CN105497722A - Preparation method for Mongolian four-species elecampane inula root decoction superfine powder tablets, granules and capsules - Google Patents

Preparation method for Mongolian four-species elecampane inula root decoction superfine powder tablets, granules and capsules Download PDF

Info

Publication number
CN105497722A
CN105497722A CN201510990820.4A CN201510990820A CN105497722A CN 105497722 A CN105497722 A CN 105497722A CN 201510990820 A CN201510990820 A CN 201510990820A CN 105497722 A CN105497722 A CN 105497722A
Authority
CN
China
Prior art keywords
volatile oil
preparation
powder
extraction
superfine powder
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201510990820.4A
Other languages
Chinese (zh)
Inventor
包保全
张屏
李玉棠
陈建平
宋宏春
杭凌宇
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CN201510990820.4A priority Critical patent/CN105497722A/en
Publication of CN105497722A publication Critical patent/CN105497722A/en
Pending legal-status Critical Current

Links

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
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/28—Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
    • 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)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
    • A61K36/489—Sophora, e.g. necklacepod or mamani
    • 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)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/73—Rosaceae (Rose family), e.g. strawberry, chokeberry, blackberry, pear or firethorn
    • 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)
    • A61K36/906—Zingiberaceae (Ginger family)
    • 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
    • A61K9/2004—Excipients; Inactive ingredients
    • A61K9/2009—Inorganic compounds
    • 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
    • A61K9/2004—Excipients; Inactive ingredients
    • A61K9/2013—Organic compounds, e.g. phospholipids, fats
    • 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
    • A61K9/2004—Excipients; Inactive ingredients
    • A61K9/2022—Organic macromolecular compounds
    • A61K9/205—Polysaccharides, e.g. alginate, gums; Cyclodextrin
    • A61K9/2054—Cellulose; Cellulose derivatives, e.g. hydroxypropyl methylcellulose
    • 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
    • A61K9/2004—Excipients; Inactive ingredients
    • A61K9/2022—Organic macromolecular compounds
    • A61K9/205—Polysaccharides, e.g. alginate, gums; Cyclodextrin
    • A61K9/2059—Starch, including chemically or physically modified derivatives; Amylose; Amylopectin; Dextrin
    • 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
    • A61K9/28—Dragees; Coated pills or tablets, e.g. with film or compression coating
    • A61K9/2893—Tablet coating processes
    • 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
    • A61K9/4841—Filling excipients; Inactive ingredients
    • A61K9/4866—Organic macromolecular compounds
    • 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
    • A61K9/5005—Wall or coating material
    • A61K9/5021—Organic macromolecular compounds
    • A61K9/5036—Polysaccharides, e.g. gums, alginate; Cyclodextrin
    • A61K9/5042—Cellulose; Cellulose derivatives, e.g. phthalate or acetate succinate esters of hydroxypropyl methylcellulose
    • 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
    • A61K2236/10—Preparation or pretreatment of starting material
    • A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
    • 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
    • A61K2236/30—Extraction of the material
    • A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • 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
    • 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

Abstract

The invention discloses a preparation method for Mongolian four-species elecampane inula root decoction superfine powder tablets, granules and capsules. A superfine grinding technology adopted the four-species elecampane inula root decoction superfine powder is based on the theory of breaking plant medicine cell walls and promoting dissolution and dispersion of ingredients in cells, and the dissolving-out quantity and speed of the ingredients in the plant cells in vivo or a solvent are increased to achieve the aims of improving the bioavailability of medicine, reducing the taking amount and improving preparation quality. Processes adopted in the four-species elecampane inula root decoction granules comprise the freeze-drying process, the beta-cyclodextrin inclusion process and the coating process. Effective ingredients are fully kept, and meanwhile the problems that the taste is poor, carrying is inconvenient, and taking is inconvenient are solved. Processes adopted in the four-species elecampane inula root decoction capsules comprise the freeze-drying process, the beta-cyclodextrin inclusion process and the capsule preparation process. The effective ingredients are fully kept, the defects of solid dosage forms are overcome, the bioavailability is improved, and meanwhile the problem that the taste is poor and other problems are solved.

