CN101011541A - Chinese traditional medicine composition for treating influenza and quality controlling method thereof - Google Patents
Chinese traditional medicine composition for treating influenza and quality controlling method thereof Download PDFInfo
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- CN101011541A CN101011541A CNA2007100634524A CN200710063452A CN101011541A CN 101011541 A CN101011541 A CN 101011541A CN A2007100634524 A CNA2007100634524 A CN A2007100634524A CN 200710063452 A CN200710063452 A CN 200710063452A CN 101011541 A CN101011541 A CN 101011541A
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Abstract
The invention relates to a pharmaceutical preparation for treating common cold, its preparing process and quality control method, wherein the preparation is made mainly from buffalo horn, arctium fruit, prepared soybean, honeysuckle flower, ledebouriella root, capsule of weeping forsythia, bamboo leaves, root of ballon flower, peppermint oil and licorice root.
Description
Technical field
The present invention relates to a kind of Chinese medicine composition and preparation method thereof and method of quality control, particularly relate to a kind of Chinese medicine composition for the treatment of flu and preparation method thereof and method of quality control.
Background technology
Flu is meant to experience to touch emits ailment said due to cold or exposure, a kind of common exterior syndrome of symptoms such as nasal obstruction, watery nasal discharge, sneeze, cough, headache, fever with aversion to cold, general malaise occurs.Influenza is the extremely strong common cold of a kind of infectiousness that is caused by influenza virus.Influenza virus is divided into first, second, the third three types, and wherein, the most normal what cause morbidity is the first type.Influenza A virus is everlasting and is undergone mutation in 10～15 years, new hypotype occurs, causes and is very popular.Because human body is to no cross immunity ability between the various influenza virus, so the annual new subtype influenza pandemic that different range is all arranged.
In stage occurred frequently of this type of respiratory system disease especially autumn and winter season.The medicine for the treatment of this type of disease is innumerable, western medicine is many based on Tri-Biocin, antipyretic-antalgic class medicine and antiviral class medicine, though Western medicine instant effect, but be easy to generate drug resistance, and too much use also can cause other diseases of human body, especially in the child, use aspirin, Reye can take place " s syndrome.
Use this type of disease of treatment by Chinese herbs then can avoid the shortcoming of above-mentioned Western medicine, Chinese medicine thinks that flu is because ailment said due to cold or exposure when taking advantage of human body to drive evil scarce capacity, and the invasion and attack lung is defended due to the fur.The many medicines with dispelling exopathogens from superficies of the body, releasing table disease of Chinese medicine are main treatment, and exopathogen is separated from antiperspirant, are equipped with heat-clearing and toxic substances removing such as eliminating fire and detoxication, removing heat from the lung and relieving sorethroat, and the medicine of reconciling superficies and interior makes the flu disease be alleviated and cure.Therefore the patient uses saferly during the treatment by Chinese herbs flu, is difficult for producing drug resistance, can also strengthen the human body prevention ability of pathogenic factor to external world.
Summary of the invention
The object of the invention is to provide a kind of Chinese medicine composition for the treatment of flu;
The object of the invention also is to provide a kind of Chinese medicine composition preparation method for the treatment of flu;
The object of the invention also is to provide a kind of method of quality control for the treatment of the Chinese medicine composition of flu.
The present invention seeks to be achieved through the following technical solutions:
The Chinese medicine composition of treatment flu of the present invention is to be made by the crude drug of following weight ratio:
Cornu Bubali 3-25 weight portion Fructus Arctii 100-400 weight portion
Semen Sojae Preparatum 100-400 weight portion Flos Lonicerae 200-500 weight portion
Radix Saposhnikoviae 100-500 weight portion Fructus Forsythiae 2 00-500 weight portions
Herba Lophatheri 100-400 weight portion Radix Platycodonis 100-400 weight portion
Oleum menthae 5-40 parts by volume Radix Glycyrrhizae 100-400 weight portion;
Oleum menthae can substitute with Mentholum 0.75-10 weight portion in the above-mentioned raw materials.
