CN105561275B - A kind of preparation method of cough-relieving tablet - Google Patents

A kind of preparation method of cough-relieving tablet Download PDF

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CN105561275B
CN105561275B CN201610058942.4A CN201610058942A CN105561275B CN 105561275 B CN105561275 B CN 105561275B CN 201610058942 A CN201610058942 A CN 201610058942A CN 105561275 B CN105561275 B CN 105561275B
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ethanol
extract
dried
preparation
cough
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CN105561275A (en
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伍伟成
赵瑞胜
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Special Pharmaceutical Group Ltd By Share Ltd
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Special Pharmaceutical Group Ltd By Share Ltd
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    • 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)
    • A61K36/9068—Zingiber, e.g. garden ginger
    • A—HUMAN NECESSITIES
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    • 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)
    • A61K36/23—Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
    • A—HUMAN NECESSITIES
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    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/34—Campanulaceae (Bellflower family)
    • A61K36/346—Platycodon
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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • 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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    • A61K36/185—Magnoliopsida (dicotyledons)
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    • A61K36/484—Glycyrrhiza (licorice)
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    • A61K36/185—Magnoliopsida (dicotyledons)
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    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/57—Magnoliaceae (Magnolia family)
    • A—HUMAN NECESSITIES
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    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/66—Papaveraceae (Poppy family), e.g. bloodroot
    • A—HUMAN NECESSITIES
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    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/75—Rutaceae (Rue family)
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    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/79—Schisandraceae (Schisandra family)
    • A—HUMAN NECESSITIES
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    • A61K36/18—Magnoliophyta (angiosperms)
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    • A61K36/904—Stemonaceae (Stemona family), e.g. croomia
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    • A61K9/20—Pills, tablets, discs, rods
    • A61K9/28—Dragees; Coated pills or tablets, e.g. with film or compression coating
    • A61K9/2806—Coating materials
    • A61K9/2833—Organic macromolecular compounds
    • A61K9/286—Polysaccharides, e.g. gums; Cyclodextrin
    • A61K9/2866—Cellulose; Cellulose derivatives, e.g. hydroxypropyl methylcellulose
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    • 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
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    • A61K2236/30—Extraction of the material
    • A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
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    • A61K2236/30—Extraction of the material
    • A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50—Methods involving additional extraction steps
    • A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying

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Abstract

A kind of cough-relieving method for preparing tablet thereof, is related to the field of Chinese medicines.Comprise the following steps：(1) preparation of .I extract powders, the preparation of (2) .II extract powders, (3). the preparation of tablet.In the preparation method of the cough-relieving tablet of the present invention, the drying means of medicinal extract greatly shortens can drying time to be dried stage by stage, and the impact to active ingredient in medicine is reduced, and improves therapeutic effect.

Description

A kind of preparation method of cough-relieving tablet
Technical field
The present invention relates to a kind of preparation method of cough-relieving tablet.
Background technology
As atmosphere pollution is increasingly serious, the incidence of haze is also increasing.Respiratory system of the dirty air to human body Injury is huge, counts according to national health department, and 300,000,000 people infection respiratory disease, wherein cough patients are often close on up to by China More than 5000 ten thousand.Every winter, air are cold, and haze is more serious, and cough patients' quantity further increases.Chronic cough patient be also easy to Cause the complication such as hypertension, cerebral anoxia, pulmonary heart disease.
Cough-relieving treasured piece is that Mr. that Taishan distinguished veteran doctors of TCM Liu obtains is formulated in the Chinese patent drug of 1915,2010 editions pharmacopeia Include, its composition be pappy shell medicinal extract, aster, Radix Glycyrrhizae, Exocarpium Citri Rubrum, the tuber of stemona, the fruit of Chinese magnoliavine, balloonflower root, Fructus Aurantii, dried orange peel, schizonepeta, the root of purple-flowered peucedanum, Rhizoma zingiberis, ammonium chloride, peppermint oil dementholized etc..Full side's monarch coordinates appropriate, complements each other, and has played relieving exterior syndrome and dispelling cold, a surname's lung eliminating phlegm, Beneficial lung qi supports the work(of lung yin, plays reason lung eliminating the phlegm, relieving cough and asthma function.
Chinese invention patent (101862442 B of Authorization Notice No. CN) is disclosed the invention discloses a kind of cough relief traditional Chinese medicine Composition and its preparation method, precious using traditional herbal medicine cough-relieving, Jing is modern to be extracted for example hot backflow of manufacture craft, economic benefits and social benefits and steams Send out, be spray-dried etc. and making medicinal extract, and being configured to corresponding formulation.Wherein to taking spray drying in the preparation technology of medicinal extract Method, which is higher to equipment requirement, can cause the increase of production cost.
The content of the invention
For above-mentioned technical problem, the present invention provides a kind of preparation method of cough-relieving tablet, comprises the following steps：
(1) preparation of .I extract powders：The pappy shell of 150～130kg is extracted into 2 with the alcohol reflux of 1400～1800L Secondary, each 4h merges extract, is vacuum dried stage by stage and crushes, obtain I medicinal extract comminuted powders after recovery ethanol, concentration；
(2) preparation of .II extract powders：Weigh Exocarpium Citri Rubrum 75～100kg of meal, balloonflower root 100～150kg of meal, Fructus Aurantii thick 10～30kg of powder, the tuber of stemona 75～100kg of meal, the fruit of Chinese magnoliavine 10～30kg of meal, dried orange peel 100～150kg of meal, rhizoma zingiberis meal 10 ～30kg, schizonepeta 50～80kg of meal, the root of purple-flowered peucedanum 150～200kg of meal, with 60 ± 5 DEG C of the ethanol of 8 times of weight extract 2 times, often Secondary 48h, merges extract, reclaims ethanol, is concentrated to give II extractum As；Weigh 100～150kg of aster, 350～400kg of Radix Glycyrrhizae net Medicinal material, puts in multi-function extractor, boils extraction 2 times with the water of 8 times of weight, and each 2h merges extract, is concentrated to give No. II leaching Cream B；It is vacuum dried stage by stage and crushes after the II extractum As are well mixed with II medicinal extract B, obtains the crushing of II medicinal extract Powder；
(3). the preparation of tablet：By the I medicinal extract 65～90kg of comminuted powder, cough-relieving treasured piece II cream comminuted powder 161～ 231kg, ammonium chloride 150kg～180kg are pelletized after being mixed with pharmaceutically acceptable auxiliary material, are added 1kg peppermint oil dementholizeds with lubrication After agent always mixes 20min, compressing tablet, coating obtain the cough-relieving tablet.