Description

The preparation method of dry soup submicron powder sheet, granule, capsule looked into by mongolian medicine
Technical field
The present invention relates to pharmaceutical formulating art, be specifically related to the preparation method that a kind of mongolian medicine looks into dry soup submicron powder sheet, granule, capsule.
Background technology
Current commercially available Sophara Flavescens Ait is ground into coarse powder by Radix Inulae, Radix Sophorae Flavescentis, Fructus Rubi corchorifolii Immaturus, Rhizoma Kaempferiae four Chinese medicine material, and sieve, mixing prepares.Instructions of taking is for being decocted in water for oral dose.Owing to containing Radix Sophorae Flavescentis in Sophara Flavescens Ait, during decoction, in Radix Sophorae Flavescentis, alkaloids becomes branch's pungent taste to feel, makes Sophara Flavescens Ait mouthfeel extremely bitter, is not easy to take, especially for child.
Summary of the invention
For solving the problem, the invention provides the preparation method that a kind of mongolian medicine looks into dry soup submicron powder sheet, granule, capsule.
For achieving the above object, the technical scheme that the present invention takes is:
A preparation method for dry soup superfine powder looked into by mongolian medicine, it is characterized in that, comprises the steps:
S11, Radix Inulae, Radix Sophorae Flavescentis, Fructus Rubi corchorifolii Immaturus, Rhizoma Kaempferiae are ground into coarse powder after, use Baily pulverizing mill (BFM-6A) gained coarse powder is carried out micronizing respectively;
S12, in mass ratio 4: 4: 2: 1 take Radix Inulae, Radix Sophorae Flavescentis, Fructus Rubi corchorifolii Immaturus, Rhizoma Kaempferiae Homogeneous phase mixing, add filler and disintegrating agent, binding agent is added again after mixing, the consumption of binding agent with 80% ethanol for test material, by a small amount of (to add to namely loose being as the criterion of loosing one's grip after soft material is held), moderate (hold agglomerating rear hands and pinch the dispersion that granulates to add to soft material and be as the criterion), volume (hold agglomerating rear hands and pinch into bulk to add to soft material and be separated into standard) 3 kinds of additions, be respectively used to soft material processed, each soft material granulation and compression tablet molding effect are compared.
S13, the soft material of gained is crossed 20 mesh sieves, the wet granular made, be placed in 60 DEG C of baking ovens, dry 40min, after 20 mesh sieve granulate, after adding lubricant, use diameter to be the shallow round punch die tabletting of 10 millimeters.
Present invention also offers the preparation method that dry decoction particles looked into by a kind of mongolian medicine, comprise the steps:
S21, in mass ratio 4: 4: 2: 1 take Radix Inulae, Radix Sophorae Flavescentis, Fructus Rubi corchorifolii Immaturus and Rhizoma Kaempferiae, and Radix Inulae coarse powder vapor extraction method extracts volatile oil, and the another device of the aqueous solution after distillation is collected, and obtains volatile oil and water solution A;
The coarse powder of S22, alcohol extraction Radix Sophorae Flavescentis, Rhizoma Kaempferiae, Fructus Rubi corchorifolii Immaturus, the another device of alcohol extract is collected, and reclaim ethanol, extracting solution is separately deposited, and water extraction is carried out in the medicinal residues mixing of the medicinal residues of alcohol extraction and volatile oil is drawn, obtains aqueous solution B,
S23, aqueous solution B and water solution A are merged, after being concentrated to 500mL, merge with alcohol extract, lyophilization becomes lyophilized powder;
S24, the volatile oil of step S21 gained adopted after beta-cyclodextrin inclusion compound mix with lyophilized powder, coated granule processed.
Present invention also offers the preparation method that dry soup capsule looked into by a kind of mongolian medicine, it is characterized in that, comprise the steps:
S31, in mass ratio 4: 4: 2: 1 take Radix Inulae, Radix Sophorae Flavescentis, Fructus Rubi corchorifolii Immaturus and Rhizoma Kaempferiae, extract volatile oil by vapor extraction method, and the another device of the aqueous solution after distillation is collected, and obtains volatile oil and water solution A;
The coarse powder of S32, alcohol extraction Radix Sophorae Flavescentis, Rhizoma Kaempferiae, Fructus Rubi corchorifolii Immaturus, the another device of alcohol extract is collected, and reclaim ethanol, extracting solution is separately deposited, and water extraction is carried out in the medicinal residues mixing of the medicinal residues of alcohol extraction and volatile oil is drawn, obtains aqueous solution B;
S33, aqueous solution B and water solution A are merged, after being concentrated to about 500mL, merge with alcohol extract, lyophilization becomes lyophilized powder;
S34, the volatile oil of step S31 gained adopted after beta-cyclodextrin inclusion compound be mixed and made into capsule with lyophilized powder.
Wherein, the described adjuvant making tablet is: binding agent be 80% alcoholic solution, filler be the microcrystalline Cellulose of 3% and micropowder silica gel, the disintegrating agent of 0.5% be the carboxymethyl starch sodium of 5%, lubricant is the magnesium stearate of 1.0%.
Wherein, Radix Inulae, Radix Sophorae Flavescentis, Fructus Rubi corchorifolii Immaturus coarse powder micronizing time are 80 minutes; The Rhizoma Kaempferiae coarse powder micronizing time is 60 minutes; Radix Inulae superfine powder particle diameter: D 50=25.12 μm; D 90=80.79 μm; Less than 75 μm micropowders account for 88.69%; Radix Sophorae Flavescentis superfine powder particle diameter: D 50=23.70 μm; D 90=69.97 μm; Less than 75 μm micropowders account for 91.29%; Fructus Rubi corchorifolii Immaturus superfine powder particle diameter: D 50=17.46 μm; D 90=49.74 μm; Less than 75 μm micropowders account for 96.68%; Rhizoma Kaempferiae superfine powder particle diameter: D 50=23.14 μm; D 90=46.72 μm; Less than 75 μm micropowders account for 98.22%.
Wherein, the process conditions of the vapor extraction method in described step S21 are the water adding 7 times amount, extract 6 hours, extract once.
Wherein, the process conditions of alcohol extraction in described step S22 are the ethanol adding 8 times amount, and concentration of alcohol is 50%, extract 1.5 hours, extract three times.
The present invention has following beneficial effect:
Looking into the superfine communication technique that dry soup superfine powder uses is based on destruction vegetable drug cell wall, promote that cellular content dissolves, the principle of diffusion, make composition in plant cell in vivo or in solvent stripping quantity and dissolution rate increase reach the object improving drug bioavailability, reduce dose, improve preparation quality.Use the impact of mechanical crusher, Chinese traditional powder that diameter is more than 3mm by collision, friction, shearing, grinding approach is crushed to the superfine powder of 10 ~ 75 μm, makes the cell-wall breaking ratio of medical material under this granularity condition be greater than 95%
Look into the technique that dry decoction particles agent uses and be respectively freeze drying process, beta-cyclodextrin inclusion compound technique, art for coating, while fully retaining effective ingredient, improve mouthfeel difference, carry inconvenience, take the problems such as not convenient.
Look into the technique that dry soup capsule uses and be respectively freeze drying process, beta-cyclodextrin inclusion compound technique, capsules preparation technique, while fully retaining effective ingredient, compensate for the deficiency of solid dosage forms, improve bioavailability, solve the problems such as mouthfeel difference.Under preserving the prerequisite of Traditional Curative Effect, look into dry soup submicron powder sheet and granule, capsule all solve the problem taking mouthfeel difference.Convenient for children and different age people are taken.Promote the stripping quantity in vivo of material in crude drug cell and dissolution rate, improve drug effect.