The Chinese medicine composition of treatment flu of the present invention can be made by the crude drug of following weight ratio:
Cornu Saigae Tataricae 3-25 weight portion Fructus Arctii 100-400 weight portion
Semen Sojae Preparatum 100-400 weight portion Flos Lonicerae 200-500 weight portion
Herba Schizonepetae 100-500 weight portion Fructus Forsythiae 200-500 weight portion
Herba Lophatheri 100-400 weight portion Radix Platycodonis 100-400 weight portion
Oleum menthae 5-40 parts by volume Radix Glycyrrhizae 100-400 weight portion;
The above-mentioned raw materials optimum ratio is:
Cornu Saigae Tataricae 15-20 weight portion Fructus Arctii 100-200 weight portion
Semen Sojae Preparatum 100-200 weight portion Flos Lonicerae 400-500 weight portion
Herba Schizonepetae 100-200 weight portion Fructus Forsythiae 400-500 weight portion
Herba Lophatheri 100-300 weight portion Radix Platycodonis 300-400 weight portion
Oleum menthae 30-50 parts by volume Radix Glycyrrhizae 300-400 weight portion
Oleum menthae can be replaced with Mentholum 5-10 weight portion in the above-mentioned raw materials.
Weight portion/parts by volume is corresponding with g/ml in the compositions of the present invention.
Compositions of the present invention technology adding adjuvant is routinely made clinical acceptable forms such as tablet, capsule, oral liquid, drop pill, spray, granule; Described adjuvant comprises solvent, disintegrating agent, correctives, antiseptic, coloring agent, binding agent, lubricant, substrate etc.
The preparation method of Chinese medicinal composition capsules preparation of the present invention is:
Choose crude drug:
Cornu Saigae Tataricae 3-25 weight portion Fructus Arctii 100-400 weight portion
Semen Sojae Preparatum 100-400 weight portion Flos Lonicerae 200-500 weight portion
Herba Schizonepetae 100-500 weight portion Fructus Forsythiae 200-500 weight portion
Herba Lophatheri 100-400 weight portion Radix Platycodonis 100-400 weight portion
Oleum menthae 5-40 parts by volume Radix Glycyrrhizae 100-400 weight portion;
The Cornu Saigae Tataricae file is ground into fine powder, and balloonflower powder is broken into fine powder, Herba Schizonepetae, Fructus Forsythiae extracts volatile oil, add water 8-12 and doubly measure, distillation time 4-7 hour, medicinal residues and medicinal liquid added Flos Lonicerae, Herba Lophatheri, Semen Sojae Preparatum, Fructus Arctii, Radix Glycyrrhizae decocts 2-3 time, add 5-9 times of water gaging at every turn, each 1-3 hour, collecting decoction filtered, filtrate is concentrated into relative density and is about 1.3-1.6 (50～55 ℃), add Platycodon Root and right amount of auxiliary materials, mixing is made granule, dry, pulverize, sieve, spray is with Oleum menthae and Herba Schizonepetae, the ethanol dilution liquid of Forsythia volatile oil, add the Cornu Saigae Tataricae fine powder again, mixing incapsulates, promptly.
