CN110354202A - The preparation process of glutinous rehmannia Xiaoke Tablets - Google Patents

The preparation process of glutinous rehmannia Xiaoke Tablets Download PDF

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CN110354202A
CN110354202A CN201910695170.9A CN201910695170A CN110354202A CN 110354202 A CN110354202 A CN 110354202A CN 201910695170 A CN201910695170 A CN 201910695170A CN 110354202 A CN110354202 A CN 110354202A
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glutinous rehmannia
xiaoke
tablets
tablet
weight
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王秀英
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Jilin Agricultural Science and Technology College
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Jilin Agricultural Science and Technology College
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/42—Cucurbitaceae (Cucumber family)
    • A61K36/428—Trichosanthes
    • 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
    • A61K36/481—Astragalus (milkvetch)
    • 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
    • A61K36/484—Glycyrrhiza (licorice)
    • 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
    • A61K36/488—Pueraria (kudzu)
    • 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)
    • A61K36/80—Scrophulariaceae (Figwort family)
    • A61K36/804—Rehmannia
    • 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)
    • A61K36/894—Dioscoreaceae (Yam family)
    • A61K36/8945—Dioscorea, e.g. yam, Chinese yam or water yam
    • 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)
    • A61K36/896—Liliaceae (Lily family), e.g. daylily, plantain lily, Hyacinth or narcissus
    • A61K36/8968—Ophiopogon (Lilyturf)
    • 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
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P3/00—Drugs for disorders of the metabolism
    • A61P3/08—Drugs for disorders of the metabolism for glucose homeostasis
    • A61P3/10—Drugs for disorders of the metabolism for glucose homeostasis for hyperglycaemia, e.g. antidiabetics
    • 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
    • A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps

Abstract

The invention discloses the preparation processes of glutinous rehmannia Xiaoke Tablets, the formula material of glutinous rehmannia Xiaoke Tablets is glutinous rehmannia, Radix Astragali, radices trichosanthis, Chinese yam, Radix Ophiopogonis, pueraria lobata, Radix Glycyrrhizae, CMS-Na, dehydrated alcohol, magnesium stearate, filler, the following steps are included: step 1: being cleaned by ultrasonic cleaner to glutinous rehmannia, Radix Astragali, radices trichosanthis, Chinese yam, Radix Ophiopogonis, pueraria lobata, Radix Glycyrrhizae, powder mixing is broken by pulverizer in prescription ratio, it is put into Soxhlet extractor, add 8-12 times of water, refluxing extraction, it extracts 1-3 times, 2h is extracted every time, obtains aqueous extract；Step 2: obtained extracting solution is filtered with suction filtration machine, is concentrated with Rotary Evaporators, then concentrate is put into electric drying oven with forced convection.Products obtained therefrom of the present invention meets pharmacopeia defined by the hardness determination of tablet, friability detection, tablet weight variation, disintegration time limited detection, and traditional decoction is changed to tablet, and convenient for saving, transporting, patient is easy to receive, and bioavilability is good.

Description

The preparation process of glutinous rehmannia Xiaoke Tablets
Technical field
The present invention relates to technical field of pharmaceuticals, the specially preparation process of glutinous rehmannia Xiaoke Tablets.
Background technique
Improved with living standard, one of the people with corresponding disease also gradually increases, and diabetes are, diabetes it is main Symptom is hyperglycemia, and causing factor is due to insulin secretion failure, and sick blood vessel, kidney, heart, eye etc. of will lead to too long is organized Many damages, damage relevant organ dysfunction.
In the theory of Chinese medicine, diabetes be referred to as " diabetes ", the world medically, China to this disease earliest record In Huangdi's Internal Classics, mainly stomach and kidney are got angry scorching, consume excessive body fluid, the time can injure long very much it is excessive, so causing Other internal organs organs it is impaired to corresponding complication occur.
There is history for a long time using glutinous rehmannia treatment diabetes, " book on Chinese herbal medicine is newly organized ", " Synopsis Golden Chamber ", " prescriptions worth thousand gold " etc. are all to use Glutinous rehmannia preferably treats the effect quenched one's thirst as key medicine, from the arrival of different medicine compatibilities, from ancient times to the present to have application more.
