CN1251733C - Preparation of enhanced agastache capsules and quality control thereof - Google Patents
Preparation of enhanced agastache capsules and quality control thereof Download PDFInfo
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- CN1251733C CN1251733C CN 200310122427 CN200310122427A CN1251733C CN 1251733 C CN1251733 C CN 1251733C CN 200310122427 CN200310122427 CN 200310122427 CN 200310122427 A CN200310122427 A CN 200310122427A CN 1251733 C CN1251733 C CN 1251733C
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- 238000003908 quality control method Methods 0.000 title abstract description 9
- 241001529821 Agastache Species 0.000 title 1
- 239000002775 capsule Substances 0.000 title 1
- 239000007901 soft capsule Substances 0.000 claims abstract description 79
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- 239000000843 powder Substances 0.000 claims abstract description 38
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- 235000006886 Zingiber officinale Nutrition 0.000 claims abstract description 25
- 235000008397 ginger Nutrition 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 25
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Landscapes
- Medicines Containing Plant Substances (AREA)
- Medicinal Preparation (AREA)
Abstract
The present invention discloses a preparation method for a modified soft capsule of herba agastachis and a quality control method for the soft capsule. The preparation method comprises: taking cablin patchouli herb, perilla leaf, dahurian angelica, largehead atractylodes rhizome (fried), dried old orange peel, pinellia tuber (prepared), officinal magnolia bark (prepared with ginger), tuckahoe, platycodon root, liquoric root and areca peel as raw medicinal materials; extracting the officinal magnolia bark with ethanol; extracting volatile oil by distilling the cablin patchouli herb, the perilla leaf, the dried old orange peel, the largehead atractylodes rhizome and the dahurian angelica with steam; decocting dregs of decoction, the pinellia tuber, the tuckahoe, the platycodon root, the liquoric root, the areca peel ginger and Chinese date with water to be dried under reduced pressure, pulverized into fine powder and then sieved; adding the volatile oil, refined vegetable oil and beeswax which are of a proper quantity to the fine powder to be evenly milled with a colloidal mill and made into a soft capsule by pressing. The quality control method for the soft capsule prepared with the method of the present invention comprises an identification method and a content determination method.
Description
Technical field
The present invention relates to a kind of preparation method and quality control method of soft capsule, particularly relate to a kind of preparation method and quality control method of 'Jia Wei Huo Xiang ' soft capsule.
Background technology
What use in the market is modified inspirex extract, be mainly used in clinically catching cold, internal injury humidity hysteresis, headache dusk the diseases such as weight, abdominal distention, vomiting diarrhea, but said preparation is that conventional dosage forms and quality controllable property are poor. The invention discloses a kind of 'Jia Wei Huo Xiang ' soft capsule, and to the preparation technology of soft capsule, the quality control method is studied, and makes this formulation have better controllability and stability.
Summary of the invention
The object of the invention is to provide a kind of preparation method and quality control method of 'Jia Wei Huo Xiang ' soft capsule.
The present invention seeks to be achieved through the following technical solutions.
Prescription:
Pogostemon cablin 300-350 weight portion perilla leaf 90-110 weight portion
The root of Dahurain angelica 90-110 weight portion bighead atractylodes rhizome (stir-fry) 180-220 weight portion
The dried orange peel 180-220 weight portion tuber of pinellia (system) 180-220 weight portion
The bark of official magnolia (ginger system) 180-220 weight portion Poria cocos 90-110 weight portion
Balloonflower root 180-220 weight portion Radix Glycyrrhizae 180-220 weight portion
Shell of areca nut 90-110 weight portion.
Method for making: above ten simply, bark of official magnolia 50-80% alcohol extract 2-3 time, and each 1-2 hour, filter, merging filtrate, Recycled ethanol, being concentrated into relative density is the clear cream A of 1.15 (80 ℃); Pogostemon cablin, perilla leaf, dried orange peel, the bighead atractylodes rhizome, root of Dahurain angelica steam distillation are extracted volatile oil, and the aqueous solution after the distillation filters, and device is collected in addition; The dregs of a decoction and the tuber of pinellia, Poria cocos, balloonflower root, Radix Glycyrrhizae, the shell of areca nut, ginger 30-35 weight portion and the boiling of date 50-55 weight portion 2-3 time, each 1-2 hour, collecting decoction, filter, filtrate and the above-mentioned aqueous solution merge, be concentrated into 80 ℃ of lower relative densities and be 1.12 clear cream, centrifugal, supernatant concentration to relative density is the clear cream B of 1.15 (80 ℃); Merge clear cream A and B, be concentrated into relative density and be the thick paste of (80 ℃) 1.30-1.35, drying under reduced pressure is ground into fine powder, sieves; Other takes food the weight portion with vegetable oil 340-380, and it is an amount of to add beeswax etc., and temperature is treated in fusing, adds above-mentioned powder and volatile oil, and is even through the colloid mill mill, is pressed into soft capsule; Every heavy 0.6g of soft capsule content is equivalent to crude drug 2.157g.
The method for making of soft capsule of the present invention can also for: above ten simply, and the bark of official magnolia is with 50-80% alcohol extract 2-3 time, each 1-2 hour, filtration, merging filtrate, Recycled ethanol, being concentrated into relative density is the clear cream A of 1.15 (80 ℃); Pogostemon cablin, perilla leaf, dried orange peel, the bighead atractylodes rhizome, root of Dahurain angelica steam distillation are extracted volatile oil, and the aqueous solution after the distillation filters, and device is collected in addition; The dregs of a decoction and the tuber of pinellia, Poria cocos, balloonflower root, Radix Glycyrrhizae, the shell of areca nut, ginger 30-35 weight portion and the boiling of date 50-55 weight portion 2-3 time, each 1-2 hour, collecting decoction, merge with the above-mentioned aqueous solution, filter, filtrate is concentrated into the clear cream that relative density is 1.12 (80 ℃), and is centrifugal, and supernatant concentration to relative density is the clear cream B of 1.15 (80 ℃); With clear cream A drying under reduced pressure, be ground into fine powder, sieve. With clear cream B, being concentrated into relative density is the thick paste of 1.30-1.35 (80 ℃), and drying under reduced pressure is ground into fine powder, sieves. The above-mentioned extract powder of mixing, adding volatile oil and refined plant are oily, beeswax is an amount of, and be even through the colloid mill mill, is pressed into soft capsule.
