CN105769991A - Preparation method of motherwort herb granules - Google Patents

Preparation method of motherwort herb granules Download PDF

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CN105769991A
CN105769991A CN201610325097.2A CN201610325097A CN105769991A CN 105769991 A CN105769991 A CN 105769991A CN 201610325097 A CN201610325097 A CN 201610325097A CN 105769991 A CN105769991 A CN 105769991A
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preparation
yimucao
herba leonuri
extractum
drop
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高凯
戴初雄
庄太波
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Hangzhou Zhongbao Pharmaceutical Co Ltd
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Hangzhou Zhongbao Pharmaceutical Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/53Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
    • A61K36/533Leonurus (motherwort)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/14Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1605Excipients; Inactive ingredients
    • A61K9/1629Organic macromolecular compounds
    • A61K9/1652Polysaccharides, e.g. alginate, cellulose derivatives; Cyclodextrin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • 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
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization

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  • Natural Medicines & Medicinal Plants (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Chemical & Material Sciences (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Alternative & Traditional Medicine (AREA)
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  • Medicines Containing Plant Substances (AREA)

Abstract

The invention discloses a preparation method of motherwort herb granules. The preparation method comprises the following steps: (1) dynamic extraction: taking minced motherwort herb, adding an appropriate amount of water, and performing dynamic extraction at 95+/-3 DEG C to obtain dregs and an extract; (2) centrifugal separation: performing centrifugal separation on the extract to obtain clarified liquid; (3) vacuum concentration: performing vacuum concentration on the clarified liquid to obtain a motherwort herb extractum; (4) first screening: heating the motherwort herb extractum until boiling, and then screening the heated motherwort herb extractum through a sieve; (5) spray drying: performing spray drying to prepare motherwort herb dry extract powder; (6) granulation: proportioning the motherwort herb dry extract powder and auxiliary materials, mixing uniformly, and granulating; and (7) second screening: performing second screening to collecting qualified granules. By adopting the preparation method disclosed by the invention, the motherwort herb granules, which are high in active ingredient content, cannot absorb moisture easily, and are stable in performance and high in rate of finished products, can be obtained.

Description

A kind of preparation method of yimucao drop preparation
Technical field
The invention belongs to Chinese drug preparation field, the preparation method particularly relating to a kind of yimucao drop preparation.
Background technology
Herba Leonuri, have another name called for, motherwort, Herba Leonuri, nine Rhizoma Paridis, the careless and gloomy base of a fruit of Muscovitum, for Labiatae, mother wort plant, summer-flowering.Its dry aerial parts are conventional Chinese medicine, and most of China area is all produced, and give birth to or endure cream and use.1 year or biennial herb whole nation most area all have distribution, are born in hill wasteland, ridge, meadow etc..Plucking when the non-standard-sized sheet of riotous growth flower in summer, acrid in the mouth is bitter, cool, invigorates blood circulation, silts of dispelling, regulating menstruation, disappear water, treats menoxenia, vaginal bleeding during pregnancy difficult labour, retention of placenta, puerperal blood faints, abdominal pain due to blood stasis, metrorrhagia and metrostaxis, hematuria, rushes down blood, carbuncle skin infection.Herba Leonuri has inducing diuresis to remove edema, shrinks the effect of uterus effect, is that ancient Chinese medicine doctor is for treating gynopathic key medicine.Herba Leonuri can all herbal medicine, effective ingredient be Herba Leonuri element, Herba Leonuri is containing multiple alkaloid and benzoic acid, potassium chloride etc. such as leonurine, stachydrine, leonuridine, leonurinines.
Chinese medicine granules is the extract by medicine in prescription or some drugs, mixes with suitable quantitative adjuvant, makes the uniform granule of content through special process.By its dissolubility in water, it is divided into sol particle and suspension ability granule and effervescent granule.This dosage form because carrying, taking convenience, become a kind of solid preparation of Chinese medicine that developed recently is the fastest.But the yimucao drop preparation water content of currently available technology is high, it is easy to moisture absorption is lumpd, and unstable properties, the shelf-life is short;And the extraction efficiency of preparation technology is low, extracts active ingredients is insufficient, and yield rate is low.
Summary of the invention
Reflect with this, the preparation method that it is an object of the invention to provide a kind of yimucao drop preparation, adopt preparation method of the present invention can obtain the yimucao drop preparation that active constituent content height, not easily moisture absorption, stable performance and yield rate are high.