" Diabetes decoction " comes from " prescriptions worth thousand gold " written by SUN Si miao, can relieve inflammation or internal heat, help, has tonifying spleen, nourshing kidney, promotes the production of body fluid, heat-clearing, benefit The effect of blood, can tonneau three it is burnt, can alleviate that eating for diabete performance is more, urine is more and people is aobvious thin, be easy tired out, sleep quality The symptoms such as difference.
Glutinous rehmannia nourishing Yin and promoting production of body fluid in side, heat-clearing kidney tonifying；Radix Astragali ascending YANG and invigorating QI, fosters the spirit of nobility and promotes the production of body fluid, and is all monarch drug in a prescription, and radices trichosanthis heat-clearing is rushed down Fire promotes the production of body fluid to quench thirst；Radix Ophiopogonis clearing heat and promoting fluid, nourishing Yin and moistening lung；Stomach is mended in Chinese yam tonifying spleen, is all ministerial drug, and pueraria lobata rising Yang cloth saliva, is adjutant, Radix Glycyrrhizae, can reconcile drug effect, be to make medicine, this several medicines have small component to play a major role.
This prescription is used till today, and the development with experience different generations and doctor is perfect, there is a good curative effect, but due to Its conventional dosage forms decoction, applies and is restricted, and decoction is time-honored a kind of dosage form from ancient times to the present, it is convenient for absorbing, but Highly volatile, decoction need to take juice to remove slag, process relatively overelaborates, and to the time of decoction, fire by decocting Chinese medicine It waits, equipment has certain requirement, and should not save.
Summary of the invention
The purpose of the present invention is to provide the preparation process of glutinous rehmannia Xiaoke Tablets, have glutinous rehmannia Xiaoke Tablets be easy to use it is excellent Point solves glutinous rehmannia and quenches one's thirst decoction inconvenient problem with use.
To achieve the above object, the invention provides the following technical scheme: the preparation process of glutinous rehmannia Xiaoke Tablets, glutinous rehmannia Xiaoke Tablets Formula material be glutinous rehmannia, Radix Astragali, radices trichosanthis, Chinese yam, Radix Ophiopogonis, pueraria lobata, Radix Glycyrrhizae, CMS-Na, dehydrated alcohol, magnesium stearate, fill out Fill agent, comprising the following steps:
Step 1: glutinous rehmannia, Radix Astragali, radices trichosanthis, Chinese yam, Radix Ophiopogonis, pueraria lobata, Radix Glycyrrhizae are cleaned by ultrasonic cleaner, Powder mixing is broken by pulverizer in prescription ratio, is put into Soxhlet extractor, adds 8-12 times of water, refluxing extraction is extracted 1-3 times, 2h is extracted every time, obtains aqueous extract；
Step 2: obtained extracting solution is filtered with suction filtration machine, is concentrated with Rotary Evaporators, concentrate is then put into electric heating In air dry oven, the temperature of electric drying oven with forced convection is 60 DEG C, dry to constant weight, obtains dry extract；
Step 3: taking dry extract and filler to mix in 1: 1,1: 3,1: 5 ratio, and be added appropriate 75-95%'s 1-5% disintegrating agent CMS-Na is added in dehydrated alcohol, is mixed to prepare softwood, crosses 20 mesh medicines sieve, particle is made, is put into electric heating air blast 60 DEG C of dryings in drying box are taken out, and 0.1-0.5% magnesium stearate is added, and are carried out tabletting using tablet press machine, are obtained glutinous rehmannia and quench one's thirst Piece；
Step 4: glutinous rehmannia Xiaoke Tablets 20 are taken at random, is first weighed using assay balance, then calculate average slice weight, it is then accurate The weight for weighing single yellow Xiaoke Tablets, compares single slice weight and average slice weight, detects to the slice weight of glutinous rehmannia Xiaoke Tablets；
Step 5: the hanging basket of instrument being fixed, is put into 1000ml beaker, adjustment hanging basket can be up and down, bottom of the beaker 37 DEG C of temperature of water pours into away from sieve 25mm in portion, allows the water to submergence sieve and the 25mm when highest water surface is higher by sieve highest point, Take glutinous rehmannia Xiaoke Tablets 12 at random, be respectively put into the glass tube of hanging basket, to carry out check glutinous rehmannia Xiaoke Tablets disintegration time limited into Row detection；
Step 6: randomly selecting glutinous rehmannia Xiaoke Tablets 20, check tablet with tablet hardness instrument, detect the hard of glutinous rehmannia Xiaoke Tablets Degree；
Step 7: randomly selecting glutinous rehmannia Xiaoke Tablets 55, the floating powder on surface is blown away with hair dryer, claims its gross mass, is put into piece In the glass cylinder of agent friability instrument, setting revolving speed is 25r/min, is taken out after 4min, then blow away floating powder on surface with hair dryer, is weighed Gross weight calculates the weight of loss, detects to the tablet friability of glutinous rehmannia Xiaoke Tablets；
Step 8: taking dry funnel and funnel is fixed on iron stand, spread a blank sheet of paper in the underface of bell mouth, survey The distance for measuring bell mouth and paper is denoted as H, the particle that granulation obtains slowly is poured into funnel close to hopper walls, until granule Until the vertebral height formed at bell mouth is equal to height of the bell mouth apart from blank sheet of paper, measure what granule was formed in paper Centrum diameter is denoted as R, and the base angle ∠ α of granule cone is calculated according to formula tan α=H/R, and ∠ α is angle of repose, disappears to glutinous rehmannia The angle of repose of thirsty piece is calculated.