Detailed description of the invention
In order to make objects and advantages of the present invention clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Embodiment 1
This concrete enforcement adopts wet granule compression tablet, the interior addition that brings Selection In of disintegrating agent.
Filler kind and consumption are selected
On the basis of preliminary experiment, fixing disintegrating agent is 5% carboxymethyl starch sodium (CMS-Na), binding agent is 80% alcoholic solution, and lubricant is 1.0% magnesium stearate, and 0.5% micropowder silica gel and different proportion microcrystalline Cellulose (MCC) are filler.With label outward appearance, hardness and disintegration for inspection target, filter out optimum filler ratio.
Get prescription ratio four taste Radix Inulae superfine powder to mix homogeneously with filler and disintegrating agent, add appropriate adhesive soft material, cross 20 mesh sieves to granulate, wet granular was in 60 DEG C of baking oven inner dryings 40 minutes, take out, even with mix lubricant after 20 mesh sieve granulate, finally use the shallow round punch die tabletting that diameter is 10.0mm.With label outward appearance, hardness and disintegration for inspection target, filter out optimum filler ratio.
The selection of table 1 filler
Experimental result shows: when selection 3% microcrystalline Cellulose with, it is shorter that hardness is suitable for disintegration, and other index also meets the requirements.Therefore select 3% microcrystalline Cellulose and micropowder silica gel coupling to be filler
Disintegrating agent kind is selected
On the basis of preliminary experiment, fixing filler is 3% microcrystalline Cellulose (MCC) and 0.5% micropowder silica gel, and binding agent is 80% ethanol solution, and lubricant is 1.0% magnesium stearate.Starch, carboxymethyl starch sodium (CMS-Na), low-substituted hydroxypropyl cellulose (L-HPC) is selected to be disintegrating agent, the feed postition of disintegrating agent all adopts interior addition, get prescription ratio four taste Radix Inulae superfine powder to mix homogeneously with filler and disintegrating agent, add appropriate adhesive soft material, cross 20 mesh sieves to granulate, wet granular, in 60 DEG C of baking oven inner drying 40min, takes out, even with mix lubricant after 20 mesh sieve granulate, finally use the shallow round punch die tabletting that diameter is 10.0mm.With particle appearance, label outward appearance, hardness and disintegration for inspection target, filter out optimum disintegrating agent.Experimental result is in table 2.
The selection of table 2 disintegrating agent
Experimental result shows: when tablet prepared by above-mentioned three kinds of disintegrating agents, the equal smooth and beautiful appearance of label.When selecting L-HPC to be disintegrating agent, hardness is bad, and disintegration is longer.When selecting starch and CMS-Na to be disintegrating agent, nonhomogeneous hardness is little, and starch disintegration time is longer.Therefore select 5%CMS-Na to be disintegrating agent.
The selection of binding agent
On the basis of preliminary experiment, fixing filler is 3% microcrystalline Cellulose (MCC) and 0.5% micropowder silica gel, and disintegrating agent is 5% carboxymethyl starch sodium (CMS-Na), and lubricant is 1.0% magnesium stearate.80% ethanol, 10% starch slurry and 5%PVPK30 dehydrated alcohol is selected to be adhesive.With soft material viscosity, granulation difficulty, particle appearance for inspection target, filter out optimum adhesive.Experimental result is in table 3.
The selection of table 3 binding agent
Experimental result shows: select 5%PVPK 30when ethanol is adhesive, soft material stickiness is less, and grain forming is poor, and tablet hardness does not reach requirement.Select the soft material stickiness obtained by 10% starch slurry larger, granule is easy-formation not, when adopting 80% alcoholic solution moistening, made soft material stickiness is moderate, granule is complete and hardness suitable, label smooth and beautiful appearance, hardness and disintegration all can reach requirement, therefore selection 80% alcoholic solution is the adhesive in prescription.
80% ethanol different amounts granulating efficiency
The consumption of binding agent with 80% ethanol for test material, by a small amount of (to add to namely loose being as the criterion of loosing one's grip after soft material is held), moderate (hold agglomerating rear hands and pinch the dispersion that granulates to add to soft material and be as the criterion), volume (hold agglomerating rear hands and pinch into bulk to add to soft material and be separated into standard) 3 kinds of additions, be respectively used to soft material processed, each soft material granulation and compression tablet molding effect are compared.
The selection of table 4 binder dosage
Look into dry soup submicron powder sheet
Get prescription ratio four taste Radix Inulae superfine powder to mix homogeneously with 0.5% micropowder silica gel and 5%CMS-Na with 3% microcrystalline Cellulose, spray into 80% appropriate ethanol soft material, cross 20 mesh sieves to granulate, wet granular is in 60 DEG C of baking oven inner drying 40min, take out, mix homogeneously with 1.0% magnesium stearate after 20 mesh sieve granulate, finally use the shallow round punch die tabletting that diameter is 10.0mm.
Embodiment 2
Optimal extraction technology is studied
In raw material Study on extraction process, literature research is carried out to prescription 4 taste Chinese crude drug, different according to medical material effective ingredient physicochemical property, take the ethanol reflux extraction and the steam distillation that are easy to large production respectively, utilize orthogonal design, optimize optimised process.
Extraction by steam distillation volatile oil technique
Orthogonal trial: select to adopt water to be that solvent extracts, on affecting the factor amount of water of extraction process by water, digestion time (room temperature, normal pressure), decocting number of times, screen, following 3 levels of each factor design, orthogonal test (see table 5) is carried out by L9 (34), the effective elements of the medicine and physicochemical property in clear and definite every taste simultaneously, with oil mass of volatilizing for evaluation index, screening optimum extraction condition.
Table 5 orthogonal table
Fetch earth Common Aucklandia Root 70.00g, adds the water of the corresponding times amount of people by orthogonal array, and soak the corresponding time, then press Chinese Pharmacopoeia 2015 editions four determination of volatile oil methods and extract volatile oil, after extracting the stipulated time, according to extractor scale, read the volume orthogonal experiments of volatile oil in table 6
Table 6 orthogonal experiment intuitive analysis table
By known to the analysis of orthogonal experiments, each factor on the primary and secondary order that the extraction effect of total biological matrine affects is: the amount (doubly) that B digestion time > A adds water) > C extraction time, and obtain optimum extraction process: A 2b 3c 1, the amount namely added water 10 times, extracts 7 hours, extracts once.
By Radix Sophorae Flavescentis, Rhizoma Kaempferiae, Fructus Rubi corchorifolii Immaturus mixing, add the certain density ethanol of certain multiple, decoct certain number of times and time, extracting certain hour, take matrine content as index, and often experiment number in triplicate, measures the Radix Sophorae Flavescentis alkali number of each extraction conditions.
Orthogonal trial: according to several influence factor and the preliminary experiment of medical material alcohol extraction process, determine investigation factor and scope
Table 7 orthogonal table
Take Sophora flavescens coarse powder 40g respectively, totally 9 parts, test by orthogonal table.Using matrine content as the index investigated, adopt HPLC method to measure matrine content, the results are shown in Table 8,