Pharmaceutical composition method of quality control of the present invention comprises one or more in following discrimination method and/or the assay:
Differentiate:
(1) get pharmaceutical composition solid preparation of the present invention, put microscopically and observe: irregular shape fragment, nearly colourless or light gray, sub-translucent, glossy slightly, accidental sepia pigment granule; Fractionlet is more, shows graininess, and big fragment is evenly distributed with most longitudinal voids that closely are arranged in parallel, space Long Circle, crescent, strip or slit-like; Conduit is scalariform, reticulate pattern and bordered pit vessel, diameter 20～70 μ m;
(2) get the drug combination preparation of the present invention that is equivalent to crude drug 18-25g, add ethanol 25ml reflux 0.8-1.5 hour, filter, filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets the arctiin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to the thin layer chromatography test, draw reference substance solution 1～2ul, sample solution 2～4ul, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water (35-45: 8-12: 1) be developing solvent, launch, take out, dry, spray is with 4-6% vanillin sulfuric acid solution, and hot blast blows to clear spot; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(3) get and be equivalent to crude drug 18-25g drug combination preparation of the present invention, add 15% sulphuric acid 20ml, add chloroform 30ml after the jolting, reflux 1-3 hour, divide and get chloroform layer, evaporate into about 1ml, as need testing solution; Other gets Radix Platycodonis control medicinal material 2g, shines medical material solution in pairs with legal system; According to the thin layer chromatography test, draw control medicinal material solution 1～2ul, sample solution 2～4ul, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction-ethyl acetate (1-4: 0.5-1) be developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and hot blast blows to clear spot; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the aubergine speckle of same color;
Assay:
High performance liquid chromatography, chromatographic condition and system suitability test are filler (4.6 * 150mm, 5 μ m) with octadecylsilane chemically bonded silica; Methanol-water solution (1: 1-2) be mobile phase; The detection wavelength is 280nm; Number of theoretical plate calculates by arctiin should be not less than 1500;
The preparation of reference substance solution: precision takes by weighing the 5mg arctiin, places the 10ml volumetric flask, adds methanol to scale, shakes up, and filters with microporous filter membrane (0.45 μ m), promptly; (containing arctiin 0.5mg among every 1ml)
The preparation of need testing solution: get the about 2g of powder under the drug combination preparation content uniformity item of the present invention, the accurate title, decide, and puts in the tool plug conical flask, precision adds methanol 50ml, claims to decide weight, supersound process (power 250W, frequency 40KHZ) 15-25 minute, cool, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, get supernatant and filter with microporous filter membrane (0.45 μ m),, promptly;
Algoscopy: accurate respectively reference substance liquid and each 10 μ l injection chromatograph of liquid of test sample liquid drawn, measure, promptly; Be equivalent to crude drug 1.5-2.5g drug combination preparation of the present invention and contain Fructus Arctii with arctiin (C
37H
34O
11) must not be less than 2.30mg.
Pharmaceutical composition method of quality control of the present invention is preferably as follows one or more in discrimination method and/or the assay:
Differentiate:
(1) get pharmaceutical composition solid preparation of the present invention, put microscopically and observe: irregular shape fragment, nearly colourless or light gray, sub-translucent, glossy slightly, accidental sepia pigment granule; Fractionlet is more, shows graininess, and big fragment is evenly distributed with most longitudinal voids that closely are arranged in parallel, space Long Circle, crescent, strip or slit-like; Conduit is scalariform, reticulate pattern and bordered pit vessel, diameter 20～70 μ m;
(2) get the drug combination preparation of the present invention that is equivalent to crude drug 18-25g, add ethanol 25ml reflux 1 hour, filter, filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets the arctiin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to the thin layer chromatography test, draw reference substance solution 1～2ul, sample solution 2～4ul, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water (40: 10: 1) is developing solvent, launches, and takes out, dry, spray is with 5% vanillin sulfuric acid solution, and hot blast blows to clear spot; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(3) get and be equivalent to crude drug 18-25g drug combination preparation of the present invention, add 15% sulphuric acid 20ml, add chloroform 30ml after the jolting, reflux 2 hours is divided and is got chloroform layer, waves to about 1ml, as need testing solution; Other gets Radix Platycodonis control medicinal material 2g, shines medical material solution in pairs with legal system; According to the thin layer chromatography test, draw control medicinal material solution 1～2ul, sample solution 2～4ul, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction-ethyl acetate (2: 0.8) is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and hot blast blows to clear spot; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the aubergine speckle of same color;
Assay:
High performance liquid chromatography, chromatographic condition and system suitability test are filler (4.6 * 150mm, 5 μ m) with octadecylsilane chemically bonded silica; Methanol-water solution (1: 1.1) is mobile phase; The detection wavelength is 280nm; Number of theoretical plate calculates by arctiin should be not less than 1500;
The preparation precision of reference substance solution takes by weighing the 5mg arctiin, places the 10ml volumetric flask, adds methanol to scale, shakes up, and filters with microporous filter membrane (0.45 μ m), promptly; (containing arctiin 0.5mg among every 1ml)
The about 2g of powder under the drug combination preparation content uniformity item of the present invention is got in the preparation of need testing solution, and accurate the title decides, and puts in the tool plug conical flask, precision adds methanol 50ml, claims to decide weight, supersound process (power 250W, frequency 40KHZ) 20 minute, cool, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, get supernatant and filter with microporous filter membrane (0.45 μ m),, promptly;
Accurate respectively reference substance liquid and each the 10 μ l injection chromatograph of liquid of test sample liquid drawn of algoscopy measured, promptly;
Be equivalent to crude drug 1.5-2.5g drug combination preparation of the present invention and contain Fructus Arctii with arctiin (C
37H
34O
11) must not be less than 2.30mg.