Preferably, the filler can be dextrin or lactose or isomalt.
Preferably, the step 4,5,6 and 7 are detected by tablet four with detector.
Glutinous rehmannia: the monarch drug in a prescription in the side of being, effective component are Dihuang polysaccharide, and oligosaccharides, a variety of glycosides include iridoid glycoside Class, Catalpol, for iridoid glycosides compound and Dihuang polysaccharide, so using reflux water extraction method.
Radix Astragali: monarch drug in a prescription in the side of being, effective component have an astragaloside, polysaccharide, flavone compound, in order to obtain polysaccharide, institute Using the water extraction method that flows back.
Radices trichosanthis: ministerial drug in the side of being, effective component are saponins, trichosanic acid, polysaccharide etc., in order to obtain polysaccharose substance, So using reflux water extraction method.
Chinese yam: ministerial drug in the side of being, effective component are saponin(e, Chinese yam polysaccharide etc., in order to obtain Chinese yam polysaccharide, so using back Day-to-day drawing method.
Radix Ophiopogonis: ministerial drug in the side of being, effective component are saponins compound, polysaccharide, flavones, in order to obtain polysaccharide, so adopting With reflux water extraction method.
Pueraria lobata: adjutant in the side of being, effective component are daidzin, Puerarin etc., and Puerarin, flows back so using in order to obtain Water extraction method.
Radix Glycyrrhizae: making medicine in the side of being, effective component is liquiritin, glycyrrhizin etc., and glycyrrhizin, flows back so using in order to obtain Water extraction method.
Compared with prior art, beneficial effects of the present invention are as follows: products obtained therefrom of the present invention by the hardness determination of tablet, Friability detection, tablet weight variation, disintegration time limited detection meet pharmacopeia defined, and traditional decoction is changed to tablet, convenient for saving, Transport, patient is easy to receive, and bioavilability is good.
Detailed description of the invention
Fig. 1 is the curve graph of extraction time of the present invention and paste-forming rate；
Fig. 2 is the curve graph of extraction time and paste-forming rate of the invention；
Fig. 3 is the curve graph of the present invention plus water multiple and paste-forming rate.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects It encloses.