Table 8 orthogonal experiment intuitive analysis table
By known to the analysis of orthogonal experiments, each factor on the primary and secondary order that the extraction effect of matrine content affects is: D (extraction time) > C (digestion time) > A (adding the amount of ethanol) > B (concentration of alcohol), and obtains optimum extraction process: A 2b 1c 2d 3, namely add the amount 8 times of ethanol, concentration of alcohol is 50%, extracts 1.5 hours, extracts three times.
Water extraction is carried out in medicinal residues mixing after the medicinal residues of alcohol extraction Radix Sophorae Flavescentis, Rhizoma Kaempferiae, Fructus Rubi corchorifolii Immaturus and Radix Inulae are extracted volatile oil, obtains paste-forming rate and polyoses content.
Orthogonal trial: select to adopt water to be that solvent extracts, on affecting the factor amount of water of extraction process by water, digestion time (room temperature, normal pressure), decocting number of times, screen, following 3 levels of each factor design, orthogonal test (see table 9) is carried out by L9 (34), simultaneously the effective elements of the medicine and physicochemical property in clear and definite every taste, with paste-forming rate and polyoses content for evaluation index, screening optimum extraction condition.
Table 9 orthogonal table
Select L10 (34) table, according to experimental design institute fixed condition, under operation repetitive condition, the two medicinal residues is added the water of certain multiple, decoct certain number of times and time, extract certain hour, often experiment number in triplicate, reflux lixiviate in hot bath, sucking filtration, collects filtrate; Rotary Evaporators concentrates, and adds ethanol, makes ethanol final volume reach more than 80%, hold over night.By gained precipitate at 4000r/min pelleted by centrifugation 15min, obtain Radix Inulae crude polysaccharides, the results are shown in Table 10.
Table 10 orthogonal experiment intuitive analysis table
By known to the analysis of orthogonal experiments, the primary and secondary order of each factor to paste-forming rate influential effect is: amount (doubly) > B digestion time (h) the > C extraction time that A adds water, and obtains optimum extraction process: A 3b 2c 1, the amount namely added water 12 times, extracts 1.5 hours, extracts once.
The clathrate process of beta-schardinger dextrin-
Enclose condition preferred:
The principal element affecting inclusion essential oil is the ratio of beta-schardinger dextrin-and volatile oil, enclose temperature, mixing time, and each factor gets a level respectively, carries out orthogonal test, screen optimum process condition with clathrate yield and inclusion rate for index.The factor level of clathrate process is in Table, and the factor level of clathrate process is in table 11 and table 12.
Orthogonal table 11
Table 12 orthogonal experiment intuitive analysis table
By known to the analysis of orthogonal experiments, each factor on the primary and secondary order that clathrate yield affects is: the ratio > C mixing time of B enclose temperature > A beta-schardinger dextrin-and volatile oil, and obtains optimum extraction process: A 2b 3c 1, i.e. temperature 70 C, the ratio of beta-schardinger dextrin-and volatile oil is 8: 1, mixing time one hour.
Freeze drying process
Aqueous solution 1 after aqueous solution 2 and above-mentioned volatile oil is drawn merges, and after being concentrated to certain volume, merge with alcohol extract, lyophilization becomes lyophilized powder.
Shown by drying mechanism analysis and single factor experiment research, when volume and volume change have considerable influence to freeze-drying time, material rehydration for cryodesiccation chamber's pressure, temperature of heating plate and material thickness.According to the production process of Radix Ginseng vacuum lyophilization, orthogonal design is adopted to be optimized combination to test.Choosing material thickness, temperature of heating plate and drying chamber pressure 3 factors is the orthogonal design factor, each predictor selection 5 levels, and establishment factor level table, in table 13
According to Three factors five level quadratic regression Orthogonal Experiment and Design, arrange to test for 25 times, orthogonal design scheme and result of the test are in table 14.
Analyze according to extreme difference Rj, secondary factors is followed successively by material thickness > temperature of heating plate > drying chamber pressure.By drawing orthogonal test result analysis, work as material thickness, temperature of heating plate and drying chamber pressure are respectively 3mm, 60 DEG C, and during 80Pa, dry rate is maximum.
Work as material thickness, temperature of heating plate and drying chamber pressure are respectively 3mm, 60 DEG C, during 80Pa, the aqueous solution 1 after aqueous solution 2 and above-mentioned volatile oil is drawn is merged, after being concentrated to certain volume, merge with alcohol extract and decoct, maintain boiling 5min, while hot centrifugal 20min under 3500rpm/min condition, be evaporated to containing crude drug amount 1g/ml, concentrated solution obtains freeze-dried powder at-45 DEG C of lyophilization 24h after-20 DEG C of refrigerator freezing 24h.
Preparations shaping technical study
Prepare coated granule: the volatile oil extracted by beta-cyclodextrin inclusion compound mixes coated granule processed with lyophilized powder
This art for coating is specially adapted to bitter in the mouth, is difficult to the granule swallowed, and the granule after coating masks the bitterness of medicine, is easy to swallow, and as added a little correctives, effect is better.This product looks into this method coating of dry decoction particles, masks the bitterness of medicine, obtains gratifying effect.
The basic prescription of coating:
6%HPMC ethanol 16.8kg, Tween 80 0.384kg, Polyethylene Glycol ethanol 0.48kg, Pulvis Talci, 0.65kg, ethanol 30kg.
Coating solution is prepared:
Accurately take HPMC, put in appropriate containers, add ethanol moistening after mix with the adjuvant such as other Icing Sugar, use vertical colloid mill defibrination, make it to become uniform liquid, can be used for the coating of 50kg granule.
Coating operations:
Taken out by granule and put in exsiccator and cool, with 20 orders and 42 mesh sieve granulate, getting by 20 orders is not conforming particle by the granule of 42 mesh sieves.Before coating, granule is put in Mixers with Multi-direction Movement and mix, to ensure the uniformity of sample.First preheating coating pan (rotating speed 32r/min, hot-blast outlet temperature 70 C), then the granule conformed to quality requirements is put in coating pan, start coating pan, granule is preheated to 60 DEG C, start pulp shooting machine (spouting liquid 100ml/min), make coating solution evenly spray into the particle surface of rotation, with the hot air drying of 60 DEG C.Can continued operation in the NA situation of granule, until coating solution has sprayed.
Moisture-resistant test
By the granule of non-coating and bag HPMC clothing, being exposed in air with putting indoor, conventionally measuring granule change of moisture content, the results are shown in subordinate list 15.
As can be seen from the table, along with the change of open-assembly time in atmosphere, coated granule moisture content change is little, but does not have the moisture generation significant change of coated granule, obviously increases.
Whether table 15 granule coating places the change (%) of rear water content
Look into dry decoction particles agent
