CN1799622A - Mind-tranquilizing brain-replenishing soft capsule, its preparation process and quality control method - Google Patents
Mind-tranquilizing brain-replenishing soft capsule, its preparation process and quality control method Download PDFInfo
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- CN1799622A CN1799622A CN 200510200006 CN200510200006A CN1799622A CN 1799622 A CN1799622 A CN 1799622A CN 200510200006 CN200510200006 CN 200510200006 CN 200510200006 A CN200510200006 A CN 200510200006A CN 1799622 A CN1799622 A CN 1799622A
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Abstract
The invention provides a soft capsule for calming the nerves and nourishing the brain, which is prepared from concrete powder, suspension auxiliary agent and light-screening agent. The invention also discloses the process for preparing the soft capsule and its quality control method.
Description
Technical field
The present invention relates to a kind of Chinese medicinal soft capsule and preparation method thereof and method of quality control, belong to the field of Chinese medicines.
Background technology
The 3rd Chinese patent medicine kind---ANSHEN BUNAO YE of recording of " Drug Standard of Ministry of Public Health of the Peoples Republic of China " (Chinese traditional patent formulation preparation) has spermatogenesis and mends marrow, strengthens mental effect, be used for the neurasthenia, insomnia, forgetful, headache has been widely used in clinically, and comparatively ideal effect is arranged.
But also there is following deficiency:
1, the effect duration of oral liquid shorter, effective ingredient exists with liquid, easily microbiological contamination;
2, oral liquid long term storage instability is prone to precipitation.
3, oral liquid is had relatively high expectations to clarity, and yield rate is low.
And this product is changed system into soft capsule, then following benefit can be arranged:
1, after taking disintegrate in vivo, can directly absorb at intestinal, absorb soon the bioavailability height;
2, good stability, with gelatin system epithelium, air-tightness is strong, capsule intensity and film barrier property height, but content stable for extended periods of time;
3, mostly soft capsule is medicine dissolution, suspendible, is emulsified in the solvent, is filled in the capsule as content after making its solution that becomes uniformity, and every capsules contained drug error is little;
4, covered the bad smell of medicine; Taking convenience;
5, the color of film, capsule, transparency, glossiness all can freely be selected, and compare with other roundel goods, and gloss appearance is good.
Soft capsule is the soft good way that addresses the above problem, but because soft capsule is applied to monomer component always is main chemical drugs or health product, it is still immature to be applied to Chinese medicine, the preparation that is applied to the Chinese and Western compound medicine is more in distress, degree is consulted document and is not also found the relevant technical clarification that " ANSHEN BUNAO YE " made soft capsule, thereby must study at prescription, solve correlation technique problems such as its shaping, stability, drug loading.
Summary of the invention
The objective of the invention is to solve the problem that exists on the existing soft capsule forming technique, the Anshen Bunao soft capasule of a kind of safe in utilization, steady quality, evident in efficacy, taking convenience is provided.
Purpose of the present invention is implemented by the following technical programs:
One. the preparation method of Anshen Bunao extract powder: get Rhizoma Zingiberis 125 unit of weights, add 8 times of water gagings, vapor distillation extracted 5 hours, and the decocting liquid after volatile oil and distillation device is in addition preserved standby; Get medicinal residues and Radix Polygoni Multiflori Preparata 625 unit of weights of Rhizoma Zingiberis, Herba Epimedii 500 unit of weights, Radix Glycyrrhizae 62.5 unit of weights, four flavors such as Fructus Jujubae 125 unit of weights, adding 8 times of water gagings respectively decocts three times, 2 hours for the first time, second, three times each 1 hour, filter, merging filtrate, filtrate adds the ginger ale decocting liquid, (75 ± 5 ℃ of concentrating under reduced pressure,-during 0.08MPa) to relative density 1.12～1.15 (60 ℃), add ethanol and make determining alcohol reach 65%, fully stir, left standstill 48 hours, filter, decompression filtrate recycling ethanol (75 ± 5 ℃ ,-0.08MPa), and continue concentrating under reduced pressure (75 ± 5 ℃ ,-0.08MPa) to the extractum of relative density 1.10～1.15 (60 ℃); Get Cornu Cervi Pantotrichum 30 unit of weights, adding 6 times of water gagings respectively decocts five times, time was followed successively by 4,4,3,3,2 hours, filtered merging filtrate, (75 ± 5 ℃ of concentrating under reduced pressure,-0.08MPa) to 1/2 of crude drug in whole, add Cera Flava, leave standstill solidify fully to the wax layer after, remove the dewax layer, filter, filtrate adds 4 times of amount 80% ethanol, mixing, room temperature left standstill 48 hours, filter, decompression filtrate recycling ethanol (75 ± 5 ℃ ,-0.08MPa), and continue concentrating under reduced pressure (75 ± 5 ℃ ,-0.08MPa) to the extractum of relative density 1.10～1.15 (60 ℃); Merge above-mentioned extractum, mix homogeneously, spray drying (170～180 ℃ of inlet temperature, 90～100 ℃ of leaving air temps), dry extract adds Rhizoma Zingiberis volatile oil and vitamin B
1The fine powder mixing of 5 unit of weights, promptly.