Fig. 1-3, the preparation process of glutinous rehmannia Xiaoke Tablets are please referred to, the formula material of glutinous rehmannia Xiaoke Tablets is glutinous rehmannia, Radix Astragali, smallpox Powder, Chinese yam, Radix Ophiopogonis, pueraria lobata, Radix Glycyrrhizae, CMS-Na, dehydrated alcohol, magnesium stearate, filler, comprising the following steps:
Step 1: glutinous rehmannia, Radix Astragali, radices trichosanthis, Chinese yam, Radix Ophiopogonis, pueraria lobata, Radix Glycyrrhizae are cleaned by ultrasonic cleaner, Powder mixing is broken by pulverizer in prescription ratio, is put into Soxhlet extractor, adds 8-12 times of water, refluxing extraction is extracted 1-3 times, 2h is extracted every time, obtains aqueous extract；
Step 2: obtained extracting solution is filtered with suction filtration machine, is concentrated with Rotary Evaporators, concentrate is then put into electric heating In air dry oven, the temperature of electric drying oven with forced convection is 60 DEG C, dry to constant weight, obtains dry extract；
Step 3: taking dry extract and filler to mix in 1: 1,1: 3,1: 5 ratio, and be added appropriate 75-95%'s 1-5% disintegrating agent CMS-Na is added in dehydrated alcohol, is mixed to prepare softwood, crosses 20 mesh medicines sieve, particle is made, is put into electric heating air blast 60 DEG C of dryings in drying box are taken out, and 0.1-0.5% magnesium stearate is added, and are carried out tabletting using tablet press machine, are obtained glutinous rehmannia and quench one's thirst Piece；
Step 4: glutinous rehmannia Xiaoke Tablets 20 are taken at random, is first weighed using assay balance, then calculate average slice weight, it is then accurate The weight for weighing single yellow Xiaoke Tablets, compares single slice weight and average slice weight, detects to the slice weight of glutinous rehmannia Xiaoke Tablets；
Step 5: the hanging basket of instrument being fixed, is put into 1000ml beaker, adjustment hanging basket can be up and down, bottom of the beaker 37 DEG C of temperature of water pours into away from sieve 25mm in portion, allows the water to submergence sieve and the 25mm when highest water surface is higher by sieve highest point, Take glutinous rehmannia Xiaoke Tablets 12 at random, be respectively put into the glass tube of hanging basket, to carry out check glutinous rehmannia Xiaoke Tablets disintegration time limited into Row detection；
Step 6: randomly selecting glutinous rehmannia Xiaoke Tablets 20, check tablet with tablet hardness instrument, detect the hard of glutinous rehmannia Xiaoke Tablets Degree；
Step 7: randomly selecting glutinous rehmannia Xiaoke Tablets 55, the floating powder on surface is blown away with hair dryer, claims its gross mass, is put into piece In the glass cylinder of agent friability instrument, setting revolving speed is 25r/min, is taken out after 4min, then blow away floating powder on surface with hair dryer, is weighed Gross weight calculates the weight of loss, detects to the tablet friability of glutinous rehmannia Xiaoke Tablets；
Step 8: taking dry funnel and funnel is fixed on iron stand, spread a blank sheet of paper in the underface of bell mouth, survey The distance for measuring bell mouth and paper is denoted as H, the particle that granulation obtains slowly is poured into funnel close to hopper walls, until granule Until the vertebral height formed at bell mouth is equal to height of the bell mouth apart from blank sheet of paper, measure what granule was formed in paper Centrum diameter is denoted as R, and the base angle ∠ α of granule cone is calculated according to formula tan α=H/R, and ∠ α is angle of repose, disappears to glutinous rehmannia The angle of repose of thirsty piece is calculated.
The design of extraction process single factor experiment
In order to select preferably extraction factor, successively to the time of extraction, extraction time, Extracting temperature these three factors It investigates, using paste-forming rate as index, finally determines optimal extraction factor.
Glutinous rehmannia, Radix Astragali, radices trichosanthis, Chinese yam, Radix Ophiopogonis, pueraria lobata, Radix Glycyrrhizae break into powder mixing in prescription ratio, add 12 times Water, refluxing extraction extract 2h, extract 1 time respectively, extract 2 times, extract 3 times, are concentrated with Rotary Evaporators, claim the weight of drying basin Amount, then concentrate is poured out and is put into drying basin, and be put into drying box, and drying box temperature is 60 DEG C, drying to constant weight, It takes out and weighs, calculate separately to obtain paste-forming rate.
Paste-forming rate=dry cream amount/medicinal material amount * 100%
Glutinous rehmannia, Radix Astragali, radices trichosanthis, Chinese yam, Radix Ophiopogonis, pueraria lobata, Radix Glycyrrhizae break into powder mixing in prescription ratio, add 12 times of water, Refluxing extraction extracts 60,90,120,150,180min respectively, extracts 2 times, the extracting solution being concentrated to get with Rotary Evaporators, claims The weight of drying basin, then concentrate is poured out be put into drying basin, is put into drying box, and drying box temperature is 60 DEG C, dry To constant weight, takes out and weigh, calculate separately to obtain paste-forming rate.
