CN104324103A - Medicated leaven pure powder superfine decoction piece and preparation method thereof - Google Patents
Medicated leaven pure powder superfine decoction piece and preparation method thereof Download PDFInfo
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- 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
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- 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
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/899—Poaceae or Gramineae (Grass family), e.g. bamboo, corn or sugar cane
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- 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
- A61K9/141—Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers
- A61K9/143—Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers with inorganic compounds
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- 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
- A61K9/141—Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers
- A61K9/145—Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers with organic compounds
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- 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
- A61K9/20—Pills, tablets, discs, rods
- A61K9/2095—Tabletting processes; Dosage units made by direct compression of powders or specially processed granules, by eliminating solvents, by melt-extrusion, by injection molding, by 3D printing
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- 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
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/5089—Processes
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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
-
- 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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
-
- 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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
Abstract
The invention discloses a medicated leaven pure powder ultramicro decoction piece preparation method and a prepared product. The preparation method is as follows: crushing dried medicated leaven active extracts to the particle size below 300 microns, performing ultramicro-crushing in an airflow crusher to prepare a the ultramicro decoction piece, and the ultramicro-crushing conditions are as follows: the crushing temperature is 15-22 DEG C, the pressure is 1-2MPa when entering the ultramicro-crusher, the crushing pressure is 2-6MPa, the air flow velocity is 200-285m / s, and the crushing time is 1-3H. The oral medicament prepared by the preparation method has good effect, good dissolution property, good stability and high bioavailability, and the smell and taste of the oral medicament are improved.
Description
Technical field
The present invention relates to field of traditional Chinese, particularly pure powder ultramicro decoction piece of Massa Medicata Fermentata and preparation method thereof.
Background technology
" Massa Medicata Fermentata " is that the one that Han dynasty well-known doctor Liu Yi develops cures dyspeptic famous medicine.But, at the beginning of the appearance of Massa Medicata Fermentata, be but the enlightenment receiving wild animal autotherapy behavior.A period of time, Liu Yi finds that the egg in oneself chicken coop is often lost, and just pays attention to and observes, and discovery is that a fire white silk Serpentis is done.So he determines to punish this Serpentis.He wraps up in stone with Calx and has done several pieces of false eggs, is coated with last layer Ovum Gallus domesticus album again, is placed on inside chicken coop, then just wait for aside outside false egg.Soon, he sees that Serpentis crawls in chicken coop, has been swallowed by those several pieces false eggs.Few that Serpentis is painful on the ground to struggle a little while, and then it is born misery and crawls into from the grass, a kind of fluffy Caulis et Folium Polygalae Tenuifoliae of desperately eating.Time few, Serpentis has discharged a pile feces, has then climbed away impunity.Liu Yi thinks, this careless one controls dyspepsia surely.So he for principal agent, develops the dyspeptic famous medicine Massa Medicata Fermentata for the treatment of with this grass.
The needs of modern healthy, in field of traditional Chinese in succession, revive and develop middle formation numerous Chinese medicine old established firm brand, as Tongrentang (1669), Hu Qingyu Pharmaceutical Workshop (1874), large life auspicious (1885), Han Xingtang (1901), Fu Tong (1644), Fructus Pruni and hall (1600), public good is large, Chen Zhi father-in-law, bosom moral crane (1948), old man and Tai, father-in-law Changchun (1699), Fu Jichun, refined vegetarian (between bright year in Wanli year), first-class and the Chinese medicine health-care tea old established firm brand of Lei Yun is as ten thousand safe units (1860), Zhu Qiansheng, roc red sun, universe Thailand is poly-, wherein ten thousand safe first tea No. win ten thousand state's World's Fair gold medals in 1915 especially, the first-class Grand Prix of nineteen twenty-six U.S. Philadelphia World's Fair and nineteen twenty-nine first West Lake Exposition gold medal.But Chinese medicine decoction pieces is concocted in a usual manner, medical material effective ingredient runs off or cannot fully discharge, and the sporoderm-broken rate of cell is extremely low, and its bioavailability is lower, and herb resource is wasted.Because its dissolution rate is low, therefore must be enough, and adhere to that the long period continues to take just meeting effectively, but this situation can cause drug cost high.Peroral dosage form mature preparation process in prior art, but its defect also can not be ignored.The preparation method of conventional peroral dosage form; usually can with problems such as the loss of medical material effective ingredient, degeneration or impurity increase; particularly for Massa Medicata Fermentata be key agents active component preparation technology in; because the active constituents of medicine in Massa Medicata Fermentata is comparatively responsive to preparation technology parameter; preparation technology is improper; make drug dissolution low, active constituent content reduces, and bioavailability is low.