Further, it is vacuum dried and crushes in the step (1) and is：I concentrates are pumped into into material pot, dextrin is added 0.3kg, unlatching are uniformly mixed, and opening heating makes material be incubated at 60～80 DEG C；First paragraph temperature 110～120 is set DEG C, 90～100 DEG C of second segment temperature, 10～30 DEG C of the 3rd section of temperature, vacuum -0.1MPa, arranging feed pump charging rate is 90～160kg/h, 0.32～0.48m/min of crawler track speeds, the crawler belt are through the equal used time 18min of above-mentioned each section of temperature；Open Vacuum, heating are opened, after requirement to be achieved, feed pump is opened and is dried, open when material to be dried is into the 3rd section of nearly discharging Lock material and pulverizer, 80 mesh stainless steel mesh of Jing are crushed.
Further, it is vacuum dried and crushes in the step (2) and is：The II extractum As are mixed with II medicinal extract B Material pot is pumped into after uniform, adding 30～50kg of talcum powder, unlatching to be uniformly mixed, and open heating makes material 60～80 DEG C insulation；120～130 DEG C of first paragraph temperature is set, 100～110 DEG C of second segment temperature, 10～30 DEG C of the 3rd section of temperature, vacuum Degree -0.1MPa, arranges feed pump charging rate for 90～160kg/h, 0.32～0.48m/min of crawler track speeds, the crawler belt Jing The equal used time 18min of above-mentioned each section of temperature, the crawler belt are crossed through the equal used time 18min of above-mentioned each section of temperature；Open vacuum, add Heat, after requirement to be achieved, opens feed pump and is dried, open lock material and crushing when material to be dried is into the 3rd section of nearly discharging Machine, 80 mesh stainless steel mesh of Jing are crushed.
Specifically, step (1) and (2) middle extraction ethanol are the ethanol that percent by volume is 60%.
Specifically, the recovery ethanol in the step (1) and (2) is：Extract after merging is proceeded to into alcohol distillation column Ethanol is reclaimed, is stopped when 100～102 DEG C are reached to distillation temperature in the kettle, obtain liquid and reclaim the ethanol of gained.
Specifically, the concentration in the step (1) and (2) is：Control steam pressure≤0.2MPa, vacuum be one effect- 0.04～-0.08MPa, two effect -0.06～-0.08MPa, be concentrated into extract at 50 DEG C ± 2 DEG C relative density be 1.20～ 1.30。
The pharmaceutically acceptable auxiliary material can be excipient, adhesive, disintegrant, lubricant etc..The excipient Starch, Icing Sugar, dextrin, lactose, amylum pregelatinisatum, microcrystalline cellulose, inorganic salts can be included (such as calcium sulfate, calcium monohydrogen phosphate, medicine With calcium carbonate etc.), mannitol etc..Described adhesive can include distilled water, ethanol, starch slurry, sodium carboxymethylcellulose, hydroxypropyl Base cellulose, methylcellulose, ethyl cellulose, Hydroxypropyl methylcellulose, PVP, gelatin solution etc..Disintegrant Dried starch, sodium carboxymethyl starch, low-substituted hydroxypropyl cellulose, cross linked polyvinyl pyrrolidone, cross-linked carboxymethyl can be included Sodium cellulosate, gas-producing disintegrant etc..Lubricant can include magnesium stearate, superfine silica gel powder, talcum powder, hydrogenated vegetable oil, poly- second Glycol, magnesium laurylsulfate etc..The pharmaceutically acceptable auxiliary material can also include some colouring agents, flavouring etc..As One specific embodiment of the present invention, the pharmaceutically acceptable auxiliary material are specially 22.0～44.0kg of carboxyrnethyl starch sodium, paste 25.0～35.0kg of essence, 70.0～100.0kg of calcium monohydrogen phosphate, 70～160kg of microcrystalline cellulose.
Specifically, the granulation is comprised the following steps：
1. granulation binders are prepared：First polyacrylic resin IV7.2kg immersions are dissolved with ethanol, add ethanol 208kg and purified water 25kg, stir, and are made into granulation binders；
2. pelletize：Mixed powder flour is added in Wet mixed granulating machine, 180rpm stirs 5 minutes, 1500rpm choppings 5 After minute, add step 1. obtained adhesive, 180rpm stir 1～3 minute, 1500rpm discharge after shredding 10 seconds, with waving Granulator is crossed 16 mesh sieves and makes wet granular；
3. be dried, whole grain：Gained wet granular is put in HighefficientFluidbeddrier, EAT is controlled for 80～100 DEG C, is gone out Air temperature is 55～65 DEG C, and it is 2.0～4.0% to be dried to moisture；Whole grain is sieved with multi-functional pelletizing machine 2.0mm, dry particl is obtained.
