction methods
1.1 soaking time investigation
1.1.1 Instrument and reagent
Instrument: JJ1000 electronic balance, TC20K-H electronic balance, sartorius SQP one ten thousandth balance, round bottom flask, electric mantle, etc.
Reagent:rhizoma DrynariaeDecoction pieces (lot number: 200901, 2011001, 2102001), drinking water, purified water.
1.1.2 Experimental method
Taking different lot numbersRhizoma Drynariae100g decoction pieces, recording the volumes of three batch decoction pieces in a three-part beaker, calculating bulk density, transferring to the beaker, and adding each of the materials into the beaker9Soaking in water for 15, 30, 45, and 60 min, sampling, inspecting, breaking off decoction pieces, observing whether moistening thoroughly, apparent wetting percentage, recording, and comprehensively evaluating soaking time before extraction according to wetting effect.
1.1.3 experimental results and analysis results are shown in Table 1:
table 1 soaking time wet percentage results
As a result, the reciprocal bulk density was about 2.8, the amount of water added was 4 to 7 times, and after soaking for 30 minutes, the wetting percentage was > 75%, which was the majority of wetting, thus determining the soaking time to be 30 minutes.
1.2 solid-liquid separation investigation
1.2.1 Instrument and reagent
Instrument: JJ1000 electronic balance, TC20K-H electronic balance, sartorius SQP one ten thousandth balance, round bottom flask, electric mantle, etc.
Reagent:rhizoma DrynariaeDecoction pieces (lot number: 200901, 2011001, 2102001), drinking water, purified water.
1.2.2 Experimental method
Soaking the sample for 60 minutes under the investigation item of the soaking time, extracting under reflux for 1.5 hours, filtering with a 100-mesh sieve while the sample is hot, recording the water absorption rate of decoction pieces, dividing the filtrate into 4 parts, and reserving the first part of filtrate for later use; the second part is filtered by a 150-mesh screen, and the filtrate is reserved; filtering with 200 mesh filter screen for use; a fourth 300-mesh filter screen is used for filtering, and filtrate is reserved; 4 parts of filtrate are filtered according to different amounts and meshes, and checked according to clarity.
1.2.3 experimental results and analysis results are shown in Table 2:
TABLE 2 clarity of different mesh filtration
As shown by the results, the filtering of 300 meshes or more can effectively filter most decoction piece fragments, so that the clarity of the finished product is better. Therefore, the solid-liquid separation filter screen is 300 meshes.
1.3 investigation of the number of extractions
The preparation is a traditional Chinese medicine formula granule, all parameters need to be standard by taking traditional decoction, the decoction times are taken along, the decoction is carried out for 2 times, and in order to avoid incomplete extraction and incomplete transfer of active ingredients, the 1 st to 2 rd extraction and the 3 rd extraction are independently examined, and the main examination indexes are the dry paste yield and the index component content.
1.3.1 instruments and reagents
Instrument: JJ1000 electronic balance, TC20K-H electronic balance, sartorius SQP one ten thousandth balance, round bottom flask, electric mantle, etc.
Reagent:rhizoma DrynariaeDecoction pieces (lot number: 2011001), drinking water, purified water.
1.3.2 Experimental methods
Taking different lot numbersRhizoma DrynariaeDecoction pieces 100g, add9Soaking the decoction pieces respectively30Minute, heat extraction1For hours, filter, add6Extracting with water1For hours, filtering and combining the filtrates, and labeling for later use. Adding again6Extracting with water1And (3) independently labeling for later use, sampling 2 groups of water extract, measuring the yield of the dry paste, and freeze-drying the rest part to obtain the content of the dry paste for inspection.
1.3.3 experimental results and analysis
Pretreatment was performed experimentally, and the results are shown in Table 3.