To achieve the above object, the technical scheme is that and be achieved in that:
The preparation method of a kind of yimucao drop preparation, comprises the following steps: (1) dynamic extraction: take the Herba Leonuri of chopping, adds water appropriate, in 95 ± 3 DEG C of dynamic extraction, obtains medicinal residues and extracting solution;(2) centrifugation: be centrifuged extracting solution separating, it is thus achieved that clear liquor;(3) concentrating under reduced pressure: clear liquor is carried out concentrating under reduced pressure, it is thus achieved that Herba Leonuri extractum;(4) first time sieves: heating Herba Leonuri extractum is to seething with excitement after sieved filter;(5) spray drying: prepare Herba Leonuri dried cream powder;(6) granulate: Herba Leonuri dried cream powder and adjuvant are carried out dispensing, mixing, granulate;(7) second time is sieved: collect conforming particle.It is dry that the present invention adopts the processing step of dynamic extraction mode, centrifugation, concentrating under reduced pressure and spray drying that Herba Leonuri carries out extraction, preferably, Extracting temperature in described step (1) is 95 ± 3 DEG C, contribute to the dissolution of effective ingredient, reduce the loss of effective ingredient, and farthest reclaim the effective ingredient of Herba Leonuri;Before spray drying treatment, to the extractum heating after concentration to boiling after sieved filter, it is remarkably improved the moisture-proof of dried Herba Leonuri granule, is less susceptible to moisture absorption in the environment, effectively extend the storage life of Herba Leonuri granule, improve the stability of Herba Leonuri granule.
Preferably, in described step (1) dynamic extraction process: first add the hot water of 80 ± 5 DEG C toward extraction pot, add the Herba Leonuri of chopping, affiliated hot water weight is 2~4 times of Herba Leonuri, the hot water that continuation is supplementary 80 ± 5 DEG C is to 9~11 times of Herba Leonuri weight, heating makes water temperature rise to 95 ± 3 DEG C, carries out dynamic extraction, obtains medicinal residues and extracting solution after extraction.This operating procedure heats up after being added in two steps by hot water and supplying water again, and the dynamic extraction mode under this condition can remain the active component of medicine to greatest extent so that extract more fully, more thorough.
Preferably, described step (2) centrifugal separation processes includes: (a) uses centrifuge that the extracting solution that step (1) obtains is carried out solid-liquid separation, and extracting solution temperature is 95 ± 3 DEG C, and centrifuge speed is 1000~5000 revs/min;B () uses supercentrifuge that the medicinal liquid after step (a) separation is carried out ultracentrifugation, fluid temperature is 80~95 DEG C, and supercentrifuge rotating speed is 1.3~1.5 ten thousand revs/min.Described step (2) centrifugal separation processes can effectively remove impurity by low-speed centrifugal pre-separation, is separated the content that can improve effective ingredient further by ultracentrifugation, and separating medium is more clarified.
Preferably, in described step (3) concentrating under reduced pressure process: clear liquor enters concentration tank by negative pressure, feed liquor speed is 600~1000L/h, and vacuum is-0.06~-0.1MPa, and temperature is 50~60 DEG C, circulating water temperature 30~40 DEG C.The relative density having concentrated rear gained Herba Leonuri extractum 50~60 DEG C is 1.05~1.1.The relative density of medicinal liquid is very big on the impact of drying process with atomizing, and the concentration condition of this programme and relative density ensure that the efficiency of spray drying, it is thus achieved that single-size.
Preferably, described step (4) first time sieves in process: is placed in jacketed pan by the extractum that step (3) obtains, stirs, and heating, to boiling, uses 200~400 mesh sieves to be filtered.Heating is adopted to be possible not only to remove impurity that is remaining or that be reintroduced back to further to boiling after the mode that sieve processes, and the moisture-proof of Herba Leonuri granule after significantly improving spray drying, extend the storage life of Herba Leonuri granule, improve the stability of Herba Leonuri granule.
Preferably, in described step (5) spray-drying process: the concentrated solution filtered is thrown into and treats in Liquid spray reservoir, 75~85 DEG C of stirring insulations, by nebulizer feed liquor spray drying, prepare Herba Leonuri dried cream powder.The dried cream powder moisture content prepared is low, and granule is uniform.