The present composition has good drug effect, compare existing preparation flu recovering capsule and show better drug effect, and scope of the present invention can realize that pharmacological effect of the present invention simultaneously, through screening, the unexpected discovery, in some scope of compositions, more outstanding pharmacological effect is arranged.
The method of quality control of Chinese medicine composition provided by the present invention, be by obtaining behind the creative experiment sieving of big measuring, pass through screening in the discrimination method to sample treatment, the selection of developing solvent, make and differentiate that specificity is fine, and method is economic and practical, the result is quick, and can both use different lamellaes.Pass through screening in the content assaying method to sample, test sample processing method, the selection of developing solvent, make content assaying method effectivelyly to carry out quality control, and will compare more stable that product that additive method measures shows on pharmacological effect with the product that this method is measured to product.
Following experimental example and embodiment are used to further specify but are not limited to the present invention.
Experimental example 1 pharmacological testing
1, the effect of inducing sweat
Choose basic threshold value and be 10～20 seconds 40 of female mices, body weight 18～22g, be divided into 4 groups at random, every group 10, survey each Mus threshold of pain with hot plate method before the administration, drug component of the present invention An be not clinical with 30 times of dosage, 15 times of gastric infusion medicines of the present invention (press embodiment 9 prepared) once, positive controls is irritated the stomach flu recovering capsules once by clinical with dosage 30 times, the blank group gives isometric(al) normal saline 0.2ml/10g once, after the last administration under right back sufficient plantar aponeurosis SC1% carrageenin aqueous solution 0.1ml/ Mus, after the administration 30,60,90, surveyed with method in 120 minutes and respectively organize the mice threshold of pain, carry out statistical analysis, the results are shown in Table with the t check
The mice hot plate is caused the influence of pain
| Group | Dosage g.kg -1 | The threshold of pain (g), basis | Behind the medicine (minute) threshold of pain (g) | |||
| 30 | 60 | 90 | 120 | |||
| Blank | - | 9.2± 1.8 | 9.3±1.2 | 9.4±2.07 | 10.1± 1.83 | 10.0± 1.8 |
| Positive controls | 1.0 | 8.2± 1.2 | 13.6± 2.1 | 12.7± 1.57 * | 10.8± 1.5 | 9.5± 1.7 |
| Of the present invention group | 1.0 | 8.0± 0.7 | 13.3± 3.2 | 11.0± 2.62 * | 9.7± 1.7 * | 8.3± 2.6 * |
| The present invention | 0.5 | 8.4± | 13.5± | 12.6±1.8 | 10.6± | 9.7± |
| Group | 1.4 | 1.4 | 2.0 | 1.6 |
*P＜0.05
The result shows: medicine group of the present invention and positive controls relatively after 30 minutes, demonstrate analgesic effect in administration, and analgesic effect has significance to improve.
Refrigeration function
Choose 40 of the rats of 36～38 ℃ of anus temperature, body weight 180～220g, male and female have both, gastric infusion, every rat paw SC1% carrageenin 0.1ml is divided into 4 groups at random by sex, and 10 every group, the administration group is pressed 1g.kg
-1, 0.5g.kg
-1Gastric infusion, positive controls by clinical with 30 times of dosage once, the blank group gives isometric(al) normal saline 0.2ml/10g once, surveys after the pyrogenicity 4,5,6,7 hours anus temperature, with the moulding group relatively, carry out the analysis of t inspection statistics with difference, the results are shown in Table
Separate heat test
| Group | Dosage g.kg -1 | Normal anus temperature (℃) | After the pyrogenicity (hour) the anus temperature approach (℃) | |||
| 4 | 5 | 6 | 7 | |||
| Blank | - | 36.9± 0.64 | 0.66± 0.22 | 1.71± 0.86 | 1.91± 0.67 | 2.0± 0.48 |
| Positive controls | 1.0 | 37.2± 0.76 | 0.56± 0.31 | 0.95± 0.32 | 1.82± 0.72 | 1.58± 0.79 |
| Of the present invention group | 1.0 | 36.5± 1.40 | 0.50± 0.29 | 0.81± 0.57 * | 0.97± 0.88 * | 0.74± 0.48 * |
| Of the present invention group | 0.5 | 36.5± 0.54 | 0.58± 0.25 | 0.94± 0.35 | 1.81± 0.76 | 1.60± 0.83 |
*P＜0.05
The result shows: medicine group of the present invention and positive controls are relatively separated thermal effect has significance to improve.