Specifically, the coating is comprised the following steps：
(S1) zein solution is prepared：Weigh during 2～5kg of zein adds 30～50kg of ethanol and soak, wait to be completely dissolved Afterwards, stir evenly, 120 mesh are filtered, standby；
(S2) preparation of polyacrylic resin IV solution：Weigh polyacrylic resin IV2～4kg, add ethanol 60～ 80kg, adds 450～700ml of polyoxyethylene sorbitan monoleate, 2～5kg of talcum powder, palm fibre oxidation after polyacrylic resin IV is completely dissolved 2～4kg of iron, stirs, and crosses colloid mill, and 200 mesh are filtered, standby；
(S3) preparation of polyacrylic resin IV Hydroxypropyl methylcelluloses mixed solution：Weigh Hydroxypropyl methylcellulose 0.5～ 2.0kg, adds 30～50kg of ethanol, after being uniformly dispersed, adds 5～10kg of purified water, stirs evenly, obtain Hydroxypropyl methylcellulose solution； Weigh in polyacrylic resin IV0.3～2.0kg addition 4～9kg of ethanol, after polyacrylic resin IV is completely dissolved, add The Hydroxypropyl methylcellulose solution, add polyoxyethylene sorbitan monoleate 200～600ml, 200～600ml of castor oil, Brown Ferric Oxide 1～ 4kg, 30～60g of dimeticone, stirs evenly, and crosses colloid mill, and 200 mesh are filtered, standby；
(S4) coating：Plain piece is put in seed-coating machine, heating air intake and air draft is opened, plain piece is heated to 35 DEG C or so, successively Gained zein solution is taken, polyacrylic resin IV solution, polyacrylic resin IV Hydroxypropyl methylcellulose mixed solutions are sprayed Slurry, sets 4～15 revs/min of drum rotation speed, controls 45～60 DEG C of EAT, and 35～45 DEG C of leaving air temp adjusts peristaltic pump 3～15rpm of rotating speed, 0.2～0.5MPa of compressed air pressure, during whitewashing, are stirred continuously Coating Solution, and wherein zein is molten Liquid is incubated 60 ± 5 DEG C；
(S5) polishing with cool：After coating tablet obtained by step (S4) is dried, 8～15 revs/min of drum rotation speed is set, will After dimeticone and river wax mixing, uniformly it is sprinkled in label, polishing 15～20 minutes；Afterwards by polishing piece cool more than 6 hours, bag Fill to obtain finished product.
Compared with prior art, in the preparation method of cough-relieving tablet of the invention, the drying means of medicinal extract is to do stage by stage It is dry, greatly shorten can drying time, the impact to active ingredient in medicine is reduced, and improves therapeutic effect.Production process technology Stability is improved, and process stabilizing, operational control are easy.Production environment improves, and reduces operation labour intensity.Production efficiency is carried Height, labour are reduced, and are increased productivity.
In order to more fully understand and implement, the following detailed description of the present invention.
Specific embodiment
Embodiment 1：It is prepared by I extract powders
The preparation of the I extract powders of the present invention is comprised the following steps：
(1) extract
The net medicinal material 100kg of pappy shell is taken, adds 1800L60% (v/v) ethanol, circumfluence distillation 4 hours to obtain alcohol extracting for the first time Liquid is taken, second plus 1400L60% (v/v) ethanol, circumfluence distillation 4 hours obtain alcohol extract, merge alcohol extract；
(2) ethanol is reclaimed
Alcohol extract is proceeded to into alcohol distillation column and reclaims ethanol, 100～102 DEG C of stoppings are reached to distillation temperature in the kettle, obtain medicine The ethanol of liquid and recovery gained；
(3) concentrate
Liquid is proceeded to and carry out in double effect evaporator double-effect evaporation, control steam pressure≤0.2MPa, vacuum：One effect- 0.04～-0.08MPa, two -0.06～-0.08MPa of effect, it is 1.20～1.30 (50 DEG C ± 2 DEG C) to be concentrated into relative density, is only obtained Cough precious piece I medicinal extract；
(4) vacuum dehydrating at lower temperature
Cough-relieving treasured piece I medicinal extract is pumped into into material pot, dextrin 0.3kg is added, unlatching is uniformly mixed, and opens heating Material is made to be incubated at 60～80 DEG C；110～120 DEG C of first paragraph temperature, 90～100 DEG C of second segment temperature, the 3rd section of temperature are set 10～30 DEG C, vacuum -0.1MPa, it is 90～160kg/h, 0.32～0.48m/ of crawler track speeds to arrange feed pump charging rate Min, the crawler belt are through the equal used time 18min of above-mentioned each section of temperature；Vacuum, heating are opened, after requirement to be achieved, charging is opened Pump is dried, and lock material and pulverizer are opened when material to be dried is into the 3rd section of nearly discharging, and 80 mesh stainless steel mesh of Jing is crushed Precious piece I medicinal extract comminuted powders must be coughed.
Embodiment 2：It is prepared by I extract powder systems
The preparation of the I extract powders of the present invention is comprised the following steps：
(1) extract
The net medicinal material 130kg of pappy shell is taken, adds 1800L60% (v/v) ethanol, circumfluence distillation 4 hours to obtain alcohol extracting for the first time Liquid is taken, second plus 1400L 60% (v/v) ethanol, circumfluence distillation 4 hours obtain alcohol extract, merge alcohol extract；
(2) ethanol is reclaimed
Alcohol extract is proceeded to into alcohol distillation column and reclaims ethanol, 100～102 DEG C of stoppings are reached to distillation temperature in the kettle, obtain medicine The ethanol of liquid and recovery gained；
(3) concentrate
Liquid is proceeded to and carry out in double effect evaporator double-effect evaporation, control steam pressure≤0.2MPa, vacuum：One effect- 0.04～-0.08MPa, two -0.06～-0.08MPa of effect, it is 1.20～1.30 (50 DEG C ± 2 DEG C) to be concentrated into relative density, is only obtained Cough precious piece I medicinal extract；
(4) vacuum dehydrating at lower temperature
Cough-relieving treasured piece I medicinal extract is pumped into into material pot, dextrin 0.3kg is added, unlatching is uniformly mixed, and opens heating Material is made to be incubated at 60～80 DEG C；110～120 DEG C of first paragraph temperature, 90～100 DEG C of second segment temperature, the 3rd section of temperature are set 10～30 DEG C, vacuum -0.1MPa, it is 90～160kg/h, 0.32～0.48m/ of crawler track speeds to arrange feed pump charging rate Min, the crawler belt are through the equal used time 18min of above-mentioned each section of temperature；Vacuum, heating are opened, after requirement to be achieved, charging is opened Pump is dried, and lock material and pulverizer are opened when material to be dried is into the 3rd section of nearly discharging, and 80 mesh stainless steel mesh of Jing is crushed Precious piece I medicinal extract comminuted powders must be coughed.