Preferably, in described step (6) pelletization: being put in Drygranulatemachine by the material of mix homogeneously and granulate, Drygranulatemachine sets roller pressure as 90~110kg/cm2, side seal pressure be 25~50kg/cm2.Drygranulatemachine utilizes the water of crystallization in material, directly powder is made granule, does not destroy the chemical property of material, does not reduce the effective content of product; whole process is closed, and free from admixture flows into, and product purity is high; and product environmentally safe, prepared granule is completely smooth, and matter is hard.
Preferably, described step (7) second time is sieved in process: the granule that step (6) prepares is crossed shaking screen, and shaking screen screen cloth specification is upper 12 orders and lower 40 orders, is collected by 12 orders and does not pass through the granule of 40 mesh sieve gained.
Preferably, in described step (6) pelletization, described adjuvant includes dextrin, maltodextrin and steviosin, calculating by weight, described dispensing includes Herba Leonuri dried cream powder 100~130 weight portion, dextrin 70~90 weight portion, maltodextrin 20~30 weight portion and steviosin 0.4~1 weight portion.Without adding other additives, gained finished product active constituent content is high, and stable performance.
Compared with prior art, the invention have the benefit that
95 ± 3 DEG C of high temperature dynamic extraction modes in preparation method of the present invention can remain the active component of medicine to greatest extent so that extract more fully, more thorough;Can significantly remove impurity by the method for the low speed centrifugal centrifugation again that exceeds the speed limit in advance, improve the content of effective ingredient further;Before carrying out spray drying, Herba Leonuri extractum is heated to boiling then the filtration treatment that carries out sieving, and is possible not only to remove further impurity, improves active constituent content, and can improve the moisture-proof of prepared Herba Leonuri granule;The each step of preparation method of the present invention complements each other, it is not necessary to add the additive of other special efficacies, and gained finished product active constituent content is high, and stable performance and yield rate are high, long shelf-life.
Detailed description of the invention
For the technical scheme in the present invention is clearly and completely described, it is clear that inventor illustrates in conjunction with the embodiments, but the only a part of embodiment of the present invention described by following example, rather than whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under not making creative work premise, broadly fall into the scope of protection of the invention.
Embodiment 1
The preparation method of a kind of yimucao drop preparation, comprises the following steps:
(1) dynamic extraction:
First the hot water of 80 DEG C is added toward extraction pot, add the Herba Leonuri of chopping, affiliated hot water weight is 3 times of Herba Leonuri, the hot water that continuation is supplementary 80 DEG C is to 10 times of Herba Leonuri weight, heating makes water temperature rise to 98 DEG C, adopting multi-functional dynamic extraction agitator tank to carry out dynamic extraction, Extracting temperature is maintained at 98 DEG C, obtains medicinal residues and extracting solution after extraction.
(2) centrifugation:
A () uses centrifuge that the extracting solution that step (1) obtains is carried out solid-liquid separation, extracting solution temperature is 98 DEG C, and centrifuge speed is 3000 revs/min;
B () uses supercentrifuge that the medicinal liquid after step (a) separation is carried out ultracentrifugation, fluid temperature is 95 DEG C, and supercentrifuge rotating speed is 1.5 ten thousand revs/min, it is thus achieved that clear liquor.
(3) concentrating under reduced pressure:
By negative pressure, clear liquor is entered concentration tank, and feed liquor speed is 800L/h, and vacuum is-0.08MPa, and temperature is 60 DEG C, circulating water temperature 35 DEG C, it is thus achieved that Herba Leonuri extractum.The relative density having concentrated rear gained Herba Leonuri extractum 60 DEG C is 1.05~1.1.
(4) first time sieves:
Being placed in jacketed pan by the extractum that step (3) obtains, stir, heating, to boiling, uses 200 mesh sieves to be filtered, and removes the medicinal residues not passing through sieve.
(5) spray drying:
The concentrated solution filtered is thrown into be treated in Liquid spray reservoir, and 85 DEG C of stirring insulations, by nebulizer feed liquor spray drying, inlet temperature is 180 DEG C, and leaving air temp 100 DEG C is collected normal powder and whirlwind powder and sweeps powder, obtaining Herba Leonuri dried cream powder.
(6) granulate:
Herba Leonuri dried cream powder and adjuvant are carried out dispensing, described adjuvant includes dextrin, maltodextrin and steviosin, calculating by weight, described dispensing includes Herba Leonuri dried cream powder 100 weight portion, dextrin 70 weight portion, maltodextrin 20 weight portion and steviosin 0.4 weight portion.Dispensing being mixed, put in Drygranulatemachine by the material of mix homogeneously and granulate, Drygranulatemachine sets roller pressure as 100kg/cm2, side seal pressure be 40kg/cm2, prepare yimucao drop preparation.