Two, the selection of each ingredient: the inventor obtains following result after primary election:
Softgel shell is made up of the raw material of following weight ratio: gelatin 80～120, glycerol 30～60, water 80～120, polyhydric alcohol 8～16 or Polyethylene Glycol 5～15, iron oxide red or iron oxide black 0.5～5, sodium pyrosulfite 1～10, ethyl hydroxybenzoate 0.1～0.5.
Capsule liquid is made up of the raw material of following weight ratio: Anshen Bunao extract powder 2000～4000, vegetable oil or Macrogol 2000～4000, Cera Flava or propylene glycol 20～200, ethyl hydroxybenzoate 0.5～3.
In order to make better product, the inventor has done further preferred work:
Three. the selection of Anshen Bunao soft capasule capsule liquid composition: capsule liquid is made up of Anshen Bunao extract powder effective dose and diluent, screens the kind and the ratio of diluent by experiment.(T=25 ± 2 ℃, RH=50～70%) successive stability test carries out at ambient temperature to adopt room temperature reserved sample observing method.
Get Anshen Bunao extract powder 2600 weight portions, slowly add in the vegetable oil of 3900 weight portions, constantly stir, cross 100 mesh sieves behind the mix homogeneously, drop in the soft capsule production filling machine and be pressed into soft gelatin capsule, drying, promptly.The method capsule liquid material fluidity is better, and pouring process is more easily realized, but finished product stability is relatively poor, promptly occurs the stratified phenomenon of capsule liquid behind the compaction drying, does not satisfy the requirement of pharmacopeia to soft capsule preparation stability.
Get the vegetable oil of 3830 weight portions, be heated to 60 ℃～70 ℃ insulations, get Cera Flava 70 weight portions and cut into pieces, add in the vegetable oil, insulated and stirred makes dissolving.Other gets in the Anshen Bunao extract powder 2600 weight portions adding vegetable oil solution, crosses 100 mesh sieves behind the mix homogeneously, and drop in the soft capsule production filling machine and be pressed into soft gelatin capsule, drying, promptly.The method capsule liquid material fluidity is better, pouring process realizes that more easily finished product stability improves a lot, but part capsule liquid has lamination in 1 week, tangible lamination all appears in most of soft capsule after January, does not satisfy the requirement of pharmacopeia to soft capsule preparation stability.
Get the vegetable oil of 3750 weight portions, be heated to 60 ℃～70 ℃ insulations, get Cera Flava 150 weight portions and cut into pieces, add in the vegetable oil, insulated and stirred makes dissolving.Other gets in the Anshen Bunao extract powder 2600 weight portions adding vegetable oil solution, crosses 100 mesh sieves behind the mix homogeneously, and drop in the soft capsule production filling machine and be pressed into soft gelatin capsule, drying, promptly.The method capsule liquid Flow of Goods and Materials sexual satisfaction fill requirement, finished product stability is good, through the room temperature reserved sample observing, capsule liquid lamination do not occur, and satisfies the requirement of pharmacopeia to soft capsule preparation stability in 1 year half.