Soft capsule preparation moulding process: the preparation of soft capsule rubber solution
Get certain 1～2: 0.01～0.05: 1～2 glycerine, Brown Ferric Oxide and water, be heated to 70-80 ℃, mix, add 1～2 part of gelatin and stir, melting, insulation was left standstill 1-2 hour, made the foam come-up, scrape off the foam of come-up, filter heat preservation for standby use with clean calico;
Start encapsulating machine, the rubber of arranging exhibits carries out the heavy debugging of ball with paraffin as content, debug qualified after, drain paraffin oil, liquid is added in the liquid reservoir of machine top, start the medicine inlet valve, the soft capsule that contains medicine is namely compressing, compressing soft capsule micelle sent in the hothouse that dehydrating unit is housed under 25-30 ℃ of temperature, carry out drying, allow moisture slowly evaporates in the rubber, and frequently stir gently micelle, to prevent adhesion, be 4-6 hour drying time; Wash soft capsule with ethanol, the soft capsule after the washing is sent into hothouse again, and drying is about 12-18 hour under 30-35 ℃ of temperature, namely gets the soft capsule finished product.
Soft capsule quality control method of the present invention:
Differentiate: get soft capsule content 2g of the present invention, put in the 500ml round-bottomed flask, add water 200-300ml, mixing, connect volatile oil determination apparatus, add water to scale from the analyzer upper end, and till overflow enters in the flask, add again benzinum 1-3ml, connect reflux condensing tube, be heated to and boil, and kept little 1-3 of boiling hour, let cool, divide and get petroleum ether layer as need testing solution; Other gets the patchouli oil reference substance and adds benzinum and make the solution that every 1ml contains 0.1ml, in contrast product solution; Test according to thin-layered chromatography, draw above-mentioned two kinds of each 5ul of solution, put respectively on same silica gel g thin-layer plate take 0.5% sodium carboxymethylcellulose as adhesive, take 8-12: 0.8-1.2 benzinum-ethyl acetate is as solvent, launch, take out, dry, spray is with 2% vanillic aldehyde sulfuric acid test solution, and it is clear that hot blast blows to the spot colour developing; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color;
Get soft capsule content 2g of the present invention, the jolting that adds diethyl ether is extracted 2-3 time, each 20ml, discard ether solution, residue is waved most ether, adds water 40ml and makes dissolving, adds water saturated n-butanol extraction 2-3 time, each 30ml, merge n-butanol liquid, filter evaporate to dryness, residue adds methyl alcohol 5ml makes dissolving, as need testing solution; Other gets the hesperidine reference substance, adds methyl alcohol and makes every 1ml and contain 0.5mg solution, in contrast product solution; According to thin-layered chromatography test, draw above-mentioned two kinds of each 2ul of solution, put respectively on same polyamide film, take 0.8-1.2: the 0.8-1.2 acetone-water launches as solvent, takes out, and dries, and spray is put under the ultraviolet lamp and inspected with l% alchlor test solution; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious same color fluorescence spot;
Get soft capsule content 2g of the present invention, add benzinum 20-40ml, ultrasonic processing 20-40 minute discards benzinum, volatilizes, residue adds chloroform 20-30ml and hydrochloric acid 1-3ml, put and add hot reflux 1-1.5 hour in the water-bath, filtration, filtrate evaporate to dryness, residue adds methyl alcohol 1-3ml makes dissolving, as need testing solution; Extracting liquorice hypo acid reference substance in addition, add methyl alcohol and make the solution that every 1ml contains 0.5mg, product solution according to the thin-layered chromatography test, is drawn above-mentioned two kinds of each 5ul of solution in contrast, put respectively on same silica GF254 lamellae take 0.5% sodium carboxymethylcellulose as adhesive, take 28-32: 12-16: 0.8-1.2 toluene-ethyl acetate-formic acid launches as solvent, takes out, dry, put under the uviol lamp and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
Assay: according to high effective liquid chromatography for measuring
Chromatographic condition and system suitability test are take octadecylsilane chemically bonded silica as filler; 72-76: the 23-26 methanol-water is mobile phase; Flow velocity 1ml/min; Detecting wavelength 294nm column temperature is room temperature; Theoretical cam curve is calculated by the magnolol peak should be not less than 3800;
It is an amount of that the preparation of reference substance solution, precision take by weighing the Magnolol and Honokiol reference substance, and add methyl alcohol and make into the mixed solution that every 1ml contains magnolol 25-35ug, honokiol 20-30ug, mixing, and get final product;
The preparation of need testing solution, precision take by weighing the about 2g of soft capsule of the present invention, and precision adds 50-70% ethanol 15-25ml, weigh, ultrasonic processing 30-50 minute is weighed again, supply solvent and subtract the weight of mistake, shake well filters, discard just filtrate, precision is measured subsequent filtrate 5ml, to the 50ml measuring bottle, is diluted to scale with 50-60% ethanol, shake up, and get final product;
Determination method, precision is drawn reference substance solution and is supplied each 20ul of the brilliant solution of examination respectively, the injection liquid chromatography, mensuration, and get final product; Soft capsule of the present invention contains the bark of official magnolia in the total amount of magnolol (C18H1802) with honokiol (C18H1802), must not be less than 0.9mg.