(7) second time is sieved:
The granule that step (6) prepares is crossed shaking screen, and shaking screen screen cloth specification is upper 12 orders and lower 40 orders, is collected by 12 orders and does not pass through the granule of 40 mesh sieve gained, i.e. conforming particle.
Embodiment 2
The preparation method of a kind of yimucao drop preparation, comprises the following steps:
(1) dynamic extraction:
First the hot water of 75 DEG C is added toward extraction pot, add the Herba Leonuri of chopping, affiliated hot water weight is 2 times of Herba Leonuri, the hot water that continuation is supplementary 75 DEG C is to 9 times of Herba Leonuri weight, heating makes water temperature rise to 92 DEG C, adopting multi-functional dynamic extraction agitator tank to carry out dynamic extraction, Extracting temperature is maintained at 92 DEG C, obtains medicinal residues and extracting solution after extraction.
(2) centrifugation:
A () uses centrifuge that the extracting solution that step (1) obtains is carried out solid-liquid separation, extracting solution temperature is 92 DEG C, and centrifuge speed is 1000 revs/min;
B () uses supercentrifuge that the medicinal liquid after step (a) separation is carried out ultracentrifugation, fluid temperature is 80 DEG C, and supercentrifuge rotating speed is 1.3 ten thousand revs/min, it is thus achieved that clear liquor.
(3) concentrating under reduced pressure:
By negative pressure, clear liquor is entered concentration tank, and feed liquor speed is 600L/h, and vacuum is-0.06MPa, and temperature is 50 DEG C, circulating water temperature 30 DEG C, it is thus achieved that Herba Leonuri extractum.The relative density having concentrated rear gained Herba Leonuri extractum 50 DEG C is 1.05~1.1.
(4) first time sieves:
Being placed in jacketed pan by the extractum that step (3) obtains, stir, heating, to boiling, uses 300 mesh sieves to be filtered, and removes the medicinal residues not passing through sieve.
(5) spray drying:
The concentrated solution filtered is thrown into be treated in Liquid spray reservoir, and 75 DEG C of stirring insulations, by nebulizer feed liquor spray drying, inlet temperature is 170 DEG C, and leaving air temp 95 DEG C is collected normal powder and whirlwind powder and sweeps powder, obtaining Herba Leonuri dried cream powder.
(6) granulate:
Herba Leonuri dried cream powder and adjuvant are carried out dispensing, described adjuvant includes dextrin, maltodextrin and steviosin, calculating by weight, described dispensing includes Herba Leonuri dried cream powder 115 weight portion, dextrin 80 weight portion, maltodextrin 25 weight portion and steviosin 0.8 weight portion.Dispensing being mixed, put in Drygranulatemachine by the material of mix homogeneously and granulate, Drygranulatemachine sets roller pressure as 90kg/cm2, side seal pressure be 50kg/cm2, prepare yimucao drop preparation.
(7) second time is sieved:
The granule that step (6) prepares is crossed shaking screen, and shaking screen screen cloth specification is upper 12 orders and lower 40 orders, is collected by 12 orders and does not pass through the granule of 40 mesh sieve gained, i.e. conforming particle.
Embodiment 3
The preparation method of a kind of yimucao drop preparation, comprises the following steps:
(1) dynamic extraction:
First the hot water of 85 DEG C is added toward extraction pot, add the Herba Leonuri of chopping, affiliated hot water weight is 4 times of Herba Leonuri, the hot water that continuation is supplementary 85 DEG C is to 11 times of Herba Leonuri weight, heating makes water temperature rise to 95 DEG C, adopting multi-functional dynamic extraction agitator tank to carry out dynamic extraction, Extracting temperature is maintained at 95 DEG C, obtains medicinal residues and extracting solution after extraction.
(2) centrifugation:
A () uses centrifuge that the extracting solution that step (1) obtains is carried out solid-liquid separation, extracting solution temperature is 95 DEG C, and centrifuge speed is 5000 revs/min;
B () uses supercentrifuge that the medicinal liquid after step (a) separation is carried out ultracentrifugation, fluid temperature is 85 DEG C, and supercentrifuge rotating speed is 1.4 ten thousand revs/min, it is thus achieved that clear liquor.