TABLE 3 results of extraction times experiment
Analysis of results: the national standard requirement of the drynaria prescription granule is that the dry paste yield is as follows8- 12.5%From the results, the 1 st to 2 nd resultsIs thatMeets the requirements, add the third time resultAlso is provided withMeets the requirements, but the 3 rd time is only 1 st to 2 nd time4.40From the content point of view, the requirements are12.0-30.0mg/6.5g decoction piecesFrom the results, it can be seen that the 1 st to 2 nd results meet the requirements, plus the 3 rd resultAlso is provided withMeets the requirements, but the 3 rd time is only 1 st to 2 nd time4.44In% and comprehensively consider, select and extract2And twice.
1.4 investigation of the Water addition quantity
1.4.1 instruments and reagents
Instrument: JJ1000 electronic balance, TC20K-H electronic balance, sartorius SQP one ten thousandth balance, liquid chromatograph, round bottom flask, electrothermal jacket, etc.
Reagent:rhizoma DrynariaeDecoction pieces (lot number:2011001) Drinking water, purified water, reagents are all analytically pure and chromatographically pure,
1.4.2 Experimental method
Taking outRhizoma Drynariae100g decoction pieces, three portions, respectively added6、9、12Double water, soak30Minute, heating and extracting for 1 hour, filtering, and adding3、6、9Extracting with water for 1 hr, filtering, and mixing filtrates. The 3 groups of water extract are sampled respectively to measure the dry paste yield, and the rest is freeze-dried to form dry paste to measure the content of index components.
1.4.3 experimental results and analysis
Pretreatment was performed according to the experimental method, and the results are shown in table 4:
TABLE 4 results of water addition experiments
Analysis of results:rhizoma DrynariaeThe national standard requirement of the prescription granule is that the dry paste yield is as follows from the dry paste yield8- 12.5 %From the results, add6The water doubling result meets the requirements, add9Water doubling resultAlso is provided withMeets the requirements, add12Water doubling resultAlso is provided withMeets the requirements and add9Double water ratio adding6Big water21.42Percent, add12Double water ratio adding9Big water0.25From the content point of view, the requirements are12.0-30.0. 30.0mg/6.5g decoction piecesFrom the results, add6The water doubling result meets the requirements, add9The water doubling result meets the requirements, add12Water doubling resultAlso is provided withMeets the requirements and add9Double water ratio adding6Big water34.92Percent, however, add12Double water ratio adding9The water is small0.95The water addition amount is selected as the percentage9Is multiplied by the water absorption capacity of the decoction pieces3Doubling, thus the 2 nd addition6Water doubling.
1.5 extraction time investigation
1.5.1 instruments and reagents
Instrument: JJ1000 electronic balance, TC20K-H electronic balance, sartorius SQP one ten thousandth balance, liquid chromatograph, round bottom flask, electrothermal jacket, etc.
Reagent:rhizoma DrynariaeDecoction pieces (lot number:2011001) Drinking water, purified water, reagents are all analytically pure and chromatographically pure,
1.5.2 Experimental methods
Taking outRhizoma DrynariaeDecoction pieces 100g, in triplicate, add9Soaking the decoction pieces in water30Minute, separately heating and extracting0.5、1、1.5For hours, filter, add6Doubling the water, corresponding extraction0.5、1、1.5For hours, the combined filtrates were filtered. The 3 groups of water extract are sampled respectively to measure the dry paste yield, and the rest is freeze-dried to form dry paste to measure the content of index components.
1.5.3 experimental results and analysis the pretreatment was performed experimentally, the results are shown in Table 5:
TABLE 5 extraction time experiment results
Analysis of results:rhizoma DrynariaeThe national standard requirement of the prescription granule is that the dry paste yield is as follows from the dry paste yield8- 12.5%From the results, it can be seen that the extraction0.5The hour results meet the requirements, and the extraction is carried out1The hour results meet the requirements, and the extraction is carried out1.5Hour resultsAlso is provided withMeets the requirements and extracts1Hourly ratio extraction0.5Hour size15.44% but extract1.5Hourly ratio extraction1Hour size0.08From the content point of view, the requirements are12.0-30.0. 30.0mg/6.5g decoction piecesFrom the results, it can be seen that the extraction0.5The hour results meet the requirements, and the extraction is carried out1The hour results meet the requirements, and the extraction is carried out1.5Hour resultsAlso is provided withMeets the requirements, extracts1Hourly ratio extraction0.5Hour size22.74% but extract1.5The hour is instead greater than the extraction1Hours1.16In% and comprehensively considering, the extraction time is selected as1Hours.