Radix Inulae coarse powder extraction by steam distillation volatile oil, the another device of the aqueous solution after distillation is collected.Be designated as aqueous solution (1), other three tastes medicines of alcohol extraction: Radix Sophorae Flavescentis, Rhizoma Kaempferiae, Fructus Rubi corchorifolii Immaturus, the another device of alcohol extract is collected.Water extraction is carried out in the medicinal residues mixing of the medicinal residues of alcohol extraction and volatile oil is drawn.Be designated as aqueous solution (2), the aqueous solution (1) after aqueous solution (2) and above-mentioned volatile oil is drawn merges, and after being concentrated to certain volume, merge with alcohol extract, lyophilization becomes lyophilized powder.The volatile oil that beta-cyclodextrin inclusion compound said extracted goes out.The volatile oil extracted by beta-cyclodextrin inclusion compound again mixes coated granule processed with lyophilized powder.
Embodiment 3
Extraction by steam distillation volatile oil technique
Orthogonal trial: select to adopt water to be that solvent extracts, on affecting the factor amount of water of extraction process by water, digestion time (room temperature, normal pressure), decocting number of times, screen, following 3 levels of each factor design, orthogonal test (see table 16) is carried out by L9 (34), the effective elements of the medicine and physicochemical property in clear and definite every taste simultaneously, with oil mass of volatilizing for evaluation index, screening optimum extraction condition.
Table 16 orthogonal table
Fetch earth Radix Aucklandiae 70.00g, adds the water of the corresponding times amount of people by orthogonal array, and soak the corresponding time, then press Chinese Pharmacopoeia 2015 editions four determination of volatile oil methods and extract volatile oil, after extracting the stipulated time, according to extractor scale, read the volume orthogonal experiments of volatile oil in table 17
Table 17 orthogonal experiment intuitive analysis table
By known to the analysis of orthogonal experiments, each factor on the primary and secondary order that the extraction effect of volatile oil affects is: the amount (doubly) that B digestion time > A adds water) > C extraction time, and obtain optimum extraction process: A 2b 3c 1, the amount namely added water 7 times, extracts 6 hours, extracts once.
Alcohol extraction matrine
By Radix Sophorae Flavescentis, Rhizoma Kaempferiae, Fructus Rubi corchorifolii Immaturus mixing, add the certain density ethanol of certain multiple, decoct certain number of times and time, extracting certain hour, take matrine content as index, and often experiment number in triplicate, measures the Radix Sophorae Flavescentis alkali number of each extraction conditions.
Orthogonal trial: according to several influence factor and the preliminary experiment of medical material alcohol extraction process, determine investigation factor and scope
Table 18 orthogonal table
Take Sophora flavescens coarse powder 40g respectively, totally 9 parts, test by orthogonal table.Using matrine content as the index investigated, adopt HPLC method to measure matrine content, the results are shown in Table 19.
Table 19 orthogonal experiment intuitive analysis table
By known to the analysis of orthogonal experiments, each factor on the primary and secondary order that the extraction effect of matrine affects is: D (extraction time) > C (digestion time) > A (adding the amount of ethanol) > B (concentration of alcohol), and obtains optimum extraction process: A 2b 1c 2d 3, namely add the amount 8 times of ethanol, concentration of alcohol is 50%, extracts 1.5 hours, extracts three times.
The medicinal residues of alcohol extraction Radix Sophorae Flavescentis, Rhizoma Kaempferiae, Fructus Rubi corchorifolii Immaturus are mixed with the Radix Inulae medicinal residues extracted after volatile oil and carries out water extraction, obtain paste-forming rate and polyoses content
Orthogonal trial: select to adopt water to be that solvent extracts, on affecting the factor amount of water of extraction process by water, digestion time (room temperature, normal pressure), decocting number of times, screen, following 3 levels of each factor design, orthogonal test (see table 20) is carried out by L9 (34), simultaneously the effective elements of the medicine and physicochemical property in clear and definite every taste, with paste-forming rate and polyoses content for evaluation index, screening optimum extraction condition.
Table 20 orthogonal table
Select L9 (34) table, according to experimental design institute fixed condition, under operation repetitive condition, the two medicinal residues is added the water of certain multiple, decoct certain number of times and time, extract certain hour, filter, be condensed into paste, often experiment number in triplicate, the results are shown in Table 21.
Table 21 orthogonal experiment intuitive analysis table
By known to the analysis of orthogonal experiments, the primary and secondary order of each factor to paste-forming rate and polyoses content influential effect is: amount (doubly) > B digestion time (h) the > C extraction time that A adds water, and obtains optimum extraction process: A 3b 2c 1, the amount namely added water 12 times, extracts 1.5 hours, extracts once.
The clathrate process of beta-schardinger dextrin-
Enclose condition preferred:
The principal element affecting inclusion essential oil is the ratio of beta-schardinger dextrin-and volatile oil, enclose temperature, mixing time, and each factor gets a level respectively, carries out orthogonal test, screen optimum process condition with clathrate yield and inclusion rate for index.The each factor level of clathrate process is in Table, and orthogonal experiments is in table 22 table 23.
Table 22 orthogonal table
Table 23 orthogonal experiment intuitive analysis table
By known to the analysis of orthogonal experiments, each factor on the primary and secondary order that clathrate yield affects is: the ratio > C mixing time of B enclose temperature > A volatile oil and beta-schardinger dextrin-, and obtains optimum extraction process: A 2b 3c 1, i.e. temperature 70 C, ratio is 8: 1 stirring one hour.
Freeze drying process
Aqueous solution 1 after aqueous solution 2 and above-mentioned volatile oil is drawn merges, and after being concentrated to certain volume, merge with alcohol extract, lyophilization becomes lyophilized powder.
Shown by drying mechanism analysis and single factor experiment research, when volume and volume change have considerable influence to freeze-drying time, material rehydration for cryodesiccation chamber's pressure, temperature of heating plate and material thickness.According to the production process of Radix Ginseng vacuum lyophilization, orthogonal design is adopted to be optimized combination to test.Choosing material thickness, temperature of heating plate and drying chamber pressure 3 factors is the orthogonal design factor, each predictor selection 5 levels, and establishment factor level table, in table 24
According to Three factors five level quadratic regression Orthogonal Experiment and Design, arrange to test for 25 times, orthogonal design scheme and result of the test are in table 25.
Analyze according to extreme difference Rj, secondary factors is followed successively by material thickness > temperature of heating plate > drying chamber pressure.By drawing orthogonal test result analysis, work as material thickness, temperature of heating plate and drying chamber pressure are respectively 3mm, 60 DEG C, and during 80Pa, dry rate is maximum.
Work as material thickness, temperature of heating plate and drying chamber pressure are respectively 3mm, 60 DEG C, during 80Pa, the aqueous solution 1 after aqueous solution 2 and above-mentioned volatile oil is drawn is merged, after being concentrated to certain volume, merge with alcohol extract and decoct, maintain boiling 5min, while hot centrifugal 20min under 3500rpm/min condition, be evaporated to containing crude drug amount 1g/ml, concentrated solution obtains freeze-dried powder at-45 DEG C of lyophilization 24h after-20 DEG C of refrigerator freezing 24h.
Preparations shaping technical study
Preparation: the volatile oil extracted by beta-cyclodextrin inclusion compound mixes with lyophilized powder and incapsulates into capsule.
Look into dry soup capsule