Paste-forming rate=dry cream amount/medicinal material amount * 100%
Glutinous rehmannia, Radix Astragali, radices trichosanthis, Chinese yam, Radix Ophiopogonis, pueraria lobata, Radix Glycyrrhizae in prescription ratio break into powder mixing, respectively plus 8, 10,12,14 times of water, refluxing extraction extract 2h, extract 2 times, the extracting solution being concentrated to get with Rotary Evaporators, claim drying basin Weight, then concentrate is poured out and is put into drying basin, is put into drying box, drying box temperature is 60 DEG C, dry to constant weight, It takes out and weighs, calculate separately to obtain paste-forming rate.
Paste-forming rate=dry cream amount/medicinal material amount * 100%
Using reflux extraction, selection and withdrawal number (A), extraction time (B) plus water multiple (C) are three factors, design Three levels do 3 factor level tables, and inspection target is paste-forming rate, are tested with L9 (34) orthogonal trial.
Extraction process Orthogonal Experiment and Design
Table 2-4 factor level table
Test serial number Extraction time (A) Extraction time (B) Solid-liquid ratio (C)
1 1 90 1∶10
2 2 120 1∶12
3 3 150 1∶14
It takes dry extract and isomalt to mix in 1: 1,1: 3,1: 5 ratio, and appropriate wetting agent is added 95% ethyl alcohol is added 3% disintegrating agent CMS-Na, is mixed to prepare softwood, crosses 20 meshes, be made particle be put into drying box 60 DEG C it is dry It is dry, it takes out, 0.5% magnesium stearate lubricant is added, influence of the different major ingredient dosages to glutinous rehmannia Xiaoke Tablets quality is investigated in tabletting.
Tablet prepares single factor experiment design
It takes dry extract to add the fillers such as dextrin, lactose, isomalt respectively, is mixed with 1: 3 ratio, and Appropriate 95% ethyl alcohol of wetting agent is added, 3% disintegrating agent CMS-Na is added, is mixed to prepare softwood, crosses 20 meshes, particle is made, puts Enter 60 DEG C of dryings in drying box, take out, 0.5% magnesium stearate lubricant is added, tabletting investigates different fillers and quenches one's thirst to glutinous rehmannia The influence of tablet quality.
Dry extract is mixed with filler, medicinal extract and filler ratio are 1: 3, by mixed powder and various concentration 75%, 85%, 95% ethyl alcohol mixing, is added 3% disintegrating agent CMS-Na, makes softwood, and sieving makes particle, is put into drying 60 DEG C of dryings in case are taken out, and 0.5% magnesium stearate lubricant is added, and tabletting investigates various concentration wetting agent to glutinous rehmannia Xiaoke Tablets matter The influence of amount.
Dry extract is mixed with filler, medicinal extract and filler ratio are 1: 3, by mixed powder respectively with 1%, 2%, 3%, 4%, 5% disintegrating agent CMS-Na mixing, makes softwood, and sieving makes particle, is put into drying box and does for 60 DEG C It is dry, it takes out, adds 0.5% magnesium stearate lubricant, influence of the different disintegrating agent dosages to glutinous rehmannia Xiaoke Tablets quality is investigated in tabletting.
Dry extract is mixed with filler, medicinal extract and filler ratio are 1: 3, and appropriate profit is added in mixed powder 3% disintegrating agent CMS-Na is added in 95% ethyl alcohol of humectant, makes softwood, and sieving makes particle, is put into 60 DEG C of dryings in drying box, Take out, respectively plus 0.1%, 0.2%, 0.3%, 4%, 0.5% magnesium stearate lubricant, tabletting investigates different lubricants and uses Measure the influence to glutinous rehmannia Xiaoke Tablets quality.
Tablet producing technology Orthogonal Experiment and Design
Major ingredient ratio (A), three filler type (B), lubricant quantity (C) factors are chosen, it is excellent according to method of weighting scores Change the preparation process of glutinous rehmannia Xiaoke Tablets.