Embodiment 3：It is prepared by I extract powders
The preparation of the I extract powders of the present invention is comprised the following steps：
(1) extract
The net medicinal material 150kg of pappy shell is taken, adds 1800L60% (v/v) ethanol, circumfluence distillation 4 hours to obtain alcohol extracting for the first time Liquid is taken, second plus 1400L60% (v/v) ethanol, circumfluence distillation 4 hours obtain alcohol extract, merge alcohol extract；
(2) ethanol is reclaimed
Alcohol extract is proceeded to into alcohol distillation column and reclaims ethanol, 100～102 DEG C of stoppings are reached to distillation temperature in the kettle, obtain medicine The ethanol of liquid and recovery gained；
(3) concentrate
Liquid is proceeded to and carry out in double effect evaporator double-effect evaporation, control steam pressure≤0.2MPa, vacuum：One effect- 0.04～-0.08MPa, two -0.06～-0.08MPa of effect, it is 1.20～1.30 (50 DEG C ± 2 DEG C) to be concentrated into relative density, is only obtained Cough precious piece I medicinal extract；
(4) vacuum dehydrating at lower temperature
Cough-relieving treasured piece I medicinal extract is pumped into into material pot, dextrin 0.3kg is added, unlatching is uniformly mixed, and opens heating Material is made to be incubated at 60～80 DEG C；110～120 DEG C of first paragraph temperature, 90～100 DEG C of second segment temperature, the 3rd section of temperature are set 10～30 DEG C, vacuum -0.1MPa, it is 90～160kg/h, 0.32～0.48m/ of crawler track speeds to arrange feed pump charging rate Min, the crawler belt are through the equal used time 18min of above-mentioned each section of temperature；Vacuum, heating are opened, after requirement to be achieved, charging is opened Pump is dried, and lock material and pulverizer are opened when material to be dried is into the 3rd section of nearly discharging, and 80 mesh stainless steel mesh of Jing is crushed Precious piece I medicinal extract comminuted powders must be coughed.
Embodiment 4：It is prepared by II extract powders
The preparation of the II extract powders of the present invention is comprised the following steps：
(1) alcohol extracting part
1st, extract：Weigh Exocarpium Citri Rubrum 75kg, balloonflower root 100kg, Fructus Aurantii 10kg, tuber of stemona 75kg, fruit of Chinese magnoliavine 10kg, dried orange peel 100kg, Rhizoma zingiberis 10kg, schizonepeta 50kg, the net medicinal material coarse powder of nine tastes of root of purple-flowered peucedanum 150kg, put in multi-function extractor, add 8 times of amounts 60% for the first time (v/v) ethanol, heating are incubated 60 ± 5 DEG C and impregnate 48 hours, obtains alcohol extract；Second plus 8 times of amount 60% (v/v) ethanol, plus Heat, is incubated 60 ± 5 DEG C and impregnates 48 hours, obtain alcohol extract, merge alcohol extract；
2nd, ethanol is reclaimed：Alcohol extract is proceeded to into alcohol distillation column and reclaims ethanol, 100 are reached to distillation temperature in the kettle～ Stop when 102 DEG C, obtain liquid and reclaim the ethanol of gained；
3rd, concentrate：Liquid is proceeded in double effect evaporator and is concentrated, control steam pressure≤0.2MPa, vacuum：One effect- 0.04～-0.08MPa, two -0.06～-0.08MPa of effect, it is 1.20～1.30 (50 DEG C ± 2 DEG C) to be concentrated into relative density, is only obtained Cough precious piece II extractum As；
(2) water extraction part
1st, extract：Aster 100kg, the net medicinal material of bis- tastes of Radix Glycyrrhizae 350kg are weighed, is put in multi-function extractor, add 8 times for the first time Amount water, boils extraction 2 hours, obtains aqueous extract；Second plus 8 times of amount water, boil extraction 2 hours, obtain aqueous extract, merge water Extract；
2nd, concentrate：Aqueous extract is proceeded in double effect evaporator and is concentrated, control steam pressure≤0.2MPa, vacuum：One - 0.04～-0.08MPa of effect, two -0.06～-0.08MPa of effect, it is 1.20～1.30 (50 DEG C ± 2 DEG C) to be concentrated into relative density, Obtain cough-relieving treasured piece II medicinal extract B；
(3) vacuum dehydrating at lower temperature
Will cough-relieving treasured piece II extractum As and cough-relieving treasured piece II medicinal extract B are well mixed, pump into material pot, add cunning 30～50kg of stone flour, unlatching are uniformly mixed, and opening heating makes material be incubated at 60～80 DEG C；First paragraph temperature is set 120～130 DEG C, 100～110 DEG C of second segment temperature, 10～30 DEG C of the 3rd section of temperature, vacuum -0.1MPa arrange feed pump and enter Material speed is 90～160kg/h, 0.32～0.48m/min of crawler track speeds, the crawler belt through the above-mentioned each section of temperature equal used time 18min；Vacuum, heating are opened, after requirement to be achieved, feed pump is opened and is dried, material to be dried closely goes out into the 3rd section Lock material and pulverizer are opened during material, 80 mesh stainless steel mesh of Jing crushes to obtain cough-relieving treasured piece II medicinal extract comminuted powders.