Superfine communication technique developed a very fast new technique in recent years.Apply this technology, solid matter can be ground into the superfine powder that diameter is less than 10 microns, thus, the powder body through micronizing process often has good dissolubility, therefore can consider the preparation technology being applied to peroral dosage form.
But, in prior art, still superfine communication technique is not applied to the technique preparing Massa Medicata Fermentata decoction pieces, its reason is as previously mentioned: the active constituents of medicine in Massa Medicata Fermentata is comparatively responsive for preparation technology, and the technological parameter of micronizing often causes the degeneration of active constituents of medicine, therefore, obtained peroral dosage form effective ingredient easily decomposes, impurity is many, and uniformity of dosage units is poor, poor stability.On this basis, seek one and can not cause active constituents of medicine degeneration, and obtained peroral dosage form has the micronizing technological parameter of more excellent properties, is a difficult problem urgently to be resolved hurrily in prior art.
Summary of the invention
It is low that main purpose of the present invention is to overcome Massa Medicata Fermentata extract oral drug form dissolution in prior art, active constituent content reduces, bioavailability is low, and the process conditions of the superfine communication technique of routine are not suitable for the preparation of Massa Medicata Fermentata peroral dosage form, in obtained peroral dosage form, effective ingredient easily decomposes, and impurity is many, and uniformity of dosage units is poor, the defect of poor stability etc., provides preparation technology of the pure powder ultramicro decoction piece of a kind of Massa Medicata Fermentata and preparation method thereof.The peroral dosage form good drug efficacy that the preparation technology of the pure powder ultramicro decoction piece of Massa Medicata Fermentata of the present invention obtains, stripping property is good, good stability, and bioavailability is high, and the abnormal smells from the patient of peroral dosage form and mouthfeel improve.
The present invention solves the problems of the technologies described above by the following technical programs:
An object of the present invention is, provide the preparation method of the pure powder ultramicro decoction piece of a kind of Massa Medicata Fermentata, described preparation method comprises the following steps:
The Massa Medicata Fermentata activity extract of drying is crushed to particle diameter less than 300 microns, micronizing in jet mill again, obtain ultramicro decoction piece, the condition of described micronizing is: pulverize temperature 15-22 DEG C, pressure when entering super micron mill is 1-2Mpa, pulverize pressure 2-6Mpa, air velocity 200-285m/s, the time 1-3h of pulverizing.
Preferred further technical scheme below for above-mentioned steps does following explanation:
By obtained ultramicro decoction piece with meet the adjuvant that medicament requires, obtained tablet, capsule or other oral normal release dosage forms.
Described Massa Medicata Fermentata activity extract obtains for extracting according to following extracting method: by Massa Medicata Fermentata according to Massa Medicata Fermentata: ethanol=1: 6 ~ 12 add extraction vessel, wherein the ratio of Massa Medicata Fermentata and ethanol is weight ratio, and ethanol is the alcohol heating reflux lixiviate of 95%, temperature 90 DEG C, extract 2 times, time is respectively 3 ~ 4h and 1 ~ 2h, obtains crude extract; Crude extract is carried out rapid filtration under suction, and it is 1.3 that filter vacuum is concentrated into 25 DEG C of relative densities, namely obtains Massa Medicata Fermentata extract, and the condition of vacuum concentration is 45 ~ 55 DEG C, carry out under 80kPa.