Get the vegetable oil of 3700 weight portions, be heated to 60 ℃～70 ℃ insulations, get Cera Flava 200 weight portions and cut into pieces, add in the vegetable oil, insulated and stirred makes dissolving.Other gets in the Anshen Bunao extract powder 2600 weight portions adding vegetable oil solution, crosses 100 mesh sieves behind the mix homogeneously, drops into soft capsule and produces compacting glue ball in the filling machine.The method capsule liquid material fluidity is relatively poor, thickness very at room temperature, and obstruction in various degree appears in the soft capsule filling machine, can't finish fill smoothly, does not satisfy the big needs of producing.
Taking polyethylene glycol 3600 weight portions and propylene glycol 300 weight portion mix homogeneously are heated to 60 ℃～70 ℃ insulations, and other gets the adding of Anshen Bunao extract powder 2600 weight portions, cross 100 mesh sieves behind the mix homogeneously, drop into soft capsule and produce compacting glue ball in the filling machine.The method has obtained result preferably.
According to above a large amount of experimentation, determine that the weight composition of Anshen Bunao soft capasule capsule liquid of the present invention can be: Anshen Bunao extract powder 2600, vegetable oil 3750, Cera Flava 150.
Corresponding preparation technology is: get the vegetable oil of 3750 weight portions, be heated to 60 ℃～70 ℃ insulations, get Cera Flava 150 weight portions and cut into pieces, add in the vegetable oil, insulated and stirred makes dissolving.Other gets in the Anshen Bunao extract powder 2600 weight portions adding vegetable oil solution, crosses 100 mesh sieves behind the mix homogeneously, and drop in the soft capsule production filling machine and be pressed into soft gelatin capsule, drying, promptly.
The weight of capsule liquid is formed: Anshen Bunao extract powder 2600, Polyethylene Glycol 3600, propylene glycol 300.
Corresponding preparation technology is: taking polyethylene glycol and mixed with propylene glycol are even, are heated to 60 ℃～70 ℃ insulations, and other gets the extract powder adding, cross 100 mesh sieves behind the mix homogeneously, make soft capsule liquid.
Four. the selection that the Anshen Bunao soft capasule softgel shell is formed: softgel shell consists of basis by glycerol, gelatin, screens the influence of other formulated component to preparation stability by experiment.(T=25 ± 2 ℃, RH=50～70%) successive stability test carries out at ambient temperature to adopt room temperature reserved sample observing method.
1) gets gelatin 100 weight portions, add in the stirring appropriate amount of purified water down, stablely be controlled at 70 ℃～80 ℃ constantly stirrings.After treating that gelatin dissolves fully, add 30 weight portion glycerol, iron oxide red and ethyl hydroxybenzoate mix homogeneously, vacuum deaerator after the insulated and stirred, promptly.Glue is injected soft capsule produce filling machine under keeping warm mode, be drawn into rubber, the compacting capsule.The soft capsule shell that the method makes is harder, and is cracked easily after the drying.
2) get gelatin 100 weight portions, add in the stirring appropriate amount of purified water down, stablely be controlled at 70 ℃～80 ℃ constantly stirrings.After treating that gelatin dissolves fully, add 40 weight portion glycerol, iron oxide red and ethyl hydroxybenzoate mix homogeneously, vacuum deaerator after the insulated and stirred, promptly.Glue is injected soft capsule produce filling machine under keeping warm mode, be drawn into rubber, the compacting capsule.The soft capsule shell that the method makes is neither too hard, nor too soft, and dry back disintegration time was at 20 minutes～30 minutes; Behind the preparation 6 months, disintegration time was at 40 minutes～50 minutes; Preparation after 1 year disintegration time exceed qualified boundary line 60 minutes.
3) get gelatin 100 weight portions, add in the stirring appropriate amount of purified water down, stablely be controlled at 70 ℃～80 ℃ constantly stirrings.After treating that gelatin dissolves fully, add sorbitol, iron oxide red and the ethyl hydroxybenzoate mix homogeneously of 30 weight portion glycerol, 12 weight portions, vacuum deaerator after the insulated and stirred, promptly.Glue is injected soft capsule produce filling machine under keeping warm mode, be drawn into rubber, the compacting capsule.The soft capsule shell that the method makes is neither too hard, nor too soft, and dry back disintegration time was at 20 minutes～25 minutes; Behind the preparation 6 months, disintegration time was at 30 minutes～40 minutes; Preparation after 1 year disintegration time be 55 minutes, preparation 1 year half back disintegration time exceeds qualified boundary line 60 minutes.