(3) concentrating under reduced pressure:
By negative pressure, clear liquor is entered concentration tank, and feed liquor speed is 1000L/h, and vacuum is-0.1MPa, and temperature is 60 DEG C, circulating water temperature 40 DEG C, it is thus achieved that Herba Leonuri extractum.The relative density having concentrated rear gained Herba Leonuri extractum 60 DEG C is 1.05~1.1.
(4) first time sieves:
Being placed in jacketed pan by the extractum that step (3) obtains, stir, heating, to boiling, uses 400 mesh sieves to be filtered, and removes the medicinal residues not passing through sieve.
(5) spray drying:
The concentrated solution filtered is thrown into be treated in Liquid spray reservoir, and 80 DEG C of stirring insulations, by nebulizer feed liquor spray drying, inlet temperature is 175 DEG C, and leaving air temp 105 DEG C is collected normal powder and whirlwind powder and sweeps powder, obtaining Herba Leonuri dried cream powder.
(6) granulate:
Herba Leonuri dried cream powder and adjuvant are carried out dispensing, and described adjuvant includes dextrin, maltodextrin and steviosin, calculates by weight, and described dispensing includes Herba Leonuri dried cream powder 130 weight portion, dextrin 90 weight portion, maltodextrin 30 weight portion and steviosin 1 weight portion.Dispensing being mixed, put in Drygranulatemachine by the material of mix homogeneously and granulate, Drygranulatemachine sets roller pressure as 110kg/cm2, side seal pressure be 25kg/cm2, prepare yimucao drop preparation.
(7) second time is sieved:
The granule that step (6) prepares is crossed shaking screen, and shaking screen screen cloth specification is upper 12 orders and lower 40 orders, is collected by 12 orders and does not pass through the granule of 40 mesh sieve gained, i.e. conforming particle.
Embodiment 4
With embodiment 1, the preparation method of a kind of yimucao drop preparation in the present embodiment, is distinctive in that step (1) dynamic extraction comprises the following steps:
First the hot water of 50 DEG C is added toward extraction pot, add the Herba Leonuri of chopping, affiliated hot water weight is 3 times of Herba Leonuri, the hot water that continuation is supplementary 50 DEG C is to 10 times of Herba Leonuri weight, heating makes water temperature rise to 60 DEG C, adopting multi-functional dynamic extraction agitator tank to carry out dynamic extraction, Extracting temperature is maintained at 60 DEG C, obtains medicinal residues and extracting solution after extraction.
Step (2) centrifugation comprises the following steps:
A () uses centrifuge that the extracting solution that step (1) obtains is carried out solid-liquid separation, extracting solution temperature is 58 ± 2 DEG C, and centrifuge speed is 3000 revs/min;
B () uses supercentrifuge that the medicinal liquid after step (a) separation is carried out ultracentrifugation, fluid temperature is 56 ± 2 DEG C, and supercentrifuge rotating speed is 1.5 ten thousand revs/min, it is thus achieved that clear liquor.
All the other steps are identical with embodiment 1, prepare yimucao drop preparation.
Embodiment 5
The preparation method of a kind of yimucao drop preparation in the present embodiment, is distinctive in that with embodiment 1, lacks step (2) centrifugation, and all the other steps are identical with embodiment 1, prepare yimucao drop preparation.
Embodiment 6
The preparation method of a kind of yimucao drop preparation in the present embodiment, is distinctive in that with embodiment 1, lacks step (a) low speed in step (2) centrifugation and separates, and all the other steps are identical with embodiment 1, prepare yimucao drop preparation.
Embodiment 7
The preparation method of a kind of yimucao drop preparation in the present embodiment, is distinctive in that with embodiment 1, and step (b) hypervelocity lacked in step (2) centrifugation separates, and all the other steps are identical with embodiment 1, prepare yimucao drop preparation.
Embodiment 8
The preparation method of a kind of yimucao drop preparation in the present embodiment, is distinctive in that with embodiment 1, lacks step (4) first time and sieves processs, and all the other steps are identical with embodiment 1, prepared yimucao drop preparation.
Embodiment 9
The preparation method of a kind of yimucao drop preparation in the present embodiment, is distinctive in that with embodiment 1, in the process that step (4) first time sieves:
The extractum that step (3) obtains is placed in jacketed pan, stirs, under normal temperature condition, use 200 mesh sieves to be filtered, remove the medicinal residues not passing through sieve.