Described Massa Medicata Fermentata is obtained by following preparation method: take by weight: flour 100kg, Semen Armeniacae Amarum 4kg, Semen Phaseoli 4kg, fresh Herba Artemisiae Annuae 7kg, fresh Herba polygoni hydropiperis 7kg, fresh Herba Xanthii grass 7kg; By described fresh Herba Artemisiae Annuae, fresh Herba polygoni hydropiperis, fresh Herba Xanthii grass adds water 500L, decocts 50 minutes, filters, concentrates filtrate to 50L, obtain concentrated solution; Described Semen Armeniacae Amarum and Semen Phaseoli are ground into Semen Armeniacae Amarum powder and Semen Phaseoli powder, and described Semen Armeniacae Amarum powder and described Semen Phaseoli powder were the powder of 50 mesh sieves; Described concentrated solution and described flour, Semen Armeniacae Amarum powder and Semen Phaseoli powder are mixed, rub agglomerating, tight with paper bag, between 32-35 DEG C, natural fermentation 5-7 days, puts into dicer and is cut into small pieces, natural drying after taking-up.
Described adjuvant is the adjuvant of this area routine, preferably comprises one or more in disintegrating agent, lubricant, binding agent and filler.The addition of described adjuvant is preferably 10%-40%, and described percentage ratio is the mass percent accounting for described Massa Medicata Fermentata activity extract.
Wherein, described disintegrating agent is the disintegrating agent of this area routine, is preferably one or more in starch, microcrystalline Cellulose, hydroxypropyl emthylcellulose, sodium alginate, crospolyvinylpyrrolidone and cross-linking sodium carboxymethyl cellulose.The addition of described disintegrating agent is the addition of this area routine, is preferably 5%-15%, and described percentage ratio is the mass percent accounting for described Massa Medicata Fermentata activity extract.
Wherein, described lubricant is the lubricant of this area routine, is preferably one or more in magnesium stearate, sodium laurylsulfate and boric acid.The addition of described lubricant is the addition of this area routine, is preferably 3%-9%, and described percentage ratio is the mass percent accounting for described Massa Medicata Fermentata activity extract.
Wherein, described binding agent is the binding agent of this area routine, is preferably micropowder silica gel and/or Pulvis Talci.The addition of described binding agent is the addition of this area routine, is preferably 1%-5%, and described percentage ratio is the mass percent accounting for described Massa Medicata Fermentata activity extract.
Wherein, described filler is the filler of this area routine, is preferably lactose and/or calcium sulfate.The addition of described filler is the addition of this area routine, is preferably 1%-15%, and described percentage ratio is the mass percent accounting for described Massa Medicata Fermentata activity extract.
In step (1), the condition of described micronizing is preferably: pulverize temperature 20 DEG C, pressure when entering super micron mill is 1.5Mpa, pulverizes pressure 3-5Mpa, air velocity 220-260m/s, the time 1.5-2.5h of pulverizing.
In step (1), the method for described drying and condition are ability and conventional method and condition, and described drying is preferably carried out in vacuum drier.Described vacuum drying temperature is preferably 80-110 DEG C, and described vacuum drying pressure is preferably-0.1 ~ 0.2mpa.
In step (1), described is crushed to particle diameter less than 300 microns, then in jet mill before micronizing, preferably carries out sterilization treatment.The method of described sterilizing is the method for this area routine, is preferably one or more in ray sterilizing, microwave sterilizating, wet-hot steam sterilizing and ozone sterilization.
In step (1), described micronizing is preferably crushed to particle diameter 1-80 micron, and the particulate accumulation that particle diameter is less than 65 microns is no less than 90%.
Two of object of the present invention is, provides the pure powder ultramicro decoction piece of Massa Medicata Fermentata that preparation method as above is obtained.
On the basis meeting this area general knowledge, above-mentioned each optimum condition, can combination in any, obtains the preferred embodiments of the invention.
Agents useful for same of the present invention and raw material are all commercially.
Positive progressive effect of the present invention is: the peroral dosage form good drug efficacy that the preparation technology of the pure powder ultramicro decoction piece of Massa Medicata Fermentata of the present invention obtains, and stripping property is good, good stability, and bioavailability is high, and the abnormal smells from the patient of peroral dosage form and mouthfeel improve.
Detailed description of the invention
Mode below by embodiment further illustrates the present invention, but does not therefore limit the present invention among described scope of embodiments.
The raw material of the pure powder of the Massa Medicata Fermentata in embodiment 1-6 ultramicro decoction piece is as shown in table 1.