4) get gelatin 100 weight portions, add in the stirring appropriate amount of purified water down, stablely be controlled at 70 ℃～80 ℃ constantly stirrings.After treating that gelatin dissolves fully, add PEG400, iron oxide red and the ethyl hydroxybenzoate mix homogeneously of 30 weight portion glycerol, 10 weight portions, vacuum deaerator after the insulated and stirred, promptly.Glue is injected soft capsule produce filling machine under keeping warm mode, be drawn into rubber, the compacting capsule.The soft capsule shell that the method makes is neither too hard, nor too soft, and dry back disintegration time was at 15 minutes～25 minutes; Behind the preparation 6 months, disintegration time was at 30 minutes～40 minutes; Preparation after 1 year disintegration time be 55 minutes, preparation 1 year half back disintegration time exceeds qualified boundary line 60 minutes.
5) get gelatin 100 weight portions, add in the stirring appropriate amount of purified water down, stablely be controlled at 70 ℃～80 ℃ constantly stirrings.After treating that gelatin dissolves fully, add the sorbitol of 30 weight portion glycerol, 12 weight portions, sodium pyrosulfite, iron oxide red and the ethyl hydroxybenzoate mix homogeneously of 2.5 quantity parts, vacuum deaerator after the insulated and stirred, promptly.Glue is injected soft capsule produce filling machine under keeping warm mode, be drawn into rubber, the compacting capsule.The soft capsule shell that the method makes is neither too hard, nor too soft, and dry back disintegration time was at 20 minutes～25 minutes; Behind the preparation 6 months, disintegration time was at 25 minutes～30 minutes; Preparation after 1 year disintegration time be 30 minutes, preparation 1 year half back disintegration time is 35 minutes.
5) get gelatin 100 weight portions, add in the stirring appropriate amount of purified water down, stablely be controlled at 70 ℃～80 ℃ constantly stirrings.After treating that gelatin dissolves fully, add the PEG400 of 30 weight portion glycerol, 10 weight portions, sodium pyrosulfite, iron oxide red and the ethyl hydroxybenzoate mix homogeneously of 2.5 quantity parts, vacuum deaerator after the insulated and stirred, promptly.Glue is injected soft capsule produce filling machine under keeping warm mode, be drawn into rubber, the compacting capsule.The soft capsule shell that the method makes is neither too hard, nor too soft, and dry back disintegration time was at 15 minutes～25 minutes; Behind the preparation 6 months, disintegration time was at 25 minutes～30 minutes; Preparation after 1 year disintegration time be 30 minutes, preparation 1 year half back disintegration time is 35 minutes.
According to above a large amount of experimentation, determine that the weight of Anshen Bunao soft capasule softgel shell of the present invention consists of: gelatin 100, glycerol 30, water 90, sorbitol 12 or Polyethylene Glycol 10, iron oxide red or iron oxide black 2.5, sodium pyrosulfite 2.5, ethyl hydroxybenzoate 0.2.Replace glycerol with part sorbitol or PEG400 in the capsule shells rubber, can well keep the water balance in the rubber, the disintegration time of soft capsule is shortened, be beneficial to this product and absorb; The sodium pyrosulfite that adds in the capsule shells rubber is an antioxidant, can well keep soft capsule shell not by the oxidation of airborne oxygen institute, and stability of formulation has been improved greatly.
By the above-mentioned selected optimum capsule liquid and the prescription and the method for making of softgel shell, on encapsulating machine, it is pressed into soft capsule.
After the Anshen Bunao oral liquid is made soft capsule, former stability of formulation is strengthened greatly, guaranteed the quality of this medicine, safe in utilization, evident in efficacy, it is oral to be convenient to the patient, cuts easy to carry.
The specific embodiment
Embodiment 1:
Get vegetable oil 3750g, be heated to 60 ℃～70 ℃ insulations, get Cera Flava 150g and cut into pieces, add in the vegetable oil, stir and make dissolving, get extract powder 2600g and add in the vegetable oil solution, cross 100 mesh sieves behind the mix homogeneously, make medicinal liquid.Get gelatin 10Kg, add in the stirring 9Kg pure water down, stablely be controlled at 40 ℃～50 ℃ constantly stirrings.After treating that gelatin dissolves fully, add glycerol 4kg, sorbitol 1.2Kg, Polyethylene Glycol 1Kg, iron oxide red 250g, sodium pyrosulfite 250g and ethyl hydroxybenzoate 200g mix homogeneously, insulated and stirred is made the capsule material.Above-mentioned medicinal liquid and capsule material are pressed into 10000 of soft capsules on the soft capsule press.