Experimental example 2
Prescription I
Cornu Saigae Tataricae 15g Fructus Arctii 200g Semen Sojae Preparatum 150g Flos Lonicerae 500g
Herba Schizonepetae 200g Fructus Forsythiae 500g Herba Lophatheri 100g Radix Platycodonis 300g
Oleum menthae 30ml Radix Glycyrrhizae 300g
Prescription II
Cornu Saigae Tataricae 18g Fructus Arctii 100g Semen Sojae Preparatum 100g Flos Lonicerae 450g
Herba Schizonepetae 150g Fructus Forsythiae 450g Herba Lophatheri 120g Radix Platycodonis 350g
Oleum menthae 40ml Radix Glycyrrhizae 350g
Matched group:
Cornu Saigae Tataricae 7.5g Fructus Arctii 240g Semen Sojae Preparatum 150g Flos Lonicerae 360g
Herba Schizonepetae 180g Fructus Forsythiae 360g Herba Lophatheri 180g Radix Platycodonis 240g
Oleum menthae (or Mentholum 0.75g) 15ml Radix Glycyrrhizae 150g
According to the prescription ratio weighting raw materials material of medicine group I, medicine group II and matched group,,, the results are shown in following table with the flu recovering capsule analgesic activity that relatively induces sweat according to the foregoing description 1 prepared.
Medicine to the mice hot plate cause the pain influence (
)
| Group | Dosage g.kg -1 | The threshold of pain (g), basis | Behind the medicine (minute) threshold of pain (g) | |||
| 30 | 60 | 90 | 120 | |||
| Medicine group I | 1.0 | 8.1± 1.4 | 12.3± 1.9 | 11.2±1.6 | 9.5± 1.6 | 8.5± 1.8 |
| Medicine group II | 1.0 | 8.2± 0.6 | 12.1± 3.3 | 11.0±2.7 | 9.6± 1.8 | 8.4± 2.4 |
| Matched group | 1.0 | 8.1± 1.1 | 13.4± 1.6* | 12.3± 2.1* | 10.7± 1.7* | 9.3± 1.4* |
| Flu recovering capsule medicine group | 1.0 | 8.0± 1.3 | 14.1± 2.5△ | 13.3±2.1 △ | 11.9± 2.2△ | 10.4± 1.8△ |
Annotate: the * matched group is compared P＜0.05 with medicine group I, II, and the △ matched group is compared P＜0.01 with flu health medicine group
The result shows: table function is separated in medicament composition capsule agent of the present invention, and there were significant differences (P＜0.01) with flu recovering capsule medicine group.Medicine group I, II and matched group are relatively separated table function better (P＜0.05).
Experimental example 3 capsules are differentiated screening experiment
1, the thin layer discrimination method of Fructus Arctii
1. the alcohol reflux time was preferred during sample solution prepared in the discrimination method of the present invention (2):
Get 5 parts of pharmaceutical preparatioies of the present invention that are equivalent to crude drug 19g, use the alcohol reflux different time, measure arctiin content in the extracting solution, the results are shown in following table:
| Extraction time (h) | 0.5 | 0.8 | 1.0 | 1.5 | 2.0 |
| Arctiin content (mg) | 2.32 | 3.24 | 3.87 | 3.89 | 3.87 |
As can be seen from the above table, reflux, extract, 1.0h just can extract arctiin wherein fully, is 1.0h so this tests preferred extraction time.