All the other steps are identical with embodiment 1, prepare yimucao drop preparation.
Embodiment 10
The preparation method of a kind of yimucao drop preparation in the present embodiment, is distinctive in that with embodiment 1, in the process that step (4) first time sieves:
The extractum that step (3) obtains is placed in jacketed pan, stirs, under 60 DEG C of conditions, use 200 mesh sieves to be filtered, remove the medicinal residues not passing through sieve.
All the other steps are identical with embodiment 1, prepare yimucao drop preparation.
Performance detects:
Yimucao drop preparation obtained by embodiment 1 to embodiment 10 is carried out measurement of water-content coefficient, assay method is: be placed in the baking oven of 100 DEG C by the yimucao drop preparation obtained by embodiment 1 to embodiment 10, dry 24 hours, and calculate sample moisture content, moisture content (%)=(MBefore dry-MAfter drying)/MBefore dry× 100%.
The mensuration of the active constituent content of the yimucao drop preparation obtained by embodiment 1 to embodiment 10: with stachydrine hydrochloride (C7H13N〇2HC1) content meter.
Yimucao drop preparation obtained by embodiment 1 to embodiment 10 is carried out wettability test, test method is: be placed in the constant humidity incubator of 60% by the yimucao drop preparation obtained by embodiment 1 to embodiment 10, place 72 hours, and calculate sample hydroscopicity, hydroscopicity (%)=(MAfter moisture absorption-MBefore moisture absorption)/MBefore moisture absorption× 100%.
Yimucao drop preparation obtained by embodiment 1 to embodiment 10 is carried out stability test, test method is: ordinary packing, place 12 months when temperature 25 DEG C ± 2 DEG C, relative humidity 50% ± 10%, observe each embodiment respectively and obtain outward appearance and the character of sample.
The performance test data such as the moisture content of the yimucao drop preparation obtained by embodiment 1 to embodiment 10, active constituent content, hydroscopicity, stability are as shown in table 1:
Table 1
Embodiment 1 to 3 performance data shows that the yimucao drop preparation moisture content that the preparation method of yimucao drop preparation provided by the invention obtains is low, and active constituent content is high, and hydroscopicity is low, excellent stability.Especially, the temperature conditions of dynamic extraction, centrifugal treating, carry out spray drying before the processing step such as heated sieved filter the impact of moisture content, active constituent content, hydroscopicity and stability is very big, different centrifugal separation process processes and also has a certain impact, and embodiment 4 can be seen that low-temperature dynamic extracts the content substantially reducing effective ingredient;Embodiment 5 owing to being just made directly concentrating under reduced pressure not past step with centrifugal separation, and not only reducing active constituent content but also water content also substantially increases, additionally owing to high impurity content causes that resistance to moisture pick-up properties is decreased obviously;Embodiment 8 shows that the heated sieved filter before spray drying can significantly reduce moisture content, improve the resistance to hygroscopicity of dried granule and stability.Embodiment 1,9 and 10 shows that heating carries out filter effect the best of sieving to fluidized state, and resistance to hygroscopicity is the strongest.
With by 12 orders and do not pass through the granule gross weight of 40 mesh sieves account for do not sieve before the percentage ratio of granule gross weight represent the grain graininess uniformity of obtained yimucao drop preparation.Yield rate is calculated by (gross weight of conforming particle gross weight/account for dispensing) × 100% and obtains.In pelletization, do not meet the granule of size specification and repeat to granulate and carry out second time again and sieve collection granule.In embodiment 1 to embodiment 3 preparation method, the grain graininess uniformity and the yield rate of the yimucao drop preparation obtained by granulating through step (6) are as shown in table 2:
Table 2
Embodiment 1 Embodiment 2 Embodiment 3
Epigranular degree (%) 99.5% 98% 96%
Yield rate (%) 100% 99.5% 99.8%
The grain graininess of the yimucao drop preparation obtained by granulating through step (6) as can be seen from Table 2 is highly uniform, and the grain graininess uniformity >=96% substantially conforms to size specification.Yield rate >=99.5% of the preparation method of yimucao drop preparation provided by the invention, yield rate is high.
The stability of the yimucao drop preparation obtained by embodiment 1 to embodiment 3 is as shown in the table: test method: ordinary packing, place 24 months when temperature 25 DEG C ± 2 DEG C, relative humidity 50% ± 10%, the 12nd, 18,24, observe each embodiment respectively and obtain outward appearance and the character of sample 30 months the end of month, result is as shown in table 3:
Table 3
In sum, the preparation method of yimucao drop preparation provided by the invention, it is not necessary to add other functional additives, it is thus achieved that yimucao drop preparation not only performance is good and good stability, long shelf-life.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention.