Embodiment 2:
Taking polyethylene glycol 3600g, propylene glycol 300g mix homogeneously is got extract powder 2600g and is added, and crosses 100 mesh sieves behind the mix homogeneously, makes medicinal liquid.Get gelatin 10Kg, add in the stirring 9Kg pure water down, stablely be controlled at 40 ℃～50 ℃ constantly stirrings.After treating that gelatin dissolves fully, add glycerol 4kg, sorbitol 1.2Kg, Polyethylene Glycol 1Kg, iron oxide red 250g, sodium pyrosulfite 250g and ethyl hydroxybenzoate 200g mix homogeneously, insulated and stirred is made the capsule material.Above-mentioned medicinal liquid and capsule material are pressed into 10000 of soft capsules on the soft capsule press.
Embodiment 3:
Qualitative identification
Get this product content 5g, add methanol 25ml, supersound process 30 minutes filters, filtrate evaporate to dryness, residue add water 20ml makes dissolving, with the Petroleum ether extraction secondary, and each 15ml, discard petroleum ether liquid, water liquid adds hydrochloric acid 2ml, chloroform 20ml, water-bath reflux, extract, 1 hour is chilled to room temperature, puts in the separatory funnel, divide and get chloroform layer, water liquid extracts once with chloroform 15ml, combined chloroform liquid, evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution.It is an amount of that other gets the emodin reference substance, adds dissolve with methanol and make the reference substance solution that every 1ml contains 0.5mg.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2000 B) test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with toluene-ethanol (4: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
Get this product content 5g, add methanol 25ml, supersound process 30 minutes, filter, filtrate evaporate to dryness, residue add water 20ml makes dissolving, put in the separatory funnel, with the ether extraction secondary, each 20ml, discard ether solution, water liquid extracts three times with water-saturated n-butanol, each 15ml, merge n-butyl alcohol liquid, evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution.It is an amount of that other gets the icariin reference substance, adds dissolve with methanol and make the reference substance solution that every 1ml contains 0.5mg.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2000 B) test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ethyl acetate-butanone-formic acid-water (10: 3: 1: 1) be developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Assay
(1) 2,3,5,4 '-assay of tetrahydroxystilbene-2-O-β-D-glucoside measures according to high performance liquid chromatography (" an appendix VI of Chinese pharmacopoeia version in 2000 D).
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Is acetonitrile looked into? 4: 86) be mobile phase; Flow velocity 1.0ml/min, 25 ℃ of column temperatures, the detection wavelength is 320nm.Number of theoretical plate by 2,3,5,4 '-tetrahydroxystilbene-2-O-β-D-glucoside peak calculates, and should be not less than 2000.
The preparation precision of reference substance solution takes by weighing 2,3,5,4 '-tetrahydroxystilbene-2-O-β-D-glucoside reference substance is an amount of, and add the mobile phase dissolving and make the reference substance solution that every 1ml contains 15 μ g, promptly.
This product content under the content uniformity item is got in the preparation of need testing solution, grinds well, and takes by weighing 1g, the accurate title, decide, and puts in the apparatus,Soxhlet's, and it is an amount of to add petroleum ether, reflux 1 hour discards petroleum ether liquid, and medicinal residues are flung to petroleum ether, shred, put in the tool plug conical flask, precision adds Diluted Alcohol 100ml, close plug claims to decide weight, supersound process (250W, 50kHz) 30 minutes, put coldly, claim to decide weight again, supply the weight that subtracts mistake with Diluted Alcohol, shake up, filter, precision is measured subsequent filtrate 2ml, put in the 10ml measuring bottle, add mobile phase, shake up to scale, filter with microporous filter membrane (0.45 μ m), promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Every of this product contains Radix Polygoni Multiflori Preparata with 2,3,5,4 '-tetrahydroxystilbene-2-O-β-D-glucoside (C
20H
22O
9) meter, must not be less than 3.75mg.
(2) vitamin B
1Assay measure according to high performance liquid chromatography (" an appendix VI of Chinese pharmacopoeia version in 2000 D).