The JIAWEI HUOXIANG ZHENGQI RUANJIAONANG test of pesticide effectiveness proves, after JIAWEI HUOXIANG ZHENGQI RUANJIAONANG is oral, can increase the small intestine propulsion functions of normal mouse; To atropine induced mice intestinal motility inhibition, after JIAWEI HUOXIANG ZHENGQI RUANJIAONANG is oral obvious excitation is arranged; To the excited model of neostigmine induced mice intestinal motility, JIAWEI HUOXIANG ZHENGQI RUANJIAONANG has obvious inhibitory action. Motion has dual regulation to mouse small intestine to show JIAWEI HUOXIANG ZHENGQI RUANJIAONANG. JIAWEI HUOXIANG ZHENGQI RUANJIAONANG has obvious analgesic activity, and Dichlorodiphenyl Acetate induced mice writhing response has obvious inhibitory action. JIAWEI HUOXIANG ZHENGQI RUANJIAONANG has obvious antidiarrheal effect, can obviously prolong the incubation period of folium sennae induced mice diarrhoea, reduces mouse diarrhoea number of times within a certain period of time. To pigeon nausea model due to the CUS04, this medicine can prolong vomiting incubation period, reduces the vomiting number of times.
Experimental example 1 Pogostemon cablin, perilla leaf, dried orange peel, the bighead atractylodes rhizome, root of Dahurain angelica Study on extraction
The volatile oil extraction and application rate of Pogostemon cablin, perilla leaf, dried orange peel, the bighead atractylodes rhizome, the root of Dahurain angelica as investigating index, is selected L9 (34) the quadrature scheme, investigate soak time, powder particle diameter, amount of water, extraction time four factors, in conjunction with producing reality, each factor is chosen 3 levels, sees Table 1.
Table 1 experimental factor water-glass
Experiment and data:
Take by weighing Pogostemon cablin 150g, perilla leaf 50g, dried orange peel 100g, bighead atractylodes rhizome 100g, root of Dahurain angelica 50g five kinds of Chinese medicine extraction volatile oil, take the extraction and application rate as index, see Table 2.
(L9 (3 for table 2 orthogonal table4))
Attached: through check, Herba Pogostemonis Volatile oil content 2.11%, Folium Perillae volatile oil content 0.73%, Pericarpium Citri Reticulatae volatile oil content are 1.94%, and Baizhu volatile oil content is 0.52%, and Essential Oil of Radix Angelicae Dahuricae content is 0.4%.
By the R value as can be known, factor A is very little on experimental result impact, thus with the sum of sguares of deviation from mean of factor A as estimation error. In order to other factors are carried out significance test, see Table 3.
Table 3 analysis of variance table
| Soruces of variation | Sum of sguares of deviation from mean (S) | The free degree (f) | All square (z) | The F value | P | Conspicuousness |
| B C D error e | 182.92 20.88 586.69 7.66 | 2 2 2 2 | 91.46 10.44 293.34 3.83 | 23.88 2.73 76.59 | ＜0.05 ＜0.05 | Significantly |
Conclusion: as shown in Table 3, factor B, D on the experimental result impact significantly can be known by inference by table 2, B1D2 is optimised process, so it is meal about 0.5cm that the extraction process of five tastes medicinal material volatile oil is selected pulverizing medicinal materials is become particle diameter, it is an amount of to add water, steam distillation 8 hours.
Experimental example 2 bark of official magnolia (ginger system) Study on extraction
With the content of magnolol, honokiol in the high effective liquid chromatography for measuring bark of official magnolia (ginger system), select L9 (34) be the quadrature scheme, investigate concentration of alcohol, soak time, extraction time, ethanol consumption, extraction time each factor, actual in conjunction with producing, each factor is chosen 3 levels, and extraction time, ethanol consumption, extraction time merged into a factor, testing program sees Table 4.
Table 4 experimental factor water-glass
Experiment and data: take by weighing the bark of official magnolia (ginger system) 200g by the requirement of experimental design scheme and extract, the content with magnolol honokiol in the high effective liquid chromatography for measuring bark of official magnolia (ginger system) take the extraction and application rate as investigating index, sees Table 5.
Table 5 orthogonal test design table
Attached: through check, the Magnolol and Honokiol total amount is 2.1% in the bark of official magnolia (ginger system).
D classifies blank column as, carries out significance test so be listed as test error with D, sees Table 6.
Table 6 analysis of variance table
| Soruces of variation | Sum of sguares of deviation from mean S | Free degree f | Equal square z | The F value | P | Conspicuousness |
| A B C error e | 894.89 304.27 348.45 17.31 | 2 2 2 2 | 447.44 152.14 174.22 8.66 | 51.67 17.57 20.12 | ＜0.05 ＜0.05 | Significantly |
Conclusion: as can be seen from Table 6, significantly sex to experimental result is A, next is factor C, and factor B is not remarkable on the experiment impact, shows according to table 5, the optimised process that the bark of official magnolia (ginger system) is extracted is A3C3, namely use 60% alcohol extract three times, for the first time 6 times of amount 60% ethanol, for the second time 4 times of amount 60% ethanol, for the third time with 4 times of amount 60% ethanol, each 1 hour.
The Study on extraction of experimental example 3 all the other flavour of a drug
To the tuber of pinellia, Poria cocos, balloonflower root, Radix Glycyrrhizae, the shell of areca nut, date, ginger and the Pogostemon cablin after extracting volatile oil, perilla leaf, dried orange peel, the root of Dahurain angelica, the bighead atractylodes rhizome totally ten two flavor medicines, select L9 (34) the quadrature scheme, investigate decocting number of times, amount of water, decocting time, medicinal extract density, centrifugation rate, each factor of centrifugation time is actual in conjunction with producing, three levels of each factor design, and decocting number of times, amount of water and decocting time merged into a factor, testing program sees Table 7.