Claims (10)

1. the preparation method of a yimucao drop preparation, it is characterised in that comprise the following steps: (1) dynamic extraction: take the Herba Leonuri of chopping, adds water appropriate, in 95 ± 3 DEG C of dynamic extraction, obtains medicinal residues and extracting solution;(2) centrifugation: be centrifuged extracting solution separating, it is thus achieved that clear liquor;(3) concentrating under reduced pressure: clear liquor is carried out concentrating under reduced pressure, it is thus achieved that Herba Leonuri extractum;(4) first time sieves: heating Herba Leonuri extractum is to seething with excitement after sieved filter;(5) spray drying: prepare Herba Leonuri dried cream powder;(6) granulate: Herba Leonuri dried cream powder and adjuvant are carried out dispensing, mixing, granulate;(7) second time is sieved: collect conforming particle.
2. the preparation method of yimucao drop preparation according to claim 1, it is characterized in that, in described step (1) dynamic extraction process: first add the hot water of 80 ± 5 DEG C toward extraction pot, add the Herba Leonuri of chopping, affiliated hot water weight is 2~4 times of Herba Leonuri, continues the hot water supplementing 80 ± 5 DEG C to 9~11 times of Herba Leonuri weight, heats and make water temperature rise to 95 ± 3 DEG C, carry out dynamic extraction, after extraction, obtain medicinal residues and extracting solution.
3. the preparation method of yimucao drop preparation according to claim 1, it is characterised in that described step (2) centrifugal separation processes includes:
A () uses centrifuge that the extracting solution that step (1) obtains is carried out solid-liquid separation, extracting solution temperature is 95 ± 3 DEG C, and centrifuge speed is 1000~5000 revs/min;
B () uses supercentrifuge that the medicinal liquid after step (a) separation is carried out ultracentrifugation, fluid temperature is 80~95 DEG C, and supercentrifuge rotating speed is 1.3~1.5 ten thousand revs/min.
4. the preparation method of yimucao drop preparation according to claim 1, it is characterized in that, in described step (3) concentrating under reduced pressure process: clear liquor enters concentration tank by negative pressure, feed liquor speed is 600~1000L/h, vacuum is-0.06~-0.1MPa, temperature is 50~60 DEG C, circulating water temperature 30~40 DEG C.
5. the preparation method of yimucao drop preparation according to claim 4, it is characterised in that the relative density having concentrated rear gained Herba Leonuri extractum 50~60 DEG C is 1.05~1.1.
6. the preparation method of yimucao drop preparation according to claim 1, it is characterized in that, described step (4) first time sieves in process: is placed in jacketed pan by the extractum that step (3) obtains, stirs, heating, to boiling, uses 200~400 mesh sieves to be filtered.
7. the preparation method of yimucao drop preparation according to claim 1, it is characterized in that, in described step (5) spray-drying process: the concentrated solution filtered is thrown into and treats in Liquid spray reservoir, 75~85 DEG C of stirring insulations, by nebulizer feed liquor spray drying, prepare Herba Leonuri dried cream powder.
8. the preparation method of yimucao drop preparation according to claim 1; it is characterized in that; in described step (6) pelletization: being put in Drygranulatemachine by the material of mix homogeneously and granulate, Drygranulatemachine sets roller pressure as 90~110kg/cm2, side seal pressure be 25~50kg/cm2
9. the preparation method of yimucao drop preparation according to claim 1, it is characterized in that, described step (7) second time is sieved in process: the granule that step (6) prepares is crossed shaking screen, shaking screen screen cloth specification is upper 12 orders and lower 40 orders, is collected by 12 orders and does not pass through the granule of 40 mesh sieve gained.
10. the preparation method of yimucao drop preparation according to claim 1, it is characterized in that, in described step (6) pelletization, described adjuvant includes dextrin, maltodextrin and steviosin, calculating by weight, described dispensing includes Herba Leonuri dried cream powder 100~130 weight portion, dextrin 70~90 weight portion, maltodextrin 20~30 weight portion and steviosin 0.4~1 weight portion.
CN201610325097.2A 2016-05-17 2016-05-17 Preparation method of motherwort herb granules Pending CN105769991A (en)

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