Table 2-1 factor level table
Test serial number Major ingredient dosage (A) Filler type (B) Lubricant quantity (C)
1 1∶1 Dextrin 3%
2 1∶3 Isomalt 5%
3 1∶5 Microcrystalline cellulose 7%
Extraction process single factor experiment result and analysis
Influence of the table 3-1 extraction time to paste-forming rate
Extraction time 1 2 3
Paste-forming rate % 28.67 31.12 31.21
Paste-forming rate is affected by extraction time known to table 3-1 data, and paste-forming rate when extracting one time is minimum, extracts two Paste-forming rate when secondary rises, when extracting three times paste-forming rate be improved but seldom, almost highest availability, therefore optimal mention Taking number is 2 times.
Influence of the table 3-2 extraction time to paste-forming rate
Extraction time min 60 90 120 150 180
Paste-forming rate % 25.40 28.81 31.39 31.48 31.45
Paste-forming rate is affected by extraction time known to table 3-2, and the time increases paste-forming rate and is also gradually increased, and extracts 1h's Paste-forming rate is minimum, extracts the paste-forming rate highest of 2.5h, and paste-forming rate starts to stablize after extracting 2h, no longer increases, therefore extracts best Extraction time is 2h.
Table 3-3 adds influence of the water multiple to paste-forming rate
Add water multiple 8 10 12 14
Paste-forming rate 30.15 30.82 31.18 31.24
Can be it is found that with the increase for adding water multiple by surface 3-3, paste-forming rate also gradually rises, when adding water multiple to reach 12 After times, paste-forming rate tends towards stability, therefore 12 times of water is added to be most preferably to add water multiple.
Extraction process orthogonal experiments and analysis
The intuitive analytical table of table 3-4
Serial number Extraction time Extraction time Add water multiple Blank Paste-forming rate
Test 1 1 1 1 1 11.21%
Test 2 1 2 2 2 19.6%
Test 3 1 3 3 3 11.29%
Test 4 2 1 2 3 29.69%
Test 5 2 2 3 1 31.27%
Test 6 2 3 1 2 30.82%
Test 7 3 1 3 2 30.54%
Test 8 3 2 1 3 31.12%
Test 9 3 3 2 1 30.34%
K1 14.060 23.813 24.383 24.273
K2 30.553 27.357 26.570 27.013
K3 30.567 24.150 24.367 24.033
R 16.607 3.544 2.203 2.980
Table 3-5 analysis of variance table
Processing Sum of square of deviations Freedom degree It is square F value Conspicuousness
Number (A) 549.138 2 274.569 33.391 *
Time (B) 22.951 2 11.476 1.396
Solid-liquid ratio (C) 9.636 2 4.818 0.886
Error 6.446 2 1.297
Infuse F(0.05)=19.0 F(0.01)=99.0
From variance analysis as can be seen that the extraction factor for influencing paste-forming rate size is followed successively by A > B > C, wherein factor A is mentioned Take times influence very significant, factor B extraction time influence it is smaller, factor C add water multiple influence not significant, A3B2C2Extraction process It is more excellent, but variable quantity is seldom, it is contemplated that and time and cost finally determine that optimal extraction process is A2B2C2That is extraction time 2 Secondary, extraction time 90min, 12 times of amount of water are optimum extraction process.
Tablet producing technology single factor experiment result and analysis
The selection of table 3-6 major ingredient dosage and result
Proportion of main and supplementary materials Disintegration time limited (min) Mouthfeel Appearance Weighted scoring
1∶1 12.2 6.8 5.4 5.4
1∶3 13.5 8.6 7.9 8.3
1∶5 13.8 8.1 8.2 8.1
1: 1 and 1: 3 is all proper ratio known to table 3-6, and tabletting flat appearance is smooth, it is contemplated that this product mouthfeel, so Select proportion of main and supplementary materials 1: 3 for optimal proportion.
The selection of table 3-7 filler type and result
Filler type Disintegration time limited Mouthfeel Appearance Weighted scoring
Dextrin 12.6 2.9 8.1 3.2
Microcrystalline cellulose 12.1 3.1 8.0 3.5
Isomalt 13.3 8.8 8.2 8.6
By table 3-7 it is found that three kinds of filler mouldabilities are not much different, it is contemplated that experimental design background, so selecting different wheat Bud ketose alcohol is best packing material.
The selection of table 3-8 wetting agent and result
Concentration of wetting agent % Disintegration time limited min Ratio of briquetting % Weight score
75 15.37 78% 7.5
85 15.63 83% 8.2
95 15.88 91% 8.7
By table 3-9 it is found that being most suitable for granulation using the softwood that the ethyl alcohol of 95% concentration is made.