2. the developing solvent consumption proportion is preferred in the discrimination method of the present invention (2):
Get need testing solution 5 μ l, point is on different silica gel g thin-layer plates, it with chloroform-methanol-water proportioning respectively 35: 8: 1,35: 10: 1,40: 10: 1,45: 10: 1,45: 12: 1 developing solvent expansion, take out, dry, spray is with 5% vanillin sulfuric acid solution, and hot blast blows to clear spot, observe the unfolded effect of test sample on each lamellae, the results are shown in following table:
| The developing solvent proportioning | 3 5∶8∶1 | 35∶10∶1 | 40∶10∶1 | 45∶10∶1 | 45∶12∶1 |
| Launch effect | Relatively poor | Difference | Good | Difference | Better |
Developing solvent proportioning as can be seen from the above table is 40: 10: 1 o'clock, and it is best that need testing solution launches effect, and appearance hangover, principal spot separate phenomenons such as bad.
3. sample solution point sample amount is preferred in the discrimination method of the present invention (2):
Get need testing solution 0.1～1 μ l, 1～2 μ l, 2～3 μ l, 3～4 μ l, reference substance solution 1～2 μ l, point is on same silica gel g thin-layer plate, developing solvent with chloroform-methanol-water (40: 10: 1) launches, and takes out, and dries, spray is with 5% vanillin sulfuric acid solution, hot blast blows to clear spot, observes the effect of test sample principal spot colour developing on the lamellae, the results are shown in following table:
| The point sample amount | 0.1～1μl | 1～2μl | 2～3μl | 3·4μl |
| Effect | Test sample is at corresponding reference substance position immaculate | Test sample is more shallow in corresponding reference substance position spot colors | Test sample is good at corresponding reference substance position speckle color developing effect | Test sample is good at corresponding reference substance position speckle color developing effect |
Test sample point sample amount is when 2～4 μ l as can be seen from the above table, and color developing effect is good on lamellae, is fit to test requirements document.
4. negative control test
Get the negative sample that lacks Fructus Arctii, prepare negative control solution, launch the back and corresponding speckle on the reference substance solution correspondence position, do not occur, illustrate that selected identification experiment specificity is strong according to need testing solution preparation method in the discrimination method of the present invention (2).
2, the discrimination method of Radix Platycodonis
1. add 15% sulphuric acid 20ml in the sample solution preparation in the discrimination method of the present invention (3), add chloroform 30ml after the jolting, reflux time preferred:
Get 5 parts of pharmaceutical preparatioies of the present invention that are equivalent to crude drug 20g, add 15% sulphuric acid 20ml, add chloroform 30ml after the jolting, the reflux different time is measured wherein total saponins percentage composition, the results are shown in following table:
| Extraction time (h) | 1.0 | 1.5 | 2.0 | 2.5 | 3.0 |
| Total saponin content (%) | 0.67 | 0.82 | 0.91 | 0.93 | 0.94 |
As can be seen from the above table, reflux, extract, 2.0h just can extract arctiin wherein fully substantially, is 2.0h so this tests preferred extraction time.
2. the developing solvent consumption proportion is preferred in the discrimination method of the present invention (3):
Get need testing solution 5 μ l, point is on different silica gel g thin-layer plates, it with hexane-ethyl acetate proportioning respectively 1: 0.5,2: 0.8,3: 0.8,4: 1 developing solvent expansion, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and hot blast blows to clear spot, observe the unfolded effect of test sample speckle on each lamellae, the results are shown in following table:
| The developing solvent proportioning | 1∶0.5 | 2∶0.8 | 3∶0.8 | 4∶1 |
| Launch effect | Difference | Good | Difference | Very poor |
Developing solvent proportioning as can be seen from the above table is 2: 0.8 o'clock, and it is best that need testing solution launches effect, and appearance hangover, principal spot separate phenomenons such as bad.