1.6 concentration method investigation
According to the concentration requirement in the quality control and standard formulation technical requirement of traditional Chinese medicine prescription granule, low-temperature concentration is adopted, the concentration temperature is lower than 65 ℃, the corresponding vacuum degree of 65 ℃ is-0.0761 Mpa according to the corresponding table of vacuum degree and water boiling point, therefore, the concentration vacuum degree is required to reach-0.0761 Mpa or below, the concentration vacuum degree is initially determined to be more than or equal to-0.08 Mpa, and the heating temperature is determined to be 65 ℃.
According to the requirements of standard decoction in quality control and standard formulation technical requirements of traditional Chinese medicine prescription granules, low-temperature drying is adopted, the mature drying mode is mainly spray drying, and the spray drying requirement on concentrated solution is mainly relative density, so that the concentration step mainly examines the concentration degree, and the relative density of the spray drying suitable liquid medicine is 1.10-1.15.
Thus, the concentration method is primarily defined as vacuum concentration, the heating temperature is 65 ℃, the vacuum degree is more than or equal to-0.08 Mpa, and the concentration is carried out until the relative density is 1.10-1.15.
1.6.1 instruments and reagents
Instrument: JJ1000 electronic balance, TC20K-H electronic balance, RE-6000A rotary evaporator, liquid chromatograph, round bottom flask, electrothermal jacket, etc.
Reagent:rhizoma DrynariaeDecoction pieces (lot number:2011001) Drinking water, purified water, reagents are all analytically pure and chromatographically pure,
1.6.2 Experimental methods
Taking outRhizoma DrynariaeDecoction pieces 100g, add9Soaking the decoction pieces in water30Minute, heating and extracting for 1 hour, filtering, and adding6Extracting with water for 1 hr, filtering, and mixing filtrates. Concentrating the filtrate under vacuum at 65deg.C until the vacuum degree reaches at least 0.08mpa and relative density is 1.10, collecting half of the sample, concentrating again, concentrating to relative density of 1.15, stopping concentrating, sampling 2 groups of concentrated solutions, measuring dry extract yield, and freeze drying the rest to obtain dry extract, and measuring index component content.
1.6.3 experimental results and analysis the pretreatment was performed experimentally, and the specific results are shown in Table 6.
TABLE 6 results of concentration level experiments
Analysis of results:rhizoma DrynariaeThe national standard requirement of the prescription granule is that the dry paste yield is as follows from the dry paste yield8- 12.5 %From the results, it was found that concentration was carried out1.15Concentrating to a specific concentration1.10Big size0.08From the content point of view, the requirements are12.0-30.0mg/ 6.5g decoction piecesFrom the results, it was found that concentration was carried out1.15Concentrating to a specific concentration1.10Small size0.11In% and at the same time, the fluid extract concentrated to 1.15 is still thinner, and can be concentrated to higher concentration, and the concentration is selected to have the relative density comprehensively considered1.15-1.20(60℃)。
1.7 spray drying investigation
1.7.1 inspection with auxiliary Material
1.7.1.1 instrument and reagent
Instrument: JJ1000 electronic balance, TC20K-H electronic balance, RE-6000A rotary evaporator, freeze dryer, spray dryer, round bottom flask, electric jacket, and the like.