The influence result of table 3-9 disintegrating agent dosage
Disintegrating agent dosage % Disintegration time limited min Ratio of briquetting % Weight score
1 17.7 74 7.1
2 15.4 78 7.5
3 13.6 89 8.1
4 11.2 87 7.9
5 9.9 77 7.3
By table 3-9 it is found that with disintegrating agent dosage raising, disintegration time is declined, but the excessively high meeting of disintegrating agent dosage Tablet compactibility energy is influenced, so selecting 3% sodium carboxymethyl starch for optimal proportion.
Tablet producing technology orthogonal experiments and analysis
The intuitive analytical table of table 3-10
Table 3-11 analysis of variance table
Factor Sum of square of deviations Freedom degree It is square F value Conspicuousness
A 2.645 2 1.323 44.117 *
B 1.647 2 0.824 27.450 *
C 1.807 2 0.904 30.117 *
D 0.060 2 0.030 1.000
Error 0.06 2 0.03
Three factors all have a significant impact the preparation process of glutinous rehmannia Xiaoke Tablets it can be seen from table 3-11, influence power Size is followed successively by A > C > B, wherein A2B2C3Score highest, that is, uses 1: 3 main and supplementary materials ratio, filled using isomalt Agent is added 0.5% magnesium stearate and does lubricant, is that optimal glutinous rehmannia is quenched one's thirst piece preparation method.
The quality examination result of glutinous rehmannia Xiaoke Tablets
Table 3-12 organoleptic detection result table
Learn that glutinous rehmannia Xiaoke Tablets appearance is glossy by table 3-10, without slight crack, uniform color is complied with standard.
Table 3-13 weight differential result table
Serial number Serial number
1 0.121 11 0.122
2 0.117 12 0.115
3 0.124 13 0.119
4 0.129 14 0.121
5 0.121 15 0.117
6 0.125 16 0.124
7 0.131 17 0.126
8 0.118 18 0.118
9 0.119 19 0.127
10 0.124 20 0.114
Table 3-14 limit test of weight variation table
Slice weight Limit test of weight variation
0.12g ± 7.5%
Average slice weight=0.12g
It is compared by table 3-11 and 3-12 it is found that meeting the weight differential standard of " pharmacopeia " defined.
Table 3-15 disintegration time limited result table
Serial number 1 group 2 groups
1 13.5 12.8
2 11.2 12.3
3 13.6 13.8
4 12.4 14.2
5 12.8 14.4
6 13.6 13.4
Average (min) 12.85 13.48
By disintegration time limited known to table 3-13 all in 15min, and disintegration time meets pharmacopeia specification greater than 10min.
Table 3-16 Determination of Hardness table
Hardness is in 4-6kg/cm2 known to table 3-14, and by consulting related data, the hardness of general plain piece is in 2-6kg/ Cm2, hardness is preferable, meets regulation.
55 are extracted from glutinous rehmannia Xiaoke Tablets obtained at random, the quality for blowing away floating powder is 6.187g, is placed in tablet friability The quality of tablet is 6.136g after instrument, and the quality for calculating loss is 0.9%, meets States Pharmacopoeia specifications about the rule of tablet friability It is fixed, it meets the requirements.
The angle of repose table 3-17 testing result table
Serial number Stearic acid magnesium amount (%) Angle of repose (°) Weight score
1 0.1 33.26 7.1
2 0.3 32.54 7.5
3 0.5 30.88 8.2
4 0.7 30.46 8.0
5 0.9 30.23 7.3
By table 3-3 it is found that the dosage with lubricant increases, the degree at angle of repose is smaller and smaller, so particle in lozenge Mobility it is better, but with magnesium stearate content increase lozenge taste bad, so select be added 0.5% it is hard Fatty acid magnesium is optimal proportion.
It is 0.12 gram that calculating, which learns that glutinous rehmannia Xiaoke Tablets are averaged in piece, and proportion of main and supplementary materials 1: 3 can be calculated according to ratio and know Average every glutinous rehmannia Xiaoke Tablets formula extraction dry extract containing group: 0.12g*1/4=0.03g.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding And modification, the scope of the present invention is defined by the appended.