Embodiment 5：It is prepared by II extract powders
The preparation of the II extract powders of the present invention is comprised the following steps：
(1) alcohol extracting part
1st, extract：Weigh Exocarpium Citri Rubrum 84kg, balloonflower root 128kg, Fructus Aurantii 20kg, tuber of stemona 84kg, fruit of Chinese magnoliavine 20kg, dried orange peel 128kg, Rhizoma zingiberis 20kg, schizonepeta 64kg, the net medicinal material coarse powder of nine tastes of root of purple-flowered peucedanum 188kg, put in multi-function extractor, add 8 times of amounts 60% for the first time (v/v) ethanol, heating are incubated 60 ± 5 DEG C and impregnate 48 hours, obtains alcohol extract；Second plus 8 times of amount 60% (v/v) ethanol, plus Heat, is incubated 60 ± 5 DEG C and impregnates 48 hours, obtain alcohol extract, merge alcohol extract；
2nd, ethanol is reclaimed：Alcohol extract is proceeded to into alcohol distillation column and reclaims ethanol, 100 are reached to distillation temperature in the kettle～ Stop when 102 DEG C, obtain liquid and reclaim the ethanol of gained；
3rd, concentrate：Liquid is proceeded in double effect evaporator and is concentrated, control steam pressure≤0.2MPa, vacuum：One effect- 0.04～-0.08MPa, two -0.06～-0.08MPa of effect, it is 1.20～1.30 (50 DEG C ± 2 DEG C) to be concentrated into relative density, is only obtained Cough precious piece II extractum As；
(2) water extraction part
1st, extract：Aster 128kg, the net medicinal material of bis- tastes of Radix Glycyrrhizae 380kg are weighed, is put in multi-function extractor, add 8 times for the first time Amount water, boils extraction 2 hours, obtains aqueous extract；Second plus 8 times of amount water, boil extraction 2 hours, obtain aqueous extract, merge water Extract；
2nd, concentrate：Aqueous extract is proceeded in double effect evaporator and is concentrated, control steam pressure≤0.2MPa, vacuum：One - 0.04～-0.08MPa of effect, two -0.06～-0.08MPa of effect, it is 1.20～1.30 (50 DEG C ± 2 DEG C) to be concentrated into relative density, Obtain cough-relieving treasured piece II medicinal extract B；
(3) vacuum dehydrating at lower temperature
Will cough-relieving treasured piece II extractum As and cough-relieving treasured piece II medicinal extract B are well mixed, pump into material pot, add cunning 30～50kg of stone flour, unlatching are uniformly mixed, and opening heating makes material be incubated at 60～80 DEG C；First paragraph temperature is set 120～130 DEG C, 100～110 DEG C of second segment temperature, 10～30 DEG C of the 3rd section of temperature, vacuum -0.1MPa arranges feed pump Charging rate is 90～160kg/h, 0.32～0.48m/min of crawler track speeds, the crawler belt are used through above-mentioned each section of temperature When 18min；Vacuum, heating are opened, after requirement to be achieved, feed pump is opened and is dried, material to be dried is near into the 3rd section Lock material and pulverizer are opened during discharging, 80 mesh stainless steel mesh of Jing crushes to obtain cough-relieving treasured piece II medicinal extract comminuted powders.
Embodiment 6：It is prepared by II extract powders
The preparation of the II extract powders of the present invention is comprised the following steps：
(1) alcohol extracting part
1st, extract：Weigh Exocarpium Citri Rubrum 100kg, balloonflower root 150kg, Fructus Aurantii 30kg, tuber of stemona 100kg, fruit of Chinese magnoliavine 30kg, dried orange peel 150kg, rhizoma zingiberis 30kg, schizonepeta 80kg, the net medicinal material coarse powder of nine tastes of root of purple-flowered peucedanum 200kg, put in multi-function extractor, add 8 times for the first time Amount 60% (v/v) ethanol, heating are incubated 60 ± 5 DEG C and impregnate 48 hours, obtains alcohol extract；Second plus 8 times of 60% (v/v) of amount Ethanol, heating are incubated 60 ± 5 DEG C and impregnate 48 hours, obtain alcohol extract, merges alcohol extract；
2nd, ethanol is reclaimed：Alcohol extract is proceeded to into alcohol distillation column and reclaims ethanol, 100 are reached to distillation temperature in the kettle～ Stop when 102 DEG C, obtain liquid and reclaim the ethanol of gained；
3rd, concentrate：Liquid is proceeded in double effect evaporator and is concentrated, control steam pressure≤0.2MPa, vacuum：One effect- 0.04～-0.08MPa, two -0.06～-0.08MPa of effect, it is 1.20～1.30 (50 DEG C ± 2 DEG C) to be concentrated into relative density, is only obtained Cough precious piece II extractum As；
(2) water extraction part
1st, extract：Aster 150kg, the net medicinal material of bis- tastes of Radix Glycyrrhizae 400kg are weighed, is put in multi-function extractor, add 8 times for the first time Amount water, boils extraction 2 hours, obtains aqueous extract；Second plus 8 times of amount water, boil extraction 2 hours, obtain aqueous extract, merge water Extract；
2nd, concentrate：Aqueous extract is proceeded in double effect evaporator and is concentrated, control steam pressure≤0.2MPa, vacuum：One - 0.04～-0.08MPa of effect, two -0.06～-0.08MPa of effect, it is 1.20～1.30 (50 DEG C ± 2 DEG C) to be concentrated into relative density, Obtain cough-relieving treasured piece II medicinal extract B；
(3) vacuum dehydrating at lower temperature
Will cough-relieving treasured piece II extractum As and cough-relieving treasured piece II medicinal extract B are well mixed, pump into material pot, add cunning 30～50kg of stone flour, unlatching are uniformly mixed, and opening heating makes material be incubated at 60～80 DEG C；First paragraph temperature is set 120～130 DEG C, 100～110 DEG C of second segment temperature, 10～30 DEG C of the 3rd section of temperature, vacuum -0.1MPa arranges feed pump Charging rate is 90～160kg/h, 0.32～0.48m/min of crawler track speeds, the crawler belt are used through above-mentioned each section of temperature When 18min；Vacuum, heating are opened, after requirement to be achieved, feed pump is opened and is dried, material to be dried is near into the 3rd section Lock material and pulverizer are opened during discharging, 80 mesh stainless steel mesh of Jing crushes to obtain cough-relieving treasured piece II medicinal extract comminuted powders.