Reagent:rhizoma DrynariaeDecoction pieces (lot number:2009001) Drinking water, purified water, reagents are all analytically pure and chromatographically pure,
1.7.1.2 experimental method
Taking the aboveFreeze-dried sample is ground into fine powder, a proper amount of fine powder is taken, precisely weighed, tiled in a clean weighing bottle, the thickness is less than or equal to 5mm, the total weight of the fine powder is precisely measured, four parts of dry paste powder are taken, and the maximum amount M of auxiliary materials is calculated Big size Adding different auxiliary materials (corn starch, dextrin and maltodextrin), uniformly mixing, spreading in a weighing bottle according to the above method, precisely weighing, placing five samples into a dryer (relative humidity 58%) filled with sulfuric acid solution (sulfuric acid 39.5mL and water 100 mL), standing for 0.25h, 0.5h, 1h, 1.5h, 2h, 3h, 4h, 6h, 8h, 10h and 24h, taking out, precisely weighing, calculating the moisture absorption of the samples, taking time as horizontal coordinate, taking moisture absorption percentage as vertical coordinate, and drawing a curve.
1.7.1.3 experimental results and analysis results are shown in the following table:
analysis of results: the result shows that the moisture absorption of the product is obvious when no auxiliary material is added, the moisture absorption reaches 6% when the equilibrium point is reached, the moisture absorption is obviously reduced after the auxiliary material is added, and the moisture absorption is 3% after the maltodextrin is added, so that the maltodextrin auxiliary material is selected to be added during spray drying.
1.7.2 investigation of adjuvant usage
According to the experimental selection, the auxiliary material addition drying is needed, the auxiliary material consumption inspection is needed, if the auxiliary material addition drying is not needed, the auxiliary material consumption inspection is not needed, and the specific auxiliary material consumption inspection is calculated as follows:
the maximum amount of auxiliary materials added during spraying is calculated by the percentage of particles: m is M Big size = (1-B x N) x100% = 18.75%, then 20% is taken.
N: the granule has standard specification, 1g granule is equivalent to N g decoction pieces, N =6.5g;
B: the dry extract has a maximum value of B, B=in the standard preparation method of the granule12.5%。
1.7.2.1 instrument and reagent
Instrument: JJ1000 electronic balance, TC20K-H electronic balance, RE-6000A rotary evaporator, freeze dryer, spray dryer, round bottom flask, electric jacket, and the like.
Reagent:rhizoma DrynariaeDecoction pieces (lot number:2009001) Drinking water, purified water, reagents are all analytically pure and chromatographically pure,
1.7.2.2 experimental method
Taking four parts of dry paste powder, adding the selected auxiliary materials according to the proportion of 0.1M Big size 、0.25 M Big size 、0.5 M Big size 、0.75 M Big size Integer M Big size Uniformly mixing, precisely weighing, spreading in a clean weighing bottle, wherein the thickness is less than or equal to 5mm, precisely weighing the total weight, and placing to an equilibrium time point of an upper experiment. And taking out, weighing, and calculating the percentage of moisture absorption.
1.7.2.3 experimental results and analysis results are shown in the following table:
the results were analyzed as follows: as shown by the results, as the auxiliary materials are increased, the moisture absorption is reduced after reaching the equilibrium point, and when the auxiliary materials are added15% of the total amount of the spray water reaches the optimal condition, so that the amount of the auxiliary materials added during the spray is15%。
1.7.3 spray drying parameter investigation
1.7.3.1 instruments and reagents
Instrument: JJ1000 electronic balance, TC20K-H electronic balance, RE-6000A rotary evaporator, spray dryer, round bottom flask, electric jacket, etc.
Reagent:rhizoma DrynariaeDecoction pieces (lot number:2009001) The drinking water, purified water and reagents are all analytically pure.