Table 7 experimental factor water-glass
Test and data: the Pogostemon cablin after taking by weighing the tuber of pinellia, Poria cocos, balloonflower root, Radix Glycyrrhizae, the shell of areca nut, date, the ginger in the prescription ratio and extract volatile oil by the experimental program requirement, perilla leaf, dried orange peel, the root of Dahurain angelica, the bighead atractylodes rhizome 12 flavor medicines altogether 890g decoct, content and the dried cream rate of choosing enoxolone are to investigate index, comprehensively mark. The content tlc scanning determination of enoxolone. See Table 8. The content of testing used Radix Glycyrrhizae hypo acid is 3.1%, and regulation enoxolone Y full marks are 70 minutes, and because of the total 890g of the medicinal material that decocts, wherein Radix Glycyrrhizae has 100g, so wherein contained enoxolone should be 100 * 3.1%/890=0.35%. So take the yield 0.35% of enoxolone as full marks 70 minutes, per 1% is 200 minutes, score Y * 200, dried cream rate full marks are 30 minutes, it is predicted the mobility scale of testing out dried cream rate, stipulate that dried cream rate 20% is 0,10% is 30 minutes, every increase by 1% deducts 30/ (20-10)=3 minute, and overall score is counted Y * 200+[30-3 (X-10)].
Table 8 orthogonal table
By the R value as can be known, the R value of factor D is minimum, shows its very little or not impact on experimental result impact, thus with the D example as test error, carry out significance test, see Table 9.
Table 9 analysis of variance table
| Soruces of variation | Sum of sguares of deviation from mean s | Free degree f | Equal square z | The F value | p | Conspicuousness |
| A B C error e | 64.41 36.54 111.06 0.49 | 2 2 2 2 | 32.20 18.27 55.53 0.24 | 134.17 76.12 231.38 | ＜0.01 ＜0.05 ＜0.01 | Extremely significantly extremely remarkable |
Conclusion: as shown in Table 9, the principal element that affects paste-forming rate and enoxolone yield is A, C, secondly be B, according to table 8, optimised process is A2 B1 C1, it is the decocting secondary, 8 times of water gagings were fried in shallow oil 2 hours for the first time, added 6 times of water gagings for the second time and fried in shallow oil 1 hour, and being concentrated into decocting liquid clearly, cream density is 1.12 (80 ℃), carry out centrifugally, centrifugation rate is 7000 rev/mins.
Experimental example 4 concentrates, the research of drying process
Get bark of official magnolia 536g, press optimised process and extract, collect extract, therefrom get 3000ml, be divided into two parts, behind the Recycled ethanol, under condition of different temperatures, be condensed into clearly cream, measure again the content of Magnolol and Honokiol. We by temperature as seen from Table 15 the content of Magnolol and Honokiol are had certain impact, so when pilot scale, can be evaporated to extract relative density 1.15 (80 ℃ of surveys). See Table 10,
The concentrated condition of table 10 is investigated
| Method | Extract | Concentrate | The content of Magnolol and Honokiol |
| Normal pressure reclaims (95～90 ℃) recovered under reduced pressure (75～80 ℃) | 1500ml 1500ml | 85ml 85ml | 3.07mg/ml 4.19mg/ml |
The method of extract dry and temperature: owing to contain volatile material in this product, so we adopt the drying means of drying under reduced pressure, and drying under reduced pressure can shorten drying time, therefore consider produce actual, our drying under reduced pressure in technique.
Experimental example 5 stability tests
Method: issued " provisions for new drugs approval " of execution on May 1st, 1999 according to the Ministry of Public Health about annex " specification requirement of new Chinese medicine steady quality Journal of Sex Research " in the amendment and supplement regulation of Chinese medicine part, prepare JIAWEI HUOXIANG ZHENGQI RUANJIAONANG by technique, the aluminium-plastic panel packing is observed (seeing the following form) by declaring clinical testing with drug quality draft standard (data numbering 11) requirement under the 10/plate normal temperature.