The raw material of the pure powder ultramicro decoction piece of the Massa Medicata Fermentata in table 1 embodiment 1-6
Note: in upper table, the addition of active constituents of medicine is weight portion; The addition of adjuvant is the mass percent accounting for active constituents of medicine.
In embodiment 1-3, the preparation method of Massa Medicata Fermentata extract comprises the following steps:
Massa Medicata Fermentata is obtained by following preparation method: take by weight: flour 100kg, Semen Armeniacae Amarum 4kg, Semen Phaseoli 4kg, fresh Herba Artemisiae Annuae 7kg, fresh Herba polygoni hydropiperis 7kg, fresh Herba Xanthii grass 7kg; By described fresh Herba Artemisiae Annuae, fresh Herba polygoni hydropiperis, fresh Herba Xanthii grass adds water 500L, decocts 50 minutes, filters, concentrates filtrate to 50L, obtain concentrated solution; Described Semen Armeniacae Amarum and Semen Phaseoli are ground into Semen Armeniacae Amarum powder and Semen Phaseoli powder, and described Semen Armeniacae Amarum powder and described Semen Phaseoli powder were the powder of 50 mesh sieves; Described concentrated solution and described flour, Semen Armeniacae Amarum powder and Semen Phaseoli powder are mixed, rub agglomerating, tight with paper bag, between 32-35 DEG C, natural fermentation 5-7 days, puts into dicer and is cut into small pieces, natural drying after taking-up.Described Massa Medicata Fermentata activity extract obtains for extracting according to following extracting method: by Massa Medicata Fermentata according to Massa Medicata Fermentata: ethanol=1: 6 ~ 12 add extraction vessel, wherein the ratio of Massa Medicata Fermentata and ethanol is weight ratio, and ethanol is the alcohol heating reflux lixiviate of 95%, temperature 90 DEG C, extract 2 times, time is respectively 3 ~ 4h and 1 ~ 2h, obtains crude extract; Crude extract is carried out rapid filtration under suction, and it is 1.3 that filter vacuum is concentrated into 25 DEG C of relative densities, namely obtains Massa Medicata Fermentata extract, and the condition of vacuum concentration is 45 ~ 55 DEG C, carrying out amount of water under 80kPa should at 35%-45%, and ferment effect is better; The sample fermented 7 days, its enzyme activity is all higher; This shortens the production time, decreases industrial land, improves production efficiency.Improve sanitary condition and production environment, facilitate the clean of place and production management, simplify production procedure, production process is easy to control, and is conducive to achieving the automatization of the process of preparing Chinese medicine, scale and standardization.
Massa Medicata Fermentata activity extract obtains for extracting according to following extracting method: by Massa Medicata Fermentata according to Massa Medicata Fermentata: ethanol=1: 6 ~ 12 add extraction vessel, wherein the ratio of Massa Medicata Fermentata and ethanol is weight ratio, and ethanol is the alcohol heating reflux lixiviate of 95%, temperature 90 DEG C, extract 2 times, time is respectively 3 ~ 4h and 1 ~ 2h, obtains crude extract; Crude extract is carried out rapid filtration under suction, and it is 1.3 that filter vacuum is concentrated into 25 DEG C of relative densities, namely obtains Massa Medicata Fermentata extract, and the condition of vacuum concentration is 45 ~ 55 DEG C, carry out under 80kPa.The extraction rate carrying active component of this extracting method is high, and when Massa Medicata Fermentata and proportion of ethanol are 1: 9, the extraction rate of the active abstract of Massa Medicata Fermentata is the highest, simultaneously, when 90 degree, ensure that its active component can better stripping, ensure that the stability of its active component, when extracting twice simultaneously, active component can propose 60%, when identical condition extracts three times, its active component also can only reach 62%, when therefore extracting twice, it is maximum that active component extracts, and simultaneously most economical.Crude extract is carried out rapid filtration under suction, and filter vacuum is concentrated into 25 DEG C of relative densities when being 1.3, and convenient next time uses.