1.7.3.2 experimental method
Taking outRhizoma DrynariaeDecoction pieces300g, extracting2Extracting under heating for 1 hr, adding 1 st time9Soaking the medicinal materials in water30Minute, add times 2 and above6Double water, filtering, and combining filtrates. Concentrating the filtrate under vacuum at 65deg.C to a vacuum degree of not less than-0.08 mpa, concentrating to a relative density of 1.15-1.20 (60deg.C), adding adjuvantsMaltodextrin 7gMixing, spray drying, and collecting dry extractThe parameters are shown in the following table:
parameter table for spray drying
1.7.3.4 experimental results and analysis
The results statistics are shown in the following table:
results table of spray drying parameters
Analysis of results: the result shows that the spray dry paste powder at all temperatures reaches the dry loose fine powder, the dry paste yield is basically consistent, and the moisture reaches a lower value, so that the air inlet temperature of 135-180 ℃ is selected for spray drying, and the optimal temperature is 140-150 ℃.
1.8 study of the Forming method
Rhizoma DrynariaeThe prescription granule has the requirements of the preparation amount in the national standard or local standard, and 1g of the granule in the reference standard specification contains6.5g (N) decoction pieces, the yield of the dry paste of the decoction pieces is11.79The content of the auxiliary materials is%15And (B), combining the standard, and calculating the dosage of the auxiliary materials and the dry paste as follows:
the usage percentage of auxiliary materials is = {1- (N.A) } 100% -B=8.4%
Dry paste usage percentage= (n×a) ×100++b=91.6%
1.8.1 adjuvant and dose investigation
According to the national standard of the formula granule,rhizoma DrynariaeThe formula particle is6500The g decoction pieces are prepared into 1000g granules, so the dosage of the auxiliary materials is determined, and each gram of granules is prepared by adding the auxiliary materials into dry paste powder6.5G decoction pieces.
At present, the auxiliary materials of the granule and the auxiliary materials of the existing formula granule are mainly corn starch, dextrin and maltodextrin. Therefore, the three auxiliary materials were examined, and the dry granulation was performed, and the formability was used as an index after granulation.
1.8.1.1 instrument and reagent
Instrument: JJ1000 electronic balance, TC20K-H electronic balance, RE-6000A rotary evaporator, freeze dryer, round bottom flask, electric jacket, etc.
Reagent:rhizoma DrynariaeDecoction pieces (lot number:2009001) Corn starch, dextrin, maltodextrin, drinking water, purified water
1.8.1.2 experimental method
Taking a proper amount of dry paste powder and the screened corrective, uniformly mixing the materials according to the auxiliary materials in table 10, granulating by a dry method, and observing the formability (including granule dissolubility, granule hygroscopicity, granule granularity, granule friability, granule fluidity and the like).
1.8.1.3 experimental results and analysis
Pretreating according to an experimental method to obtain dry paste powder, adding different auxiliary materials according to screening results to prepare granules, detecting the formability of the granules, and granulating the granules, wherein the granulating results are shown in Table 10:
table 10 results of screening auxiliary materials for granulation
Remarks: hygroscopicity is expressed as percent dilution; fluidity is expressed in terms of angle of repose;
results analysis discussion: from the above results, the dry paste, after adding the dextrin auxiliary materials, meets the standard requirements in terms of appearance, granularity, friability and solubility, and the hygroscopicity and fluidity reach above requirements, so the auxiliary materials are selected as follows: and (3) dextrin.
1.9 inspection of packaging Material
And packaging by adopting a composite aluminum film. The composite aluminum film is a conventional packaging material of granules, is also a packaging material of the existing formula granule manufacturer, and has mature packaging method and high industrial mass production efficiency. The package has good sealing performance and moisture resistance, can effectively block the influence of light, heat, water vapor, oxygen and the like on medicines, and is convenient to carry and use.
Example 2
Instrument and reagent
Instrument: JJ1000 electronic balance, TC20K-H electronic balance, RE-6000A rotary evaporator, spray dryer, round bottom flask, electric jacket, etc.
Reagent:rhizoma DrynariaeDecoction pieces (lot number: 200901, 2011001, 2102001), corn starch, dextrin, maltodextrin, drinking water, purified water.