The coarse powder of Radix Inulae coarse powder extracts volatile oil by vapor extraction method, and the another device of the aqueous solution after distillation is collected.Be designated as aqueous solution (1), other three tastes medicines of alcohol extraction: Radix Sophorae Flavescentis, Rhizoma Kaempferiae, Fructus Rubi corchorifolii Immaturus, the another device of alcohol extract is collected.Water extraction is carried out in the medicinal residues mixing of the medicinal residues of alcohol extraction and volatile oil is drawn.Be designated as aqueous solution (2), the aqueous solution (1) after aqueous solution (2) and above-mentioned volatile oil is drawn merges, and after being concentrated to certain volume, merge with alcohol extract, lyophilization becomes lyophilized powder.The volatile oil that beta-cyclodextrin inclusion compound said extracted goes out.The volatile oil again beta-cyclodextrin inclusion compound extracted and lyophilized powder mixing glue wafer.
Look into dry soup submicron powder sheet, granule, capsule method of quality control as follows:
Look into the quality examination of dry soup submicron powder sheet:
Appearance character: tablet surface uniform color, bright and clean, without assorted speckle, foreign, tablet is qualified.
Tablet weight variation: it is 5.1% that 1 tablet weight variation does not meet States Pharmacopoeia specifications, and all the other all meet States Pharmacopoeia specifications 5%, and tablet is qualified.
Look into the quality examination of dry decoction particles agent:
Granularity: the two sieve algoscopys adopting granularity and particle size distribution method, the weighed weight of thing of getting it filled, put in upper strata (aperture is large) the medicine sieve under this dosage form or kind item (being furnished with closely sealed receiving vessel under the sieve of lower floor), level is kept to sieve, left and right come and go, sieve limit, limit pats 3 minutes, get not by large aperture sieve and by small-bore sieve granule and powder, weighed weight, calculates its proportion (%).Must not more than 15%. by No. 1 sieve and the summation by No. 5 sieves
Loss on drying: in 80 DEG C of drying under reduced pressure to constant weight, less loss weight must not be less than 2.0%.
Melting: get test sample 10 grams, heating water 200ml, stir 5 minutes, observe immediately, sol particle should all be dissolved or slight haze.
Look into the quality examination of dry soup capsule:
Appearance character: capsule is complete bright and clean, soap-free emulsion polymeization, distortion, softgel shell fracture phenomena, without macroscopic exogenous impurity.
Content uniformity: specify according under the Pharmacopoeia of the People's Republic of China 2015 editions four capsule content uniformity items, Chinese medicine capsules content uniformity limit is ± 10.0%.
Disintegration: get test sample 6, be placed in the glass tubing of hanging basket, enable lift disintegration tester and check, each capsule should whole disintegrate in 30 minutes, does not have disintegrate, separately should get one group of 6 retrial, all should conform with the regulations if any one.
Look into the assay of the isoalantolactone in dry soup
The preparation of reference substance solution: get isoalantolactone reference substance appropriate, accurately weighed, add methanol make every 1ml about containing 50 μ g solution and get final product.
The preparation of need testing solution: get this product in right amount, porphyrize, gets 0.3g accurately weighed, and put in tool plug conical flask, precision adds methanol 25ml, close plug, weighed weight, placement is spent the night, and supersound process 30 minutes, lets cool, weighed weight, supplies the weight of less loss, shakes up with methanol, filter, and gets subsequent filtrate and both obtains.
Chromatographic condition
Chromatographic column: YMC-PACKODS (4.6mm × 250mm, 5 μm) column temperature: 25 DEG C
Mobile phase: acetonitrile-0.04% phosphoric acid solution (50: 50) determined wavelength: 210nm, sample size: 10 μ l
Look into the assay of the Radix Sophorae Flavescentis alkaloid in dry soup
The preparation of reference substance solution: get oxymatrine reference substance, N-oxysophocarpine reference substance is appropriate, accurately weighed, the mixed solution adding acetonitrile-dehydrated alcohol (80: 20) make respectively every 1 milliliter about containing oxymatrine 0.0438mg, N-oxysophocarpine 0.0142mg solution and get final product.
The preparation of need testing solution: take 1 part of tablet powder 0.3g, accurately weighed, put in conical flask, add strong ammonia solution 0.5mL, chloroform 20mL, shakes up, weigh, after placing half an hour, ultrasonic 40min, lets cool, weight is supplied with chloroform, filter, get subsequent filtrate 5mL, cross neutral alumina (100 ~ 200 orders, 5g, internal diameter 1cm), use chloroform, chloroform successively: each 20mL eluting of methanol (7: 3), merge eluent, evaporate to dryness, use appropriate anhydrous alcohol solution, standardize solution, in 10mL volumetric flask, to obtain final product.
Chromatographic condition: ThermoSCIENTIFICUltiMate3000 chromatographic column is UltimteXB-NH2 (250 × 4.6mm, 5 μm)
Mobile phase: acetonitrile: dehydrated alcohol: 3% phosphoric acid water (80: 10: 10)
Flow velocity: 1mlmin-1
Sample size: 20 μ L
Column temperature: 30 DEG C
Determined wavelength: 210nm
Sample granularity measures: adopt laser particle analyzer to measure the granularity of superfine powder
The superfine grinding method of Radix Inulae, Radix Sophorae Flavescentis, Fructus Rubi corchorifolii Immaturus, Rhizoma Kaempferiae medical material is set up
Radix Inulae pulverizing medicinal materials is become coarse powder, use Baily pulverizing mill (BFM-6A) that Radix Inulae coarse powder is carried out micronizing, by the relation between the different grinding time of MALVERNNano-s type laser fineness gage Observe and measure and superfine powder particle diameter, in conjunction with OLYMPUS (BX41) observation by light microscope powder body cellular morphology, optimize best superfine grinding method.
The superfine grinding method of Radix Sophorae Flavescentis, Fructus Rubi corchorifolii Immaturus, Rhizoma Kaempferiae medical material is preferably identical with preferred Radix Inulae superfine grinding method.
Result: Radix Inulae, Radix Sophorae Flavescentis, Fructus Rubi corchorifolii Immaturus coarse powder micronizing time are 80 minutes; The Rhizoma Kaempferiae coarse powder micronizing time is 60 minutes.
Radix Inulae superfine powder particle diameter: D 50=25.12 μm; D 90=80.79 μm; Less than 75 μm micropowders account for 88.69%;
Radix Sophorae Flavescentis superfine powder particle diameter: D 50=23.70 μm; D 90=69.97 μm; Less than 75 μm micropowders account for 91.29%;
Fructus Rubi corchorifolii Immaturus superfine powder particle diameter: D 50=17.46 μm; D 90=49.74 μm; Less than 75 μm micropowders account for 96.68%;
Rhizoma Kaempferiae superfine powder particle diameter: D 50=23.14 μm; D 90=46.72 μm; Less than 75 μm micropowders account for 98.22%.
The comparison of alantolactone content
Take 3 batches of medical material superfine powder and common flour, by 7.4 below legal system available test products and by the content measuring alantolactone under 7.4 lower chromatographic conditions.
Dissolution compares employing pulpous state paddling process and measures dissolution, add water 900mL in stripping rotor, constant temperature (37 ± 0.5) DEG C, precision takes each 5g of Radix Inulae common flour superfine powder and puts in stripping rotor respectively, rotating speed 75rmin-1, starts timing, respectively at 1,3,5,10,15,20,30,40,50,60min respectively samples in right amount, filter through 0.45 μm of microporous filter membrane, after filtration, supplement isothermal equal-volume water and filter cake thing immediately.Precision measures appropriate subsequent filtrate and measures by above-mentioned chromatographic condition, compares the dissolution of alantolactone in Radix Inulae superfine powder and common flour different time dissolution fluid.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.