Embodiment 1
Preparation technology:
Massa Medicata Fermentata activity extract described in drying is crushed to particle diameter less than 300 microns, ray sterilizing, then in jet mill micronizing to 40 micron, the particulate accumulation 90% that particle diameter is less than 65 microns, obtains ultramicro decoction piece;
Wherein, vacuum drying temperature is 100 DEG C, and pressure is 0.1mpa; The condition of micronizing is: pulverize temperature 20 DEG C, pressure when entering super micron mill is 1.5Mpa, pulverizes pressure 3Mpa, air velocity 220m/s, the time 1.5h of pulverizing;
By obtained ultramicro decoction piece with meet the adjuvant that medicament requires, obtained tablet, capsule or other oral normal release dosage forms.
Embodiment 2
Preparation technology:
Massa Medicata Fermentata activity extract described in drying is crushed to particle diameter less than 300 microns, microwave sterilizating, then in jet mill micronizing to 50 micron, the particulate accumulation 95% that particle diameter is less than 65 microns, obtains ultramicro decoction piece;
Wherein, vacuum drying temperature is 90 DEG C, and pressure is 0.2mpa; The condition of micronizing is: pulverize temperature 20 DEG C, pressure when entering super micron mill is 1.5Mpa, pulverizes pressure 5Mpa, air velocity 260m/s, the time 1.5h of pulverizing;
By obtained ultramicro decoction piece with meet the adjuvant that medicament requires, obtained tablet, capsule or other oral normal release dosage forms.
Embodiment 3
Preparation technology:
Massa Medicata Fermentata activity extract described in drying is crushed to particle diameter less than 300 microns, ozone sterilization, then in jet mill micronizing to 35 micron, the particulate accumulation 93% that particle diameter is less than 65 microns, obtains ultramicro decoction piece;
Wherein, vacuum drying temperature is 90 DEG C, and pressure is 0.1mpa; The condition of micronizing is: pulverize temperature 20 DEG C, pressure when entering super micron mill is 1.5Mpa, pulverizes pressure 5Mpa, air velocity 240m/s, the time 2.5h of pulverizing;
By obtained ultramicro decoction piece with meet the adjuvant that medicament requires, obtained tablet, capsule or other oral normal release dosage forms.
Embodiment 4
Preparation technology:
Massa Medicata Fermentata activity extract described in drying is crushed to particle diameter less than 300 microns, then in jet mill micronizing to 80 micron, the particulate accumulation 90% that particle diameter is less than 65 microns, obtains ultramicro decoction piece;
Wherein, vacuum drying temperature is 80 DEG C, and pressure is 0.2mpa; The condition of micronizing is: pulverize temperature 15 DEG C, pressure when entering super micron mill is 1Mpa, pulverizes pressure 6Mpa, air velocity 200m/s, the time 3h of pulverizing;
By obtained ultramicro decoction piece with meet the adjuvant that medicament requires, obtained tablet, capsule or other oral normal release dosage forms.
Embodiment 5
Preparation technology:
(1) the Massa Medicata Fermentata activity extract described in drying is crushed to particle diameter less than 300 microns, wet-hot steam sterilizing, then in jet mill micronizing to 10 micron, the particulate accumulation 90% that particle diameter is less than 65 microns, obtains ultramicro decoction piece;
Wherein, vacuum drying temperature is 80 DEG C, and pressure is-0.1mpa; The condition of micronizing is: pulverize temperature 22 DEG C, pressure when entering super micron mill is 2Mpa, pulverizes pressure 6Mpa, air velocity 285m/s, the time 1h of pulverizing;
By obtained ultramicro decoction piece with meet the adjuvant that medicament requires, obtained tablet, capsule or other oral normal release dosage forms.
Embodiment 6
Preparation technology:
Massa Medicata Fermentata activity extract described in drying is crushed to particle diameter less than 300 microns, then in jet mill micronizing to 1 micron, the particulate accumulation 90% that particle diameter is less than 65 microns, obtains micropowder;
Wherein, vacuum drying temperature is 80 DEG C, and pressure is 0.2mpa; The condition of micronizing is: pulverize temperature 22 DEG C, pressure when entering super micron mill is 2Mpa, pulverizes pressure 6Mpa, air velocity 285m/s, the time 3h of pulverizing;
By obtained ultramicro decoction piece with meet the adjuvant that medicament requires, obtained tablet, capsule or other oral normal release dosage forms.