Experimental method
Taking outRhizoma DrynariaeDecoction pieces325g, soaking in water30Minute, reflux extraction2Twice, each time1For an hour, add for the first time9Doubling the water yield, adding for the second time6Multiple water amount, filtering, mixing filtrates, concentrating under reduced pressure (temperature 65deg.C, vacuum degree not less than-0.08 mpa), concentrating to relative density 1.15-1.20 (60deg.C), sampling (total sample 1/10), detecting dry extract yield, adding maltodextrin 6.75g, mixing, spray drying to obtain dry extract powder, and addingDextrinMixing, granulating by dry method, and making into 45g rhizoma Drynariae granule. And (5) inspecting the content and the characteristic map.
Experimental results and analysis
Pretreatment is carried out according to an experimental method, particles are prepared, and the characteristic spectrum and naringin content of the particles are detected, and the results are shown in Table 11:
table 11 small test evidence verification data
Analysis of results: according to 3 batches of decoction piece experiments, the rhizoma drynariae formula particles have stable yield data and controllable quality in each working procedure, and the method is proved to be satisfactory.
Example 3 pilot test method validation
Taking outRhizoma DrynariaeDecoction pieces6500g, soaking in water30Minute, reflux extraction2Twice, each time1Hour, 1 st addition9Doubling the water yield, add 2 nd time6Double water amount, filtering, mixing filtrates, concentrating under reduced pressure (temperature 65deg.C, vacuum degree not less than-0.08 mpa), concentrating to relative density 1.15-1.20 (60deg.C), adding 10g maltodextrin, mixing, spray drying to obtain dry extract powder, addingDextrinMixing, granulating by dry method, and making 1000g rhizoma Drynariae granule.
Example 4 evaluation index
1.1.1 yield of dry extract
The detection method comprises the following steps: taking a proper amount of medicine liquid, accurately weighing, placing in a dried clean evaporating dish, evaporating in water bath, drying at 105 ℃ for more than 3 hours, taking out, placing in a dryer for cooling for 30 minutes, rapidly taking out, weighing, and calculating.
1.1.2 titration of content
The detection method comprises the following steps: according to high performance liquid chromatography (rule 0512 of Chinese pharmacopoeia 2020 edition).
Chromatographic conditions and system applicability octadecylsilane chemically bonded silica was used as a filler (column length of 100mm, inner diameter of 2.1mm, particle size of 1.9 μm); methanol-acetic acid-water (35:4:65) is used as mobile phase; the flow rate was 0.3mL per minute; the detection wavelength was 283nm. The theoretical plate number should be not less than 3000 calculated according to naringin peak.
Preparing a control solution, namely taking a proper amount of naringin control, precisely weighing, and adding methanol to prepare a solution with the volume of 70 mu g per 1 mL.
The preparation of the test sample solution comprises taking a proper amount of the sample, grinding, taking about 1.3g of decoction pieces of the test sample, precisely weighing, placing in a conical bottle with a plug, precisely adding 50mL of 50% methanol, sealing, weighing, performing ultrasonic treatment (power is 250W and frequency is 40 kHz) for 30 minutes, cooling, weighing again, supplementing the weight loss with 50% methanol, shaking uniformly, filtering, and taking the subsequent filtrate.
The measurement method comprises precisely sucking 1 μl of each of the reference solution and the sample solution, and injecting into a liquid chromatograph for measurement.
1.1.3 characteristic Spectrum
The detection method comprises the following steps: according to high performance liquid chromatography (rule 0512 of Chinese pharmacopoeia 2020 edition).
Chromatographic conditions and system applicability octadecylsilane chemically bonded silica is used as a filler; methanol is taken as a mobile phase A, 0.1% phosphoric acid solution is taken as a mobile phase B, and gradient elution is carried out according to the specifications in the following table; the flow rate is 1mL per minute; the column temperature is 30 ℃; the detection wavelength was 283nm. The theoretical plate number should be not less than 3000 calculated according to naringin peak.