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile-aqueous solution (glacial acetic acid 10ml and water 200ml, jolting makes dissolving, adds water to 1000ml for sodium lauryl sulphate 0.4g, triethylamine 2ml) (34: 66) is a mobile phase; Flow velocity 1.0ml/min, 40 ℃ of column temperatures, the detection wavelength is 246nm.Number of theoretical plate is pressed vitamin B
1The peak calculates, and should be not less than 2000.
The preparation precision of reference substance solution takes by weighing vitamin B
1Reference substance is an amount of, adds the mobile phase dissolving and makes the reference substance solution that every 1ml contains 20 μ g, promptly.
This product content under the content uniformity item is got in the preparation of need testing solution, grinds well, and takes by weighing 1g, the accurate title, decide, and puts in the apparatus,Soxhlet's, and it is an amount of to add petroleum ether, reflux 1 hour discards petroleum ether liquid, and medicinal residues are flung to petroleum ether, shred, put in the 100ml measuring bottle, add water 100ml, close plug, supersound process (250W, 50kHz) 30 minutes, put cold, add water to scale, shake up, filter, precision is measured subsequent filtrate 2ml, put in the 10ml measuring bottle, add mobile phase, shake up to scale, filter with microporous filter membrane (0.45 μ m), promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Every of this product contains vitamin B
1Should be 4.5～5.5mg.
Claims (10)
1. Anshen Bunao soft capasule, form by softgel shell and capsule liquid, capsule liquid is made up of Anshen Bunao extract powder and adjuvant, it is characterized in that what softgel shell was made up of the raw material of following weight ratio: gelatin 80～120, glycerol 30～60, water 80～120, polyhydric alcohol 8～16 or Polyethylene Glycol 5～15, iron oxide red or iron oxide black 0.5～5, sodium pyrosulfite 1～10, ethyl hydroxybenzoate 0.1～0.5; Capsule liquid is made up of the raw material of following weight ratio: Anshen Bunao extract powder 2000～4000, vegetable oil or Macrogol 2000～4000, Cera Flava or propylene glycol 20～200, ethyl hydroxybenzoate 0.5～3.
2. Anshen Bunao soft capasule as claimed in claim 1 is characterized in that what softgel shell was made up of the raw material of following weight ratio: gelatin 100, glycerol 30, water 90, sorbitol 12 or Polyethylene Glycol 10, iron oxide red or iron oxide black 2.5, sodium pyrosulfite 2.5, ethyl hydroxybenzoate 0.2.
3. Anshen Bunao soft capasule as claimed in claim 2 is characterized in that what capsule liquid was made up of the raw material of following weight ratio: Anshen Bunao extract powder 2600, vegetable oil 3750, Cera Flava 150.
4. Anshen Bunao soft capasule as claimed in claim 2 is characterized in that what capsule liquid was made up of the raw material of following weight ratio: Anshen Bunao extract powder 2600, Polyethylene Glycol 3600, propylene glycol 300.
5. the preparation method of the described Anshen Bunao soft capasule of claim 3 is characterized in that comprising following steps:
A. get vegetable oil and be heated to 60 ℃～70 ℃ insulations.
B. get Cera Flava and cut into pieces, add in the vegetable oil, stir and make dissolving.
C. get extract powder in addition and add in the vegetable oil solution, cross 100 mesh sieves behind the mix homogeneously, make soft capsule liquid.
6. the preparation method of the described Anshen Bunao soft capasule of claim 4 is characterized in that comprising following steps:
A. taking polyethylene glycol and mixed with propylene glycol are even, are heated to 60 ℃～70 ℃ insulations.
B. get extract powder in addition and add, cross 100 mesh sieves behind the mix homogeneously, make soft capsule liquid.
7. as the preparation method of claim 5 or 6 described Anshen Bunao soft capasules, it is characterized in that also comprising following steps:
A. get gelatin 100 weight portions, add in the stirring appropriate amount of purified water down, stablely be controlled at 70 ℃～80 ℃ constantly stirrings.
B. after treating that gelatin dissolves fully, add glycerol, sorbitol, Polyethylene Glycol-400, iron oxide red or iron oxide black, sodium pyrosulfite and ethyl hydroxybenzoate mix homogeneously, insulated and stirred.