Comparative example 1
Raw material and addition thereof are with embodiment 1;
Preparation technology: the condition of micronizing is: pulverizing temperature is 25 DEG C, and all the other step of preparation process and condition are with embodiment 1.
Comparative example 2
Raw material and addition thereof are with embodiment 2;
Preparation technology: the condition of micronizing is: pulverize pressure 8Mpa, all the other step of preparation process and condition are with embodiment 2.
Comparative example 3
Raw material and addition thereof are with embodiment 2;
Preparation technology: the condition of micronizing is: the time 4h of pulverizing, all the other step of preparation process and condition are with embodiment 3.
Effect example 1
Stability comparative experiments
1, sample acceleration environment: after sample being put high-density polyethylene bottle packaging, in temperature 40 ± 2 DEG C, place under the condition of relative humidity 75 ± 5%, after accelerated test March, inspection character, dissolution, content and related substance are carried out in sampling.
2, assay method:
1) dissolution method is according to dissolution method (Chinese Pharmacopoeia 2,010 two annex XC the 3rd methods), and with water 100ml for dissolution medium, rotating speed is 50 turns per minute, operates in accordance with the law, samples, get subsequent filtrate as need testing solution when 30 minutes; Every m1 is prepared about containing the solution product solution in contrast of rasagiline 10 μ g, respectively injection liquid chromatography, by external standard method with calculated by peak area stripping quantity with reference substance.
2) content and related substance all adopt high performance liquid chromatography (Chinese Pharmacopoeia 2,010 two annex VD) to measure, and be filler with octadecylsilane silica gel, determined wavelength is 210nm, and record chromatogram, by external standard method with calculated by peak area.
3, stability data compares: in table 2.
Table 2 stability data compares
Effect example 3 uniformity of dosage units compares
According to Chinese Pharmacopoeia version annex XE Content uniformity test in 2010, adopt the content of the every sheet of high effective liquid chromatography for measuring, and calculate uniformity of dosage units (A+1.80S).The results are shown in Table 3.
Table 3 uniformity of dosage units tables of data
| Group | Average content | Uniformity of dosage units |
| Embodiment 1 | 100.4 | 2.47 |
| Embodiment 2 | 100.8 | 2.37 |
| Embodiment 3 | 99.1 | 2.76 |
| Embodiment 4 | 99.2 | 2.45 |
| Embodiment 5 | 99.6 | 2.65 |
| Embodiment 6 | 99.4 | 2.98 |
| Comparative example 1 | 99.8 | 4.12 |
| Comparative example 2 | 99.1 | 4.89 |
| Comparative example 3 | 98.9 | 4.87 |
The above; be only preferred embodiment of the present invention; not to any formal and substantial restriction of the present invention; should be understood that; for those skilled in the art; under the prerequisite not departing from the inventive method, also can make some improvement and supplement, these improve and supplement and also should be considered as protection scope of the present invention.All those skilled in the art, without departing from the spirit and scope of the present invention, a little change made when utilizing disclosed above technology contents, the equivalent variations of modifying and developing, be Equivalent embodiments of the present invention; Meanwhile, all according to substantial technological of the present invention to the change of any equivalent variations that above-described embodiment is done, modify and differentiation, all still belong in the scope of technical scheme of the present invention.
Claims (10)
1. a preparation method for the pure powder ultramicro decoction piece of Massa Medicata Fermentata, is characterized in that: described preparation method comprises the following steps:
The Massa Medicata Fermentata activity extract of drying is crushed to particle diameter less than 300 microns, micronizing in jet mill again, obtain ultramicro decoction piece, the condition of described micronizing is: pulverize temperature 15-22 DEG C, pressure when entering super micron mill is 1-2Mpa, pulverize pressure 2-6Mpa, air velocity 200-285m/s, the time 1-3h of pulverizing.
2. the preparation method of the pure powder ultramicro decoction piece of Massa Medicata Fermentata according to claim 1, is characterized in that: by obtained ultramicro decoction piece with meet the adjuvant that medicament requires, obtained tablet, capsule or other oral normal release dosage forms.