Preparation of reference solution the reference solution of rhizoma Drynariae was prepared by taking 0.5g of reference material, placing in a conical flask with a plug, adding 25mL of 50% methanol, performing ultrasonic treatment (power 250W, frequency 40 kHz) for 40 min, cooling, shaking, filtering, and collecting the subsequent filtrate as reference solution of reference material. And (3) taking a proper amount of naringin reference substance, precisely weighing, and adding methanol to prepare a solution with 60 mug per lmL serving as a reference substance solution of the reference substance.
The test solutions were prepared as described above (content titration).
And respectively precisely sucking the reference object solution and the sample solution by using a measuring method, respectively 10 mu L, injecting into a liquid chromatograph, and measuring to obtain the sample solution.
The sample chromatogram should show 4 characteristic peaks, and should correspond to 4 characteristic peaks in the reference chromatogram of the reference material, wherein the peak 4 retention time should correspond to the naringin reference peak retention time. The peak corresponding to naringin reference is S peak, and the relative retention time of each characteristic peak and S peak is calculated, wherein the relative retention time is within + -10% of the specified value. The specified value is: 0.44 (Peak 1), 0.45 (Peak 2), 0.89 (Peak 3).
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should be covered by the protection scope of the present invention by making equivalents and modifications to the technical solution and the inventive concept thereof.
Claims (9)
1. The preparation method of the drynaria rhizome formula particles is characterized by comprising the following steps: soaking rhizoma Drynariae decoction pieces in water, reflux extracting, filtering, concentrating, adding adjuvant A, mixing, spray drying to obtain dry extract powder, adding adjuvant B, and dry granulating to obtain rhizoma Drynariae granule.
2. The method for preparing drynaria rhizome formulation particles according to claim 1, wherein the method comprises the following steps: the water adding amount for soaking is 3-12 times, and the soaking time is not less than 30 minutes.
3. The method for preparing drynaria rhizome formulation particles according to claim 1, wherein the method comprises the following steps: the reflux extraction time is not less than 30 minutes, and the extraction times are not less than 2 times.
4. The method for preparing drynaria rhizome formulation particles according to claim 1, wherein the method comprises the following steps: and during filtering, the mesh number of the filter screen is not less than 300 meshes.
5. The method for preparing drynaria rhizome formulation particles according to claim 1, wherein the method comprises the following steps: the concentration is vacuum concentration, the heating temperature is not higher than 65 ℃, the vacuum degree is not less than-0.08 mpa, and the concentration is carried out until the relative density is 1.15-1.20.
6. The method for preparing drynaria rhizome formulation particles according to claim 1, wherein the method comprises the following steps: the auxiliary materials A and B are selected from corn starch, dextrin or maltodextrin.
7. The method for preparing drynaria rhizome formulation particles according to claim 6, wherein the method comprises the following steps: the auxiliary material A is selected from maltodextrin, and the dosage of the auxiliary material is 14-15%; the auxiliary material B is selected from dextrin.
8. The method for preparing drynaria rhizome formulation particles according to claim 1, wherein the method comprises the following steps: the air inlet temperature of the spray drying is 135-180 ℃.
9. The method for preparing drynaria rhizome formulation particles as claimed in any one of claims 1 to 8, wherein: the drynaria rhizome formula particles are packaged by adopting a composite aluminum film.
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CN103040879A (en) * | 2012-12-20 | 2013-04-17 | 苏州天南星生物科技有限公司 | Compound preparation of rhizoma drynariae |
CN106053658A (en) * | 2016-06-29 | 2016-10-26 | 四川新绿色药业科技发展股份有限公司 | Burned Rhizoma drynariae formula granule characteristic spectrum and establishing method thereof |
CN107456479A (en) * | 2017-08-02 | 2017-12-12 | 浙江大学 | A kind of preparation of psoralea corylifolia granule and detection method |
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