C. with the glue vacuum deaerator after the insulated and stirred, make soft capsule shell.
8. the preparation method of Anshen Bunao soft capasule as claimed in claim 7 is characterized in that also comprising the steps: soft capsule liquid and the softgel shell compression moulding on encapsulating machine that will make.
9. the method for quality control of Anshen Bunao soft capasule as claimed in claim 1, one or more that it is characterized in that adopting following method are differentiated:
A. get the capsule liquid of soft capsule of the present invention, add the methanol supersound process, filter, filtrate evaporate to dryness, residue add water makes dissolving, with the Petroleum ether extraction secondary, discard petroleum ether liquid, water liquid is chilled to room temperature with salt and chloroform water-bath reflux, extract,, put in the separatory funnel, divide and get chloroform layer, water liquid with chloroform extraction once, combined chloroform liquid, evaporate to dryness, residue add methanol makes dissolving, as need testing solution.It is an amount of that other gets the emodin reference substance, adds dissolve with methanol and make reference substance solution.According to thin layer chromatography test, draw above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 4: 1 toluene of volume ratio, alcohol mixeding liquid is developing solvent, launches, and takes out, dry, put under the 365nm ultra-violet lamp and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
B. get and differentiate the acid liquid behind the chloroform extraction under a item, with the ethyl acetate extraction secondary, merge ethyl acetate liquid, evaporate to dryness, residue add methanol makes dissolving, as need testing solution.The extracting liquorice control medicinal material shines medical material solution in pairs with legal system in addition.Test according to thin layer chromatography, draw above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 8: 1: 0.5 chloroform of volume ratio, ethyl acetate, glacial acetic acid mixed liquor is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical yellow spotting;
C. get the capsule liquid of soft capsule of the present invention, add the methanol supersound process, filter, the filtrate evaporate to dryness, residue adds water makes dissolving, puts in the separatory funnel, with the ether extraction secondary, discard ether solution, water liquid extracts three times with water-saturated n-butanol, merges n-butyl alcohol liquid, evaporate to dryness, residue adds methanol makes dissolving, as need testing solution.It is an amount of that other gets the icariin reference substance, adds dissolve with methanol and make reference substance solution.Test according to thin layer chromatography, draw above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with volume ratio is 10: 3: 1: the mixed liquor of 1 ethyl acetate, butanone, formic acid and water is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
10. the method for quality control of Anshen Bunao soft capasule as claimed in claim 9, one or more that it is characterized in that adopting following method carry out assay:
A, 2,3,5,4 '-assay of tetrahydroxystilbene-2-O-β-D-glucoside
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; With volume ratio 10～20: 90～80 acetonitrile, water mixed liquid are mobile phase; Flow velocity 1.0ml/min, 25 ℃ of column temperatures, the detection wavelength is 320nm; Number of theoretical plate by 2,3,5,4 '-tetrahydroxystilbene-2-O-β-D-glucoside peak calculates, and should be not less than 2000.
The preparation precision of reference substance solution takes by weighing 2,3,5,4 '-tetrahydroxystilbene-2-O-β-D-glucoside reference substance is an amount of, and add the mobile phase dissolving and make the reference substance solution of determining concentration, promptly.
This product content is got in the preparation of need testing solution, grinds well, and accurate the title decides, and puts in the apparatus,Soxhlet's, it is an amount of to add petroleum ether, and reflux 1 hour discards petroleum ether liquid, and medicinal residues are flung to petroleum ether, shred, put in the tool plug conical flask, precision adds Diluted Alcohol, close plug, claim decide weight, supersound process is put coldly, and weight decided in title again, supply the weight that subtracts mistake with Diluted Alcohol, shake up, filter, precision is measured subsequent filtrate and is added the mobile phase dilution, filters with microporous filter membrane, promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
B, content Determination of Icariin are measured
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; With volume ratio 20～30: 80～70 acetonitrile, water mixed liquid are mobile phase; Flow velocity 1.0ml/min, 25 ℃ of column temperatures, the detection wavelength is 270nm; Number of theoretical plate is pressed the icariin peak and is calculated, and should be not less than 2000.
It is an amount of that the preparation precision of reference substance solution takes by weighing the icariin reference substance, adds dissolve with methanol and make definite concentration reference substance solution, promptly.