Embodiment 7：The preparation of cough-relieving treasured piece
The preparation of the cough-relieving treasured piece of the present invention is comprised the following steps：
(1) mix
Weigh the I cream comminuted powder 90kg of the preparation of embodiment 2, II cream comminuted powder 231kg prepared by embodiment 5, chlorination Ammonium 160.0kg, carboxyrnethyl starch sodium 44.0kg, dextrin 35.0kg, calcium monohydrogen phosphate 70.0kg, microcrystalline cellulose 160kg, add wet method In hybrid particles machine, 180rpm stirrings 5 minutes, 1500rpm are shredded 5 minutes, obtain mixed powder；
(2) crush
Mixed powder is crushed with 60 mesh sieve of Universalpulverizer, obtains mixed powder flour；
(3) pelletize
1st, granulation binders are prepared：First polyacrylic resin IV7.2kg immersions are dissolved with ethanol, add enough ethanol 208kg and purified water 25kg, stir, and are made into granulation binders；
2nd, pelletize：Mixed powder flour is added in Wet mixed granulating machine, 180rpm stirrings, 1500rpm is opened and is shredded 5 points Zhong Hou, adds polyacrylic resin IV ethanol solutions, opens 180rpm and stirs 1～3 minute, and I speed 1500rpm is shredded 10 seconds, is gone out Material, crosses 16 mesh sieves and makes particle with oscillating granulator；
3rd, dry, whole grain：The wet granular for making is dried with HighefficientFluidbeddrier, EAT is controlled for 80～100 DEG C, leaving air temp is 55～65 DEG C, and it is 2.0～4.0% to be dried to moisture；Whole grain is sieved with multi-functional pelletizing machine 2.0mm, cough-relieving is obtained Precious piece dry particl；
(4) it is total mixed
Taking dry particl adds peppermint oil dementholized 1kg, magnesium stearate 7kg to mix 20 minutes in adding two-dimensional motion mixer, obtains Cough-relieving treasured piece particle；
(5) compressing tablet.
Using Φ 10mm depth arc punch die compressing tablets, cough-relieving treasured piece plain piece is obtained
(6) coating
1st, with syrup
(1) zein solution is prepared：
Weigh during zein 2kg adds ethanol 30kg and soak, until completely dissolved, stir evenly, 120 mesh are filtered, standby；
(2) preparation of polyacrylic resin IV solution：
Polyacrylic resin IV2kg is weighed, and is added ethanol 60kg, poly- mountain is added after polyacrylic resin IV is completely dissolved 80 450ml of pear ester, talcum powder 2kg, Brown Ferric Oxide 2kg, stir, and cross colloid mill, and 200 mesh are filtered, standby；
(3) preparation of polyacrylic resin IV Hydroxypropyl methylcelluloses mixed solution：
Hydroxypropyl methylcellulose 0.5kg is weighed, ethanol 30kg is added, after being uniformly dispersed, purified water 5kg is added, is stirred evenly, obtain hydroxyl Third methylcellulose solution；Weigh in polyacrylic resin IV0.3kg addition ethanol 4kg, treat that polyacrylic resin IV is completely dissolved Afterwards, the Hydroxypropyl methylcellulose solution is added, adds polyoxyethylene sorbitan monoleate 200ml castor oil 200ml, Brown Ferric Oxide 1kg, diformazan Silicone oil 30g, stirs evenly, and crosses colloid mill, and 200 mesh are filtered, standby.
2nd, film coating
(1) weigh cough-relieving treasured piece plain piece to put in efficient sugar-coat-film coater, start high seed-coating machine, open heating air intake And air draft, plain piece is heated to 35 DEG C or so, controls suitable rotating speed, initially enters coating procedure.
(2) spray film-coating：Take successively and prepare zein solution, polyacrylic resin IV solution, polyacrylic resin IV Hydroxypropyl methylcellulose mixed solution is whitewashed, and sets 4～15 revs/min of drum rotation speed, controls 45～60 DEG C of EAT, goes out 35～45 DEG C of air temperature, adjusts 3～15rpm of wriggling revolution speed, 0.2～0.5MPa of compressed air pressure, is sprayed with suitable speed Slurry, makes coat tablets moisten and adhesion.During whitewashing, Coating Solution, wherein zein solution insulation 60 ± 5 are stirred continuously ℃。
(3) polishing with cool：First allow piece to spontaneously dry before polishing, after being dried, set 8～15 revs/min of drum rotation speed, will After dimeticone and river wax mixing, uniformly it is sprinkled in label, polishing 15～20 minutes.After coating is finished, polishing piece is laid in In stainless steel disc on cool horse, cool more than 6 hours, it be the precious piece product to be packaged of cough-relieving to collect cool good polishing piece.
Embodiment 8：The preparation of cough-relieving treasured piece
The preparation of the cough-relieving treasured piece of the present invention is comprised the following steps：
(1) mix
Weigh the I cream comminuted powder 65kg of the preparation of embodiment 1, II cream comminuted powder 161kg prepared by embodiment 4, chlorination Ammonium 160.0kg, carboxyrnethyl starch sodium 44.0kg, dextrin 35.0kg, calcium monohydrogen phosphate 70.0kg, microcrystalline cellulose 70kg, add wet method In hybrid particles machine, 180rpm stirrings 5 minutes, 1500rpm are shredded 5 minutes, obtain mixed powder；
(2) crush
Mixed powder is crushed with 60 mesh sieve of Universalpulverizer, obtains mixed powder flour；
(3) pelletize
1st, granulation binders are prepared：First polyacrylic resin IV7.2kg immersions are dissolved with ethanol, add enough ethanol 208kg and purified water 25kg, stir, and are made into granulation binders；
2nd, pelletize：Mixed powder flour is added in Wet mixed granulating machine, 180rpm stirrings, 1500rpm is opened and is shredded 5 points Zhong Hou, adds polyacrylic resin IV ethanol solutions, opens 180rpm and stirs 1～3 minute, and I speed 1500rpm is shredded 10 seconds, is gone out Material, crosses 16 mesh sieves and makes particle with oscillating granulator；
3rd, dry, whole grain：The wet granular for making is dried with HighefficientFluidbeddrier, EAT is controlled for 80～100 DEG C, leaving air temp is 55～65 DEG C, and it is 2.0～4.0% to be dried to moisture；Whole grain is sieved with multi-functional pelletizing machine 2.0mm, cough-relieving is obtained Precious piece dry particl；
(4) it is total mixed
Taking dry particl adds peppermint oil dementholized 1kg, magnesium stearate 7kg to mix 20 minutes in adding two-dimensional motion mixer, obtains Cough-relieving treasured piece particle；
(5) compressing tablet.