3. the preparation method of the pure powder ultramicro decoction piece of Massa Medicata Fermentata according to claim 2, it is characterized in that: described Massa Medicata Fermentata activity extract obtains for extracting according to following extracting method: by Massa Medicata Fermentata according to Massa Medicata Fermentata: ethanol=1: 6 ~ 12 add extraction vessel, wherein the ratio of Massa Medicata Fermentata and ethanol is weight ratio, and ethanol is the alcohol heating reflux lixiviate of 95%, temperature 90 DEG C, extract 2 times, the time is respectively 3 ~ 4h and 1 ~ 2h, obtains crude extract; Crude extract is carried out rapid filtration under suction, and it is 1.3 that filter vacuum is concentrated into 25 DEG C of relative densities, namely obtains Massa Medicata Fermentata extract, and the condition of vacuum concentration is 45 ~ 55 DEG C, carry out under 80kPa.
4. preparation method according to claim 3, is characterized in that: described Massa Medicata Fermentata is obtained by following preparation method: take by weight: flour 100kg, Semen Armeniacae Amarum 4kg, Semen Phaseoli 4kg, fresh Herba Artemisiae Annuae 7kg, fresh Herba polygoni hydropiperis 7kg, fresh Herba Xanthii grass 7kg; By described fresh Herba Artemisiae Annuae, fresh Herba polygoni hydropiperis, fresh Herba Xanthii grass adds water 500L, decocts 50 minutes, filters, concentrates filtrate to 50L, obtain concentrated solution; Described Semen Armeniacae Amarum and Semen Phaseoli are ground into Semen Armeniacae Amarum powder and Semen Phaseoli powder, and described Semen Armeniacae Amarum powder and described Semen Phaseoli powder were the powder of 50 mesh sieves; Described concentrated solution and described flour, Semen Armeniacae Amarum powder and Semen Phaseoli powder are mixed, rub agglomerating, tight with paper bag, between 32-35 DEG C, natural fermentation 5-7 days, puts into dicer and is cut into small pieces, natural drying after taking-up.
5. the preparation method according to any one of claim 1-4, is characterized in that: described adjuvant comprise in disintegrating agent, lubricant, binding agent and filler one or more; The addition of described adjuvant is 10%-40%, and described percentage ratio is the mass percent accounting for described Massa Medicata Fermentata activity extract.
6. preparation method according to claim 5, is characterized in that: described disintegrating agent is one or more in starch, microcrystalline Cellulose, hydroxypropyl emthylcellulose, sodium alginate, crospolyvinylpyrrolidone and cross-linking sodium carboxymethyl cellulose; The addition of described disintegrating agent is 5%-15%;
Described lubricant is one or more in magnesium stearate, sodium laurylsulfate and boric acid; The addition of described lubricant is 3%-9%;
Described binding agent is micropowder silica gel and/or Pulvis Talci; The addition of described binding agent is 1%-5%;
Described filler is for being lactose and/or calcium sulfate; The addition of described filler is 1%-15%;
Described percentage ratio is the mass percent accounting for described Massa Medicata Fermentata activity extract.
7. the preparation method according to any one of claim 1-4, it is characterized in that: the condition of described micronizing is: pulverize temperature 20 DEG C, pressure when entering super micron mill is 1.5Mpa, pulverize pressure 3-5Mpa, air velocity 220-260m/s, the time 1.5-2.5h of pulverizing.
8. the preparation method according to any one of claim 1-4, is characterized in that: described drying is carried out in vacuum drier; Described vacuum drying temperature is 80-110 DEG C, and described vacuum drying pressure is-0.1 ~ 0.2mpa.
9. the preparation method according to any one of claim 1-4, is characterized in that: described is crushed to particle diameter less than 300 microns, then in jet mill before micronizing, carries out sterilization treatment; Described sterilizing is one or more in ray sterilizing, microwave sterilizating, wet-hot steam sterilizing and ozone sterilization;
Described micronizing is for being crushed to particle diameter 1-80 micron.
10. the pure powder ultramicro decoction piece of Massa Medicata Fermentata that the preparation method according to any one of claim 1-9 is obtained.
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