Sample title: JIAWEI HUOXIANG ZHENGQI RUANJIAONANG (0.6 gram/grain) lot number: 990227
Date of manufacture: on February 27th, 1999
| Standing time (experiment date) is project as a result | 0 month (99.3.2) | March (99.6.2) | June (99.9.2) | December (00.3.2) | 18 months (00.9.2) | |
| Proterties | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter. | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter. | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter. | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter. | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter. | |
| Differentiate | 1. 2. 3. Radix Glycyrrhizae of dried orange peel of Pogostemon cablin | Positive positive | Positive positive | Positive positive | Positive positive | Positive positive |
| Check | Disintegration time limited (minute) | 12 | 15 | 17 | 17 | 19 |
| Assay | Magnolol, honokiol (mg/ grain) | 1.30 | 1.30 | 1.30 | 1.29 | 1.33 |
| Microbial limit | Bacterium (individual/g) mould is (individual/g) the Escherichia coli mite that lives | ＜10＜10 do not detect | 10 20 do not detect | ＜10＜10 do not detect | ＜10＜10 do not detect | 10 20 do not detect |
Sample title: JIAWEI HUOXIANG ZHENGQI RUANJIAONANG (0.6 gram/grain) lot number: 990306
Date of manufacture: on March 6th, 1999
| Standing time (experiment date) is project as a result | 0 month (99.3.8) | March (99.6.8) | June (99.9.8) | December (00.3.8) | 18 months (00.9.8) | |
| Proterties | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter. | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter. | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter. | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter. | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter. | |
| Differentiate | 1. 2. 3. Radix Glycyrrhizae of dried orange peel of Pogostemon cablin | Positive positive | Positive positive | Positive positive | Positive positive | Positive positive |
| Check | Disintegration time limited (minute) | 13 | 15 | 18 | 18 | 20 |
| Assay | Magnolol, honokiol (mg/ grain) | 1.27 | 1.27 | 1.27 | 1.20 | 1.24 |
| Microbial limit | Bacterium (individual/g) mould is (individual/g) the Escherichia coli mite that lives | 20＜10 do not detect | ＜10 10 do not detect | 10＜10 do not detect | 20 20 do not detect | 20 20 do not detect |
Sample title: JIAWEI HUOXIANG ZHENGQI RUANJIAONANG (0.6 gram/grain) lot number: 990313
Date of manufacture: on March 13rd, 1999
| Standing time (experiment date) is project as a result | 0 month (99.3.15) | March (99.6.15) | June (99.9.15) | December (00.3.15) | 18 months (00.9.15) | |
| Proterties | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter. | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter. | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter. | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter. | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter. | |
| Differentiate | 1. 2. 3. Radix Glycyrrhizae of dried orange peel of Pogostemon cablin | Positive positive | Positive positive | Positive positive | Positive positive | Positive positive |
| Check | Disintegration time limited (minute) | 15 | 18 | 19 | 18 | 22 |
| Assay | Magnolol, honokiol (mg/ grain) | 1.38 | 1.38 | 1.38 | 1.38 | 1.40 |
| Microbial limit | Bacterium (individual/g) mould is (individual/g) the Escherichia coli mite that lives | 20＜10 do not detect | 20 10 do not detect | 10＜10 do not detect | 20 20 do not detect | 20 20 do not detect |
The result: observed through 18 months, indices (proterties, discriminating, inspection, assay) all meets the quality standard requirement, and health examination meets the health examination standard.
Conclusion: JIAWEI HUOXIANG ZHENGQI RUANJIAONANG was placed 18 months with the aluminium-plastic panel room temperature respectively, steady quality.
Embodiment 1: the preparation method one of soft capsule of the present invention
Pogostemon cablin 326.8g perilla leaf 108.9g root of Dahurain angelica 108.9g
Whitewood's (stir-fry) 217.9g dried orange peel 217.9g tuber of pinellia (system) 217.9g
The bark of official magnolia (ginger system) 217.9g Poria cocos 108.9g balloonflower root 217.9g
Radix Glycyrrhizae 217.9g shell of areca nut 108.9g
More than ten simply, the bark of official magnolia is with 60% alcohol extract three times, each 1 hour, filter, merging filtrate, Recycled ethanol is concentrated into relative density and is 1.15 clear cream A; Pogostemon cablin, perilla leaf, dried orange peel, the bighead atractylodes rhizome, root of Dahurain angelica steam distillation are extracted volatile oil, and the aqueous solution after the distillation filters other device and collects; The dregs of a decoction and the tuber of pinellia, Poria cocos, balloonflower root, Radix Glycyrrhizae, the shell of areca nut, ginger 32.7g and date 54.5g boiling secondary, 2 hours for the first time, 1 hour for the second time, collecting decoction, filter, filtrate and the merging of the above-mentioned aqueous solution are concentrated into relative density and are 1.12 clear cream, centrifugal, supernatant concentration to relative density is 1.15 clear cream B; Merge clear cream A and B, be concentrated into relative density and be 1.30 thick paste, drying under reduced pressure is ground into fine powder, sieves. Other takes food and uses vegetable oil 360g, and it is an amount of to add beeswax etc., and temperature is treated in fusing, adds above-mentioned powder and volatile oil, and is even through the colloid mill mill, is pressed into 1000 of soft capsules, and get final product.
Embodiment 2: the preparation method two of soft capsule of the present invention
Pogostemon cablin 326.8g perilla leaf 108.9g root of Dahurain angelica 108.9g
The bighead atractylodes rhizome (stir-fry) the 217.9g dried orange peel 217.9g tuber of pinellia (system) 217.9g
The bark of official magnolia (ginger system) 217.9g Poria cocos 108.9g balloonflower root 217.9g
Radix Glycyrrhizae 217.9g shell of areca nut 108.9g
More than ten simply, the bark of official magnolia is with 60% alcohol extract three times, each 1 hour, filter, merging filtrate, Recycled ethanol, being concentrated into relative density is the clear cream A of 1.15 (80 ℃); Pogostemon cablin, perilla leaf, dried orange peel, the bighead atractylodes rhizome, root of Dahurain angelica steam distillation are extracted volatile oil, and the aqueous solution after the distillation filters, and device is collected in addition; The dregs of a decoction and the tuber of pinellia, Poria cocos, balloonflower root, Radix Glycyrrhizae, the shell of areca nut, ginger 32.7g and date 54.5g boiling secondary, 2 hours for the first time, 1 hour for the second time, collecting decoction, merge with the above-mentioned aqueous solution, filter, filtrate is concentrated into the clear cream that relative density is 1.12 (80 ℃), centrifugal, supernatant concentration to relative density is the clear cream B of 1.15 (80 ℃); With clear cream A drying under reduced pressure, be ground into fine powder, sieve. With clear cream B, being concentrated into relative density is the thick paste of 1.30-1.35 (80 ℃), and drying under reduced pressure is ground into fine powder, sieves. The above-mentioned extract powder of mixing, adding volatile oil and refined plant are oily, beeswax is an amount of, and be even through the colloid mill mill, is pressed into 1000 of soft capsules, and get final product.