This product content under the content uniformity item is got in the preparation of need testing solution, porphyrize, and accurate the title, decide, the accurate methanol supersound process that adds, put coldly, supply the weight that subtracts mistake with methanol, filter, precision is measured subsequent filtrate and is added the mobile phase dilution, shake up, filter with microporous filter membrane, promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
The assay of c, vitamin B1
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; With volume ratio 30～40: 70～60 acetonitrile, water mixed liquid are mobile phase; Flow velocity 1.0ml/min, 40 ℃ of column temperatures, the detection wavelength is 246nm; Number of theoretical plate is pressed the vitamin B1 peak and is calculated, and should be not less than 2000.
It is an amount of that the preparation precision of reference substance solution takes by weighing the vitamin B1 reference substance, adds the mobile phase dissolving and make the reference substance solution of determining concentration, promptly.
This product content under the content uniformity item is got in the preparation of need testing solution, grinds well, and accurate the title decides, and puts in the apparatus,Soxhlet's, it is an amount of to add petroleum ether, and reflux 1 hour discards petroleum ether liquid, and medicinal residues are flung to petroleum ether, shred, put in the 100ml measuring bottle, add the watertight plug, supersound process is put coldly, adds water to scale, shake up, filter, precision is measured subsequent filtrate and is added the mobile phase dilution, shake up, filter with microporous filter membrane, promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100450471C (en) * | 2006-08-25 | 2009-01-14 | 石药集团欧意药业有限公司 | Soft capsule of atovastatine salts and prepn. method therefor |
| CN102284062A (en) * | 2010-09-21 | 2011-12-21 | 深圳信立泰药业股份有限公司 | Capsule shell composition for soft capsule containing ciclosporin, preparation method thereof and soft capsule containing ciclosporin prepared thereby |
| CN104274674A (en) * | 2013-07-01 | 2015-01-14 | 修正药业集团长春高新制药有限公司 | Traditional Chinese medicine composition for treating blood-deficiency Yang-floating type insomnia and preparation method thereof |
| CN108896681A (en) * | 2018-06-20 | 2018-11-27 | 山东省分析测试中心 | A kind of Anshen Bunao mixture multi objective quantitative finger print atlas method for building up and its application |
| CN109846041A (en) * | 2019-01-29 | 2019-06-07 | 深圳市荣格保健品有限公司 | A kind of mind-tranquilizing brain-strengthening capsule |
| CN109953338A (en) * | 2019-01-29 | 2019-07-02 | 深圳市荣格保健品有限公司 | A kind of preparation method of mind-tranquilizing brain-strengthening capsule |
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2005
- 2005-01-05 CN CN 200510200006 patent/CN1799622B/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100450471C (en) * | 2006-08-25 | 2009-01-14 | 石药集团欧意药业有限公司 | Soft capsule of atovastatine salts and prepn. method therefor |
| CN102284062A (en) * | 2010-09-21 | 2011-12-21 | 深圳信立泰药业股份有限公司 | Capsule shell composition for soft capsule containing ciclosporin, preparation method thereof and soft capsule containing ciclosporin prepared thereby |
| CN102284062B (en) * | 2010-09-21 | 2012-11-28 | 深圳信立泰药业股份有限公司 | Capsule shell composition for soft capsule containing ciclosporin, preparation method thereof and soft capsule containing ciclosporin prepared thereby |
| CN104274674A (en) * | 2013-07-01 | 2015-01-14 | 修正药业集团长春高新制药有限公司 | Traditional Chinese medicine composition for treating blood-deficiency Yang-floating type insomnia and preparation method thereof |
| CN108896681A (en) * | 2018-06-20 | 2018-11-27 | 山东省分析测试中心 | A kind of Anshen Bunao mixture multi objective quantitative finger print atlas method for building up and its application |
| CN109846041A (en) * | 2019-01-29 | 2019-06-07 | 深圳市荣格保健品有限公司 | A kind of mind-tranquilizing brain-strengthening capsule |
| CN109953338A (en) * | 2019-01-29 | 2019-07-02 | 深圳市荣格保健品有限公司 | A kind of preparation method of mind-tranquilizing brain-strengthening capsule |
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| Publication number | Publication date |
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| CN1799622B (en) | 2010-05-26 |
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