Using Φ 10mm depth arc punch die compressing tablets, cough-relieving treasured piece plain piece is obtained
(6) coating
1st, with syrup
(1) zein solution is prepared：
Weigh during zein 5kg adds ethanol 50kg and soak, until completely dissolved, stir evenly, 120 mesh are filtered, standby；
(2) preparation of polyacrylic resin IV solution：
Polyacrylic resin IV4kg is weighed, and is added ethanol 80kg, poly- mountain is added after polyacrylic resin IV is completely dissolved 80 700ml of pear ester, talcum powder 5kg, Brown Ferric Oxide 4kg, stir, and cross colloid mill, and 200 mesh are filtered, standby；
(3) preparation of polyacrylic resin IV Hydroxypropyl methylcelluloses mixed solution：
Hydroxypropyl methylcellulose 2.0kg is weighed, ethanol 50kg is added, after being uniformly dispersed, purified water 10kg is added, is stirred evenly, obtain Hydroxypropyl methylcellulose solution；Weigh in polyacrylic resin IV2.0kg addition ethanol 9kg, treat that polyacrylic resin IV is completely molten Xie Hou, the addition Hydroxypropyl methylcellulose solution, addition polyoxyethylene sorbitan monoleate 600ml castor oil 600ml, Brown Ferric Oxide 4kg, two First silicone oil 60g, stirs evenly, and crosses colloid mill, and 200 mesh are filtered, standby.
2nd, film coating
(1) weigh cough-relieving treasured piece plain piece to put in efficient sugar-coat-film coater, start high seed-coating machine, open heating air intake And air draft, plain piece is heated to 35 DEG C or so, controls suitable rotating speed, initially enters coating procedure.
(2) spray film-coating：Take successively and prepare zein solution, polyacrylic resin IV solution, polyacrylic resin IV Hydroxypropyl methylcellulose mixed solution is whitewashed, and sets 4～15 revs/min of drum rotation speed, controls 45～60 DEG C of EAT, goes out 35～45 DEG C of air temperature, adjusts 3～15rpm of wriggling revolution speed, 0.2～0.5MPa of compressed air pressure, is sprayed with suitable speed Slurry, makes coat tablets moisten and adhesion.During whitewashing, Coating Solution, wherein zein solution insulation 60 ± 5 are stirred continuously ℃。
(3) polishing with cool：First allow piece to spontaneously dry before polishing, after being dried, set 8～15 revs/min of drum rotation speed, will After dimeticone and river wax mixing, uniformly it is sprinkled in label, polishing 15～20 minutes.After coating is finished, polishing piece is laid in In stainless steel disc on cool horse, cool more than 6 hours, it be the precious piece product to be packaged of cough-relieving to collect cool good polishing piece.
Embodiment 7 and the tablet obtained by embodiment 8 and tablet Jing full inspection data displays obtained in existing process, quality without Difference.
Above-mentioned embodiment is the invention is not limited in, if the various changes to the present invention or deformation are without departing from the present invention Spirit and scope, if these change and deformation belong to the present invention claim and equivalent technologies within the scope of, then this It is bright to be also intended to comprising these changes and deform.

Claims (3)

1. a kind of preparation method of cough-relieving tablet, it is characterised in that comprise the following steps：
(1) preparation of .I extract powders：The pappy shell of 100～150kg is extracted into 2 times with the alcohol reflux of 1400～1800L, often Secondary 4h, merges extract, is vacuum dried stage by stage and crushes, obtain No. I medicinal extract comminuted powder after recovery ethanol, concentration；
(2) preparation of .II extract powders：Weigh Exocarpium Citri Rubrum 75～100kg of meal, balloonflower root 100～150kg of meal, Fructus Aurantii meal 10 ～30kg, the tuber of stemona 75～100kg of meal, the fruit of Chinese magnoliavine 10～30kg of meal, dried orange peel 100～150kg of meal, rhizoma zingiberis meal 10～ 30kg, schizonepeta 50～80kg of meal, the root of purple-flowered peucedanum 150～200kg of meal, with 60 ± 5 DEG C of the ethanol of 8 times of weight extract 2 times, every time 48h, merges extract, reclaims ethanol, is concentrated to give II extractum As；Weigh 100～150kg of aster, the net medicines of 350～400kg of Radix Glycyrrhizae Material, puts in multi-function extractor, boils extraction 2 times with the water of 8 times of weight, and each 2h merges extract, is concentrated to give II medicinal extract B；It is vacuum dried stage by stage and crushes after the II extractum As are well mixed with II medicinal extract B, obtains II medicinal extract comminuted powders；
(3). the preparation of tablet：By No. I medicinal extract 65～90kg of comminuted powder, cough-relieving treasured piece II cream comminuted powder 161～ 231kg, ammonium chloride 150kg～180kg are pelletized after being mixed with pharmaceutically acceptable auxiliary material, are added 1kg peppermint oil dementholizeds with lubrication After agent always mixes 20min, compressing tablet, coating obtain the cough-relieving tablet；
Recovery ethanol in the step (1) and (2) is：Extract after merging is proceeded to into alcohol distillation column and reclaims ethanol, extremely Distillation temperature in the kettle stops when reaching 100～102 DEG C, obtains liquid and reclaims the ethanol of gained；
Concentration in the step (1) and (2) is：Control steam pressure≤0.2MPa, vacuum be one effect -0.04～- 0.08MPa, two -0.06～-0.08MPa of effect, it is 1.20～1.30 to be concentrated into extract relative density at 50 DEG C ± 2 DEG C；