Embodiment 3: the preparation of soft capsule rubber solution of the present invention
Get 1.5: 0.03: 1.5 glycerine, Brown Ferric Oxide and water, be heated to 75 ℃, mix, add and add in advance the swollen 1.5 parts of gelatin stirring of water logging, melting, insulation was left standstill 1.5 hours, made the foam come-up, scrape off the foam of come-up, filter heat preservation for standby use with clean calico;
Start encapsulating machine, the rubber of arranging exhibits carries out the heavy debugging of ball with paraffin as content, debug qualified after, drain paraffin oil, liquid is added in the liquid reservoir of machine top, start the medicine inlet valve, the soft capsule that contains medicine is namely compressing; Compressing soft capsule micelle sent in the hothouse that dehydrating unit is housed under 27 ℃ of temperature, carried out drying 4 hours, wash soft capsule with ethanol, soft capsule after the washing is sent into hothouse again, and drying is 15 hours under 35 ℃ of temperature, namely gets the soft capsule finished product.
Embodiment 4: the quality control method of soft capsule of the present invention
Differentiate: get soft capsule content 2g of the present invention, put in the 500ml round-bottomed flask, add water 250ml, mixing, connect volatile oil determination apparatus, add water to scale from the analyzer upper end, and till overflow enters in the flask, add again benzinum (60-90 ℃) 1.5ml, connect reflux condensing tube, be heated to and boil, and keep little and boiled 2 hours, let cool, divide and get petroleum ether layer as need testing solution; Other gets the patchouli oil reference substance and adds benzinum and make the solution that every 1ml contains 0.1ml, in contrast product solution; Test according to thin-layered chromatography, draw above-mentioned two kinds of each 5ul of solution, put respectively on same silica G lamellae take 0.5% sodium carboxymethylcellulose as adhesive, take 10: 1 benzinum (60-90 ℃)-ethyl acetates as solvent, launch, take out, dry, spray is with 2% vanillic aldehyde sulfuric acid test solution, and it is clear that hot blast blows to the spot colour developing; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color;
Get soft capsule content 2g of the present invention, secondary is extracted in the jolting that adds diethyl ether, and each 20ml discards ether solution, residue is waved most ether factory and is added water 40ml and make dissolving, add water saturated n-butanol extraction secondary, each 30ml merges n-butanol liquid, filter, evaporate to dryness, residue add methyl alcohol 5ml makes dissolving, as need testing solution; Other gets the hesperidine reference substance, adds methyl alcohol and makes every 1ml and contain 0.5mg solution, in contrast product solution; According to the thin-layered chromatography test, draw above-mentioned two kinds of each 2ul of solution, put respectively on same polyamide film, take 1: 1 acetone-water as solvent, launch, take out, to dry, spray is put under the 365nm ultraviolet lamp and is inspected with 1% alchlor test solution; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious same color fluorescence spot;
Get soft capsule content 2g of the present invention, add benzinum (60 ℃-90 ℃) 30ml, ultrasonic processing 30 minutes discards benzinum, volatilizes, residue adds chloroform 25ml and hydrochloric acid 2ml, put and added hot reflux in the water-bath 1 hour, filtration, filtrate evaporate to dryness, residue adds methyl alcohol 2ml makes dissolving, as need testing solution; Extracting liquorice hypo acid reference substance in addition, add methyl alcohol and make the solution that every 1ml contains 0.5mg, product solution according to the thin-layered chromatography test, is drawn above-mentioned two kinds of each 5ul of solution in contrast, put respectively on same silica GF254 lamellae take 0.5% sodium carboxymethylcellulose as adhesive, take 30: 15: 1 toluene-ethyl acetate-formic acid as solvent, launch, take out, dry, put under the 254nm uviol lamp and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
Assay: according to high effective liquid chromatography for measuring;
Chromatographic condition and system suitability test are take octadecylsilane chemically bonded silica as filler; 75: 25 methanol-waters are mobile phase; Flow velocity 1ml/min; Detect wavelength 294nm; Column temperature is room temperature; Theoretical cam curve is calculated by the magnolol peak should be not less than 3800;
It is an amount of that the preparation of reference substance solution, precision take by weighing the Magnolol and Honokiol reference substance, and add methyl alcohol and make into the mixed solution that every 1ml contains magnolol 30ug, honokiol 25ug, mixing, and get final product;
The system of need testing solution each, precision takes by weighing the about 2g of soft capsule of the present invention, precision adds 60% ethanol 20ml, weigh, ultrasonic processing 45 minutes is weighed again, supply solvent and subtract the weight of mistake, shake well filters, discard just filtrate, precision is measured subsequent filtrate 5ml, to the 50ml measuring bottle, is diluted to scale with 60% ethanol, shake up, and get final product;
Determination method, precision is drawn reference substance solution and is supplied each 20ul of the brilliant solution of examination respectively, the injection liquid chromatography, mensuration, and get final product.