Claims (7)

1. a preparation method for dry soup superfine powder looked into by mongolian medicine, it is characterized in that, comprises the steps:
S11, Radix Inulae, Radix Sophorae Flavescentis, Fructus Rubi corchorifolii Immaturus, Rhizoma Kaempferiae are ground into coarse powder after, use Baily pulverizing mill (BFM-6A) gained coarse powder is carried out micronizing respectively;
S12, in mass ratio 4: 4: 2: 1 take Radix Inulae, Radix Sophorae Flavescentis, Fructus Rubi corchorifolii Immaturus, Rhizoma Kaempferiae Homogeneous phase mixing, add filler and disintegrating agent, add binding agent again after mixing;
S13, the soft material of gained is crossed 20 mesh sieves, the wet granular made, be placed in 60 DEG C of baking ovens, dry 40min, after 20 mesh sieve granulate, after adding lubricant, use diameter to be the shallow round punch die tabletting of 10 millimeters.
2. a preparation method for dry decoction particles looked into by mongolian medicine, it is characterized in that, comprises the steps:
S21, in mass ratio 4: 4: 2: 1 take Radix Inulae, Radix Sophorae Flavescentis, Fructus Rubi corchorifolii Immaturus and Rhizoma Kaempferiae, and Radix Inulae coarse powder vapor extraction method extracts volatile oil, and the another device of the aqueous solution after distillation is collected, and obtains volatile oil and water solution A;
The coarse powder of S22, alcohol extraction Radix Sophorae Flavescentis, Rhizoma Kaempferiae, Fructus Rubi corchorifolii Immaturus, the another device of alcohol extract is collected, and reclaim ethanol, extracting solution is separately deposited, and water extraction is carried out in the medicinal residues mixing of the medicinal residues of alcohol extraction and volatile oil is drawn, obtains aqueous solution B,
S23, aqueous solution B and water solution A to be merged, after being concentrated to certain volume, merge with alcohol extract, maintain boiling 5min, centrifugal 20min under 3500rpm/min condition while hot, be evaporated to containing crude drug amount 1g/ml, concentrated solution obtains freeze-dried powder at-45 DEG C of lyophilization 24h after-20 DEG C of refrigerator freezing 24h;
S24, the volatile oil of step S21 gained adopted after beta-cyclodextrin inclusion compound with lyophilized powder mixing granulation, coated granule processed.
3. a preparation method for dry soup capsule looked into by mongolian medicine, it is characterized in that, comprises the steps:
S31, in mass ratio 4: 4: 2: 1 take Radix Inulae, Radix Sophorae Flavescentis, Fructus Rubi corchorifolii Immaturus and Rhizoma Kaempferiae, extract volatile oil by vapor extraction method, and the another device of the aqueous solution after distillation is collected, and obtains volatile oil and water solution A;
The coarse powder of S32, alcohol extraction Radix Sophorae Flavescentis, Rhizoma Kaempferiae, Fructus Rubi corchorifolii Immaturus, the another device of alcohol extract is collected, and reclaim ethanol, extracting solution is separately deposited, and water extraction is carried out in the medicinal residues mixing of the medicinal residues of alcohol extraction and volatile oil is drawn, obtains aqueous solution B;
S33, aqueous solution B and water solution A are merged, after being concentrated to 500mL, merge with alcohol extract, lyophilization becomes lyophilized powder
S34, the volatile oil of step S31 gained adopted after beta-cyclodextrin inclusion compound be mixed and made into capsule with lyophilized powder.
4. the preparation method of dry soup superfine powder looked into by a kind of mongolian medicine according to right 1, it is characterized in that, the described adjuvant making tablet is: binding agent be 80% alcoholic solution, filler be the microcrystalline Cellulose of 3% and micropowder silica gel, the disintegrating agent of 0.5% be the carboxymethyl starch sodium of 5%, lubricant is the magnesium stearate of 1.0%.
5. the preparation method of dry soup superfine powder looked into by a kind of mongolian medicine according to right 1, it is characterized in that, Radix Inulae, Radix Sophorae Flavescentis, Fructus Rubi corchorifolii Immaturus coarse powder micronizing time are 80 minutes; The Rhizoma Kaempferiae coarse powder micronizing time is 60 minutes; Radix Inulae superfine powder particle diameter: D 50=25.12 μm; D 90=80.79 μm; Less than 75 μm micropowders account for 88.69%; Radix Sophorae Flavescentis superfine powder particle diameter: D 50=23.70 μm; D 90=69.97 μm; Less than 75 μm micropowders account for 91.29%; Fructus Rubi corchorifolii Immaturus superfine powder particle diameter: D 50=17.46 μm; D 90=49.74 μm; Less than 75 μm micropowders account for 96.68%; Rhizoma Kaempferiae superfine powder particle diameter: D 50=23.14 μm; D 90=46.72 μm; Less than 75 μm micropowders account for 98.22%.
6. the preparation method of dry soup superfine powder looked into by a kind of mongolian medicine according to right 1, it is characterized in that, the process conditions of the vapor extraction method in described step S21 are the water adding 7 times amount, extracts 6 hours, extracts once.
7. the preparation method of dry soup superfine powder looked into by a kind of mongolian medicine according to right 1, it is characterized in that, the process conditions of alcohol extraction in described step S22 are the ethanol adding 8 times amount, and concentration of alcohol is 50%, extracts 1.5 hours, extracts twice.
CN201510990820.4A 2015-12-22 2015-12-22 Preparation method for Mongolian four-species elecampane inula root decoction superfine powder tablets, granules and capsules Pending CN105497722A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510990820.4A CN105497722A (en) 2015-12-22 2015-12-22 Preparation method for Mongolian four-species elecampane inula root decoction superfine powder tablets, granules and capsules