It is vacuum dried and crushes in the step (1) and is：No. I concentrate is pumped into into material pot, adds dextrin 0.3kg, unlatching to stir Mix and be well mixed, and opening heating makes material be incubated at 60～80 DEG C；110～120 DEG C of first paragraph temperature, second segment temperature are set 90～100 DEG C, 10～30 DEG C of the 3rd section of temperature, vacuum -0.1MPa, it is 90～160kg/h, shoe to arrange feed pump charging rate 0.32～0.48m/min of tape speed, the crawler belt are through the equal used time 18min of above-mentioned each section of temperature；Vacuum, heating are opened, is treated After reaching requirement, open feed pump and be dried, when material to be dried is into the 3rd section of nearly discharging, open lock material and pulverizer, Jing 80 mesh stainless steel mesh are crushed；
It is vacuum dried and crushes in the step (2) and is：Thing is pumped into after the II extractum As are well mixed with II medicinal extract B Batch can, adds 30～50kg of talcum powder, unlatching to be uniformly mixed, and opening heating makes material be incubated at 60～80 DEG C；Arrange 120～130 DEG C of first paragraph temperature, 100～110 DEG C of second segment temperature, 10～30 DEG C of the 3rd section of temperature, vacuum -0.1MPa, if Put feed pump charging rate for 90～160kg/h, 0.32～0.48m/min of crawler track speeds, the crawler belt through above-mentioned each section The equal used time 18min of temperature；Vacuum, heating are opened, after requirement to be achieved, feed pump is opened and is dried, material to be dried is entered Lock material and pulverizer are opened during the 3rd section of nearly discharging, 80 mesh stainless steel mesh of Jing is crushed；
The granulation is comprised the following steps：
1. granulation binders are prepared：First with ethanol by polyacrylic resinⅣ 7.2kg immersion dissolve, add ethanol 208kg and Purified water 25kg, stirs, and is made into granulation binders；
2. pelletize：Mixed powder flour is added in Wet mixed granulating machine, 180rpm stirrings 5 minutes, 1500rpm are shredded 5 minutes Afterwards, add step 1. obtained adhesive, 180rpm stir 1～3 minute, 1500rpm discharge after shredding 10 seconds, with waving particle Machine is crossed 16 mesh sieves and makes wet granular；
3. be dried, whole grain：Gained wet granular is put in HighefficientFluidbeddrier, EAT is controlled for 80～100 DEG C, goes out wind-warm syndrome Spend for 55～65 DEG C, it is 2.0～4.0% to be dried to moisture；Whole grain is sieved with multi-functional pelletizing machine 2.0mm, dry particl is obtained；
The coating is comprised the following steps：
(S1) zein solution is prepared：Weigh during 2～5kg of zein adds 30～50kg of ethanol and soak, until completely dissolved, stir Even, 120 mesh are filtered, standby；
(S2) preparation of polyacrylic resinⅣ solution：2～4kg of polyacrylic resinⅣ is weighed, 60～80kg of ethanol is added, is treated Polyacrylic resinⅣ add after being completely dissolved 450～700ml of polyoxyethylene sorbitan monoleate, 2～5kg of talcum powder, Brown Ferric Oxide 2～ 4kg, stirs, and crosses colloid mill, and 200 mesh are filtered, standby；
(S3) preparation of polyacrylic resinⅣ Hydroxypropyl methylcellulose mixed solution：0.5～2.0kg of Hydroxypropyl methylcellulose is weighed, 30～50kg of ethanol is added, after being uniformly dispersed, 5～10kg of purified water is added, is stirred evenly, obtain Hydroxypropyl methylcellulose solution；Weigh poly- During IV 0.3～2.0kg of acrylic resin adds 4～9kg of ethanol, after polyacrylic resinⅣ is completely dissolved, the hydroxyl is added Third methylcellulose solution, adds polyoxyethylene sorbitan monoleate 200～600ml, 200～600ml of castor oil, 1～4kg of Brown Ferric Oxide, diformazan 30～60g of silicone oil, stirs evenly, and crosses colloid mill, and 200 mesh are filtered, standby；
(S4) coating：Plain piece is put in seed-coating machine, heating air intake and air draft is opened, plain piece is heated to 35 DEG C or so, takes institute successively Zein solution is obtained, polyacrylic resinⅣ solution, polyacrylic resinⅣ Hydroxypropyl methylcellulose mixed solution are whitewashed, if Determine 4～15 revs/min of drum rotation speed, control 45～60 DEG C of EAT, 35～45 DEG C of leaving air temp adjusts wriggling revolution speed 3 ～15rpm, 0.2～0.5MPa of compressed air pressure, during whitewashing, are stirred continuously Coating Solution, and wherein zein solution is protected 60 ± 5 DEG C of temperature；
(S5) polishing with cool：After coating tablet obtained by step (S4) is dried, 8～15 revs/min of drum rotation speed is set, by diformazan After silicone oil and river wax mixing, uniformly it is sprinkled in label, polishing 15～20 minutes；Afterwards by polishing piece cool more than 6 hours, pack Finished product.
2. the preparation method of cough-relieving tablet according to claim 1, it is characterised in that extract in step (1) and (2) and use institute Ethanol is stated for ethanol that percent by volume is 60%.
3. the preparation method of cough-relieving tablet according to claim 1, it is characterised in that the pharmaceutically acceptable auxiliary material For：22.0～44.0kg of carboxyrnethyl starch sodium, 25.0～35.0kg of dextrin, 70.0～100.0kg of calcium monohydrogen phosphate, microcrystalline cellulose 70 ～160kg.
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CN102379927A (en) * 2011-10-25 2012-03-21 海南海力制药有限公司 Preparation methods of poppy shell extract and cough tablet

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