Claims (6)
1, a kind of preparation method of 'Jia Wei Huo Xiang ' soft capsule is characterized in that the method is:
Pogostemon cablin 300-350 weight portion perilla leaf 90-110 weight portion
Root of Dahurain angelica 90-110 weight portion rhizoma atractylodis macrocephalae 180-220 weight portion
Dried orange peel 180-220 weight portion tuber of pinellia 180-220 processed weight portion
Ginger bark of official magnolia 180-220 weight portion processed Poria cocos 90-110 weight portion
Balloonflower root 180-220 weight portion Radix Glycyrrhizae 180-220 weight portion
Shell of areca nut 90-110 weight portion;
More than ten simply, the bark of official magnolia is with 50-80% alcohol extract 2-3 time, each 1-2 hour, filtration, merging filtrate, Recycled ethanol is concentrated into relative density and is 1.15 clear cream A; Pogostemon cablin, perilla leaf, dried orange peel, the bighead atractylodes rhizome, root of Dahurain angelica steam distillation are extracted volatile oil, and the aqueous solution after the distillation filters, and device is collected in addition; The dregs of a decoction and the tuber of pinellia, Poria cocos, balloonflower root, Radix Glycyrrhizae, the shell of areca nut, ginger 30-35 weight portion and date 50-55 weight portion boilings 2-3 time, each 1-2 hour, collecting decoction, filter, filtrate and the above-mentioned aqueous solution merge, be concentrated into 80 ℃ of lower relative densities and be 1.12 clear cream, centrifugal, supernatant concentration to relative density is 1.15 clear cream B; Merge clear cream A and B, be concentrated into the thick paste that relative density is 80 ℃ of lower 1.30-1.35, drying under reduced pressure is ground into fine powder, sieves; Other takes food 380 weight portions with vegetable oil 340-, and it is an amount of to add beeswax, and temperature is treated in fusing, adds above-mentioned powder and volatile oil, and is even through the colloid mill mill, is pressed into soft capsule.
2, the preparation method of soft capsule as claimed in claim 1 is characterized in that the method is:
Pogostemon cablin 326.8 weight portion perilla leafs 108.9 weight portions
The root of Dahurain angelica 108.9 weight portion rhizoma atractylodis macrocephalaes 217.9 weight portions
The dried orange peel 217.9 weight portions tuber of pinellia 217.9 weight portions processed
The ginger bark of official magnolia 217.9 weight portion Poria cocos processed 108.9 weight portions
Balloonflower root 217.9 weight portion Radix Glycyrrhizaes 217.9 weight portions
The shell of areca nut 108.9 weight portions;
More than ten simply, the bark of official magnolia is with 60% alcohol extract three times, each 1 hour, filter, merging filtrate, Recycled ethanol is concentrated into relative density and is 1.15 clear cream A; Pogostemon cablin, perilla leaf, dried orange peel, the bighead atractylodes rhizome, root of Dahurain angelica steam distillation are extracted volatile oil, and the aqueous solution after the distillation filters other device and collects; The dregs of a decoction and the tuber of pinellia, Poria cocos, balloonflower root, Radix Glycyrrhizae, the shell of areca nut, ginger 32.7 weight portions and date 54.5 weight portion boiling secondaries, 2 hours for the first time, 1 hour for the second time, collecting decoction, filter, filtrate and the above-mentioned aqueous solution merge, and being concentrated into relative density is 80 ℃ of down clear cream of 1.12, centrifugal, supernatant concentration to relative density is 1.15 clear cream B; Merge clear cream A and B, being concentrated into relative density is 80 ℃ of down thick pastes of 1.30, and drying under reduced pressure is ground into fine powder, sieves; Other takes food with vegetable oil 360 weight portions, and it is an amount of to add beeswax, and temperature is treated in fusing, adds above-mentioned powder and volatile oil, and is even through the colloid mill mill, is pressed into soft capsule.
3, the preparation method of 'Jia Wei Huo Xiang ' soft capsule as claimed in claim 1 is characterized in that the method is:
Pogostemon cablin 300-350 weight portion perilla leaf 90-110 weight portion
Root of Dahurain angelica 90-110 weight portion rhizoma atractylodis macrocephalae 180-220 weight portion
Dried orange peel 180-220 weight portion tuber of pinellia 180-220 processed weight portion
Ginger bark of official magnolia 180-220 weight portion processed Poria cocos 90-110 weight portion
Balloonflower root 180-220 weight portion Radix Glycyrrhizae 180-220 weight portion
Shell of areca nut 90-110 weight portion;
More than ten simply, the bark of official magnolia is with 50-80% alcohol extract 2-3 time, each 1-2 hour, filter, merging filtrate, Recycled ethanol is concentrated into relative density and is 80 ℃ lower 1.15 clear cream A; Pogostemon cablin, perilla leaf, dried orange peel, the bighead atractylodes rhizome, root of Dahurain angelica steam distillation are extracted volatile oil, and the aqueous solution after the distillation filters, and device is collected in addition; The dregs of a decoction and the tuber of pinellia, Poria cocos, balloonflower root, Radix Glycyrrhizae, the shell of areca nut, ginger 30-35 weight portion and the boiling of date 50-55 weight portion 2-3 time, each 1-2 hour, collecting decoction, merge with the above-mentioned aqueous solution, filter, filtrate is concentrated into relative density and is 80 ℃ of down clear cream of 1.12, and is centrifugal, and supernatant concentration to relative density is 80 ℃ lower 1.15 clear cream B; With clear cream A drying under reduced pressure, be ground into fine powder, sieve; With clear cream B, be concentrated into the thick paste that relative density is 80 ℃ of lower 1.30-1.35, drying under reduced pressure is ground into fine powder, sieves; The above-mentioned extract powder of mixing, adding volatile oil and refined plant are oily, beeswax is an amount of, and be even through the colloid mill mill, is pressed into soft capsule.