Claims (3)

1. the preparation process of glutinous rehmannia Xiaoke Tablets, the formula material of glutinous rehmannia Xiaoke Tablets be glutinous rehmannia, Radix Astragali, radices trichosanthis, Chinese yam, Radix Ophiopogonis, Pueraria lobata, Radix Glycyrrhizae, CMS-Na, dehydrated alcohol, magnesium stearate, filler, it is characterised in that: the following steps are included:
Step 1: glutinous rehmannia, Radix Astragali, radices trichosanthis, Chinese yam, Radix Ophiopogonis, pueraria lobata, Radix Glycyrrhizae being cleaned by ultrasonic cleaner, by group Square ratio breaks into powder mixing by pulverizer, is put into Soxhlet extractor, adds 8-12 times of water, and refluxing extraction extracts 1-3 It is secondary, 2h is extracted every time, obtains aqueous extract；
Step 2: obtained extracting solution is filtered with suction filtration machine, is concentrated with Rotary Evaporators, concentrate is then put into electric heating air blast In drying box, the temperature of electric drying oven with forced convection is 60 DEG C, dry to constant weight, obtains dry extract；
Step 3: taking dry extract and filler to mix in the ratio of 1:1,1:3,1:5, and the anhydrous of appropriate 75-95% is added 1-5% disintegrating agent CMS-Na is added in ethyl alcohol, is mixed to prepare softwood, crosses 20 mesh medicines sieve, particle is made, is put into electric heating forced air drying 60 DEG C of dryings in case are taken out, and 0.1-0.5% magnesium stearate is added, and are carried out tabletting using tablet press machine, are obtained glutinous rehmannia Xiaoke Tablets；
Step 4: taking glutinous rehmannia Xiaoke Tablets 20 at random, first weighed using assay balance, then calculate average slice weight, then precision weighing The weight of single Huang Xiaoke Tablets, compares single slice weight and average slice weight, detects to the slice weight of glutinous rehmannia Xiaoke Tablets；
Step 5: the hanging basket of instrument is fixed, is put into 1000ml beaker, adjustment hanging basket can be up and down, beaker bottom away from Sieve 25mm pours into 37 DEG C of temperature of water, allows the water to submergence sieve and the 25mm when highest water surface is higher by sieve highest point, at random Glutinous rehmannia Xiaoke Tablets 12 are taken, is respectively put into the glass tube of hanging basket, is examined to inspection glutinous rehmannia Xiaoke Tablets disintegration time limited is carried out It surveys；
Step 6: randomly selecting glutinous rehmannia Xiaoke Tablets 20, check tablet with tablet hardness instrument, detect the hardness of glutinous rehmannia Xiaoke Tablets；
Step 7: randomly selecting glutinous rehmannia Xiaoke Tablets 55, the floating powder on surface is blown away with hair dryer, claims its gross mass, it is crisp to be put into tablet In the glass cylinder of broken instrument, setting revolving speed is 25r/min, is taken out after 4min, then blow away floating powder on surface with hair dryer, is weighed total Weight, calculates the weight of loss, detects to the tablet friability of glutinous rehmannia Xiaoke Tablets；
Step 8: taking dry funnel and funnel is fixed on iron stand, spread a blank sheet of paper in the underface of bell mouth, measure The distance of bell mouth and paper is denoted as H, the particle that granulation obtains slowly is poured into funnel close to hopper walls, until granule is leaking Until the vertebral height formed at quarrel is equal to height of the bell mouth apart from blank sheet of paper, the centrum that granule is formed in paper is measured Diameter is denoted as R, the base angle ∠ α of granule cone is calculated according to formula tan α=H/R, ∠ α is angle of repose, to glutinous rehmannia Xiaoke Tablets Angle of repose calculated.
2. the preparation process of glutinous rehmannia Xiaoke Tablets according to claim 1, it is characterised in that: the filler can be dextrin Or lactose or isomalt.
3. the preparation process of glutinous rehmannia Xiaoke Tablets according to claim 1, it is characterised in that: the step 4,5,6 and 7 are logical Tablet four is crossed to be detected with detector.
CN201910695170.9A 2019-07-30 2019-07-30 The preparation process of glutinous rehmannia Xiaoke Tablets Pending CN110354202A (en)

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Application publication date: 20191022