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510990820.4A CN105497722A (en) 2015-12-22 2015-12-22 Preparation method for Mongolian four-species elecampane inula root decoction superfine powder tablets, granules and capsules

Publications (1)

Publication Number Publication Date
CN105497722A true CN105497722A (en) 2016-04-20

Family

ID=55706274

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510990820.4A Pending CN105497722A (en) 2015-12-22 2015-12-22 Preparation method for Mongolian four-species elecampane inula root decoction superfine powder tablets, granules and capsules

Country Status (1)

Country Link
CN (1) CN105497722A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108210811A (en) * 2017-12-29 2018-06-29 内蒙古医科大学 A kind of anaesthetic looks into the preparation method of dry soup pellet and soup mixture
CN113332248A (en) * 2021-06-02 2021-09-03 祈蒙股份有限公司 Kaempferia galanga composition particles and preparation process thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1374111A (en) * 2002-02-27 2002-10-16 内蒙古锡林郭勒盟蒙医研究所 New prepn process of Manu as one traditional Mongolian medicine

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1374111A (en) * 2002-02-27 2002-10-16 内蒙古锡林郭勒盟蒙医研究所 New prepn process of Manu as one traditional Mongolian medicine

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108210811A (en) * 2017-12-29 2018-06-29 内蒙古医科大学 A kind of anaesthetic looks into the preparation method of dry soup pellet and soup mixture
CN113332248A (en) * 2021-06-02 2021-09-03 祈蒙股份有限公司 Kaempferia galanga composition particles and preparation process thereof

Similar Documents

Publication Publication Date Title
CN102631377A (en) Cordyceps sinensis freeze-dried nano powder tablet and preparation method thereof
CN101057926B (en) Gynaecologic menstruation regulating preparation for treating gynecopathy and its preparation method and detection method
CN102423352A (en) Chinese medicinal granules for treating cardio-cerebrovascular diseases
CN104887771A (en) Medicinal preparation for treating nerve-root cervical spondylopathy, and preparation method and quality detection method thereof
CN102114075B (en) Serial Chinese medicinal preparation for treating child common cold and preparation process and detection method thereof
CN100477985C (en) Naoxinqing Chinese medicine dispersible tablet and its preparing process
CN105497722A (en) Preparation method for Mongolian four-species elecampane inula root decoction superfine powder tablets, granules and capsules
CN103550164B (en) A kind of GUIPI WAN (micropill) of replenishing QI to invigorate the spleen
CN101972297A (en) Liver health tablet
CN102772454B (en) Brucea javanica oil dry emulsion capsule and preparation method thereof
CN103316056A (en) Radix isatidis coating dispersible tablet and preparation method thereof
CN1329062C (en) Method for preparing medicine for treating cataclasis and soft tissue injury
CN100562323C (en) A kind of pharmaceutical composition for the treatment of hysteromyoma and preparation method thereof
CN101869644B (en) Dark-skinned chicken dispersible tablet and preparation process thereof
CN102048866A (en) Toxin-expelling face-nourishing pills and preparation method thereof
CN101279055A (en) Novel therapeutic use of ginseng and astragali pollen preparations and quality control method
CN112603973A (en) Improved preparation method of pharmaceutical composition for treating lung cough
CN1931337A (en) Bock greenbrier rhizome micro pill and its prepn process
CN1695713B (en) Medication for treating diabetes and preparation method and quality control method
CN104435119B (en) Fructus schizandrae total lignans active component solid dispersions and preparation method thereof
CN100515412C (en) Chinese medicinal tablet and preparation method thereof
CN103520317B (en) Xinxuening sustained release tablet for treating cardiovascular diseases and preparation method thereof
CN112569281B (en) Yiqing composition and preparation method thereof
CN106692230A (en) Preparation method of herba lysimachiae granules
CN103356796A (en) Blood stasis removing particles and preparation method thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20160420

RJ01 Rejection of invention patent application after publication