4, the preparation method of soft capsule as claimed in claim 3 is characterized in that the method is:
Pogostemon cablin 326.8g perilla leaf 108.9g root of Dahurain angelica 108.9g
Rhizoma atractylodis macrocephalae 217.9g dried orange peel 217.9g tuber of pinellia 217.9g processed
Ginger bark of official magnolia 217.9g Poria cocos processed 108.9g balloonflower root 217.9g
Radix Glycyrrhizae 217.9g shell of areca nut 108.9g;
More than ten simply, the bark of official magnolia is with 60% alcohol extract three times, each 1 hour, filter, merging filtrate, Recycled ethanol is concentrated into relative density and is 80 ℃ lower 1.15 clear cream A; Pogostemon cablin, perilla leaf, dried orange peel, the bighead atractylodes rhizome, root of Dahurain angelica steam distillation are extracted volatile oil, and the aqueous solution after the distillation filters, and device is collected in addition; The dregs of a decoction and the tuber of pinellia, Poria cocos, balloonflower root, Radix Glycyrrhizae, the shell of areca nut, ginger 32.7g and date 54.5g boiling secondary, 2 hours for the first time, 1 hour for the second time, collecting decoction, merge with the above-mentioned aqueous solution, filter, it is 80 ℃ of down clear cream of 1.12 that filtrate is concentrated into relative density, centrifugal, supernatant concentration to relative density is 80 ℃ lower 1.15 clear cream B; With clear cream A drying under reduced pressure, be ground into fine powder, sieve; With clear cream B, be concentrated into the thick paste that relative density is 80 ℃ of lower 1.30-1.35, drying under reduced pressure is ground into fine powder, sieves; The above-mentioned extract powder of mixing, adding volatile oil and refined plant are oily, beeswax is an amount of, and be even through the colloid mill mill, is pressed into 1000 of soft capsules, and get final product.
5, such as the preparation method of claim 1,2,3 or 4 described soft capsules, it is characterized in that the preparation moulding process of soft capsule in the method is:
Get certain 1～2: 0.01～0.05: 1～2 glycerine, Brown Ferric Oxide and water, be heated to 70-80 ℃, mix, add 1～2 part of gelatin and stir, melting, insulation was left standstill 1-2 hour, made the foam come-up, scrape off the foam of come-up, filter heat preservation for standby use with clean calico;
Start encapsulating machine, the rubber of arranging exhibits carries out the heavy debugging of ball with paraffin as content, debug qualified after, drain paraffin oil, liquid is added in the liquid reservoir of machine top, start the medicine inlet valve, the soft capsule that contains medicine is namely compressing, compressing soft capsule micelle sent in the hothouse that dehydrating unit is housed under 25-30 ℃ of temperature, carry out drying, allow moisture slowly evaporates in the rubber, and frequently stir gently micelle, to prevent adhesion, be 4-6 hour drying time; Wash soft capsule with ethanol, the soft capsule after the washing is sent into hothouse again, and drying is about 12-18 hour under 30-35 ℃ of temperature, namely gets the soft capsule finished product.
6, the preparation method of soft capsule as claimed in claim 5 is characterized in that the preparation moulding process of soft capsule in the method is:
Get 1.5: 0.03: 1.5 glycerine, Brown Ferric Oxide and water, be heated to 75 ℃, mix, add and add in advance the swollen 1.5 parts of gelatin stirring of water logging, melting, insulation was left standstill 1.5 hours, made the foam come-up, scrape off the foam of come-up, filter heat preservation for standby use with clean calico;
Start encapsulating machine, the rubber of arranging exhibits carries out the heavy debugging of ball with paraffin as content, debug qualified after, drain paraffin oil, liquid is added in the liquid reservoir of machine top, start the medicine inlet valve, the soft capsule that contains about thing is namely compressing; Compressing soft capsule micelle sent in the hothouse that dehydrating unit is housed under 27 ℃ of temperature, carried out drying 4 hours, wash soft capsule with ethanol, soft capsule after the washing is sent into hothouse again, and drying is 15 hours under 35 ℃ of temperature, namely gets the soft capsule finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310122427 CN1251733C (en) | 2002-12-23 | 2003-12-23 | Preparation of enhanced agastache capsules and quality control thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN02157386 | 2002-12-23 | ||
| CN02157386.7 | 2002-12-23 | ||
| CN 200310122427 CN1251733C (en) | 2002-12-23 | 2003-12-23 | Preparation of enhanced agastache capsules and quality control thereof |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB2006100010437A Division CN100367996C (en) | 2003-12-23 | 2003-12-23 | Quality control method of 'Jia Wei Huo Xiang' soft capsule |
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| CN1509759A CN1509759A (en) | 2004-07-07 |
| CN1251733C true CN1251733C (en) | 2006-04-19 |
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| CN 200310122427 Expired - Lifetime CN1251733C (en) | 2002-12-23 | 2003-12-23 | Preparation of enhanced agastache capsules and quality control thereof |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101474323B (en) * | 2007-12-31 | 2012-05-23 | 天津中新药业集团股份有限公司达仁堂制药厂 | Ageratum soft capsule and preparation method thereof |
| CN102614335A (en) * | 2011-01-28 | 2012-08-01 | 北京亚东生物制药有限公司 | Method for preparing Huoxiang Zhengqi oral liquid |
| CN102614449A (en) * | 2012-04-06 | 2012-08-01 | 王爱玉 | Chinese herbal preparation for curing intestinal adhesion |
| CN104363773B (en) * | 2012-05-19 | 2017-03-01 | 江苏康缘药业股份有限公司 | For treating herbal-composition of gastroenteritis disease and its production and use |
| CN103005087A (en) * | 2012-10-10 | 2013-04-03 | 赵廷宝 | Folium mori bagged tea |
| CN104338062A (en) * | 2014-10-30 | 2015-02-11 | 崔银方 | Chinese medicinal preparation for treating stomachache and diarrhea |
| CN106501442B (en) * | 2016-12-13 | 2018-10-26 | 佛山科学技术学院 | A kind of quality determining method of a kind of reed mentioned in ancient books Huang powder for clearing lung-heat |
| CN107174531A (en) * | 2017-04-28 | 2017-09-19 | 成都永康制药有限公司 | A kind of low temperature drying method of small golden pellets preparation |
| CN110927322B (en) * | 2019-11-07 | 2022-05-17 | 石药集团中奇制药技术（石家庄）有限公司 | Detection method of Huoxiang Zhengqi mixture |
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