3. sample solution point sample amount is preferred in the discrimination method of the present invention (3):
Get need testing solution 0.1～1 μ l, 1～2 μ l, 2～3 μ l, 3～4 μ l, reference substance solution 1～2 μ l, point is on same silica gel g thin-layer plate, developing solvent with hexane-ethyl acetate (2: 0.8) launches, and takes out, and dries, spray is with 10% ethanol solution of sulfuric acid, hot blast blows to clear spot, observes the effect of test sample principal spot colour developing on the lamellae, the results are shown in following table:
| The point sample amount | 0.1～1μl | 1～2μl | 2～3μl | 3·4μl |
| Effect | Test sample is at corresponding reference substance position immaculate | Test sample is more shallow in corresponding reference substance position spot colors | Test sample is good at corresponding reference substance position speckle color developing effect | Test sample is good at corresponding reference substance position speckle color developing effect |
Test sample point sample amount is when 2～4 μ l as can be seen from the above table, and color developing effect is good on lamellae, is fit to test requirements document.
4. negative control test
Get the negative sample that lacks Radix Platycodonis, prepare negative control solution, launch the back and corresponding speckle on the reference substance solution correspondence position, do not occur, illustrate that selected identification experiment specificity is strong according to need testing solution preparation method in the discrimination method of the present invention (3).
The experiment of experimental example 4 capsule assays
The content assaying method of arctiin
Adopt colleges and universities' liquid phase method to measure the content of the Fructus Arctii in the medicine of the present invention, to improve quality determining method of the present invention.
1. the selection of the extracting method of need testing solution
Adopting orthogonal test, is factor with consumption, extraction time, the extraction time that extracts solvent, arranges test.Get the medicine of the present invention that is equivalent to crude drug 19g, the accurate title, decide, and puts in the tool plug conical flask, adds methanol, and supersound process (power 250W, frequency 40KHZ) is measured wherein arctiin content, the results are shown in following table:
Preferred factor level table
| Level | A solvent load (ml) | B extraction time (min) | The C extraction time |
| 1 | 10 | 10 | 1 |
| 2 | 50 | 20 | 2 |
| 3 | 100 | 40 | 3 |
Table 4. factor screening orthogonal experiment data table
| Sequence number | A | B | C | D | Arctiin content (mg/g) |
| 1 | 1 | 1 | 1 | 1 | 7.325 |
| 2 | 1 | 2 | 2 | 2 | 8.738 |
| 3 | 1 | 3 | 3 | 3 | 8.741 |
| 4 | 2 | 1 | 2 | 3 | 7.915 |
| 5 | 2 | 2 | 3 | 1 | 9.091 |
| 6 | 2 | 3 | 1 | 2 | 9.087 |
| 7 | 3 | 1 | 3 | 2 | 7.924 |
| 8 | 3 | 2 | 1 | 3 | 9.082 |
| 9 | 3 | 3 | 2 | 1 | 9.081 |
| I | 24.804 | 23.164 | 25.494 | 25.497 | Σ＝76.984 |
| II | 26.093 | 26.911 | 25.734 | 25.749 | |
| III | 26.087 | 26.909 | 25.756 | 25.738 | CT＝658.50403 |
| R j | 1.289 | 3.747 | 0.262 | 0.252 | |
| SS j | 0.367516 | 3.118338 | 0.014081 | 0.013523 |
Analysis of variance table
| Soruces of variation | Sum of deviation square | Degree of freedom | Mean square and | The F ratio | Significance |
| A | 0.367516 | 2 | 0.183758 | 27.18 | * |
| B | 3.118338 | 2 | 1.559169 | 230.60 | ** |
| C | 0.014081 | 2 | 0.007040 | 1.04 | |
| e(D) | 0.013523 | 2 | 0.006761 |
Analyze as can be seen from table R value, influence factor's primary and secondary is B＞A＞C, and the intuitive analysis optimum extraction process is A
2B
2C
3, from analysis of variance table as can be seen factor A, B have significance, and factor C does not have the significance influence to extracting the result, so choose A
2B
2C
1Be the optimum extraction scheme.Promptly adding 50ml methanol supersound extraction 20min once gets final product.
To the detection method of content that medicine of the present invention adopted, carried out related side's science of law from aspects such as linear relationship, stability, precision, repeatability, the response rate and investigated, concrete outcome is as follows:
(1) linear relationship is investigated and to be got reference substance solution (50mg-10ml) and shake up, accurate respectively 2,4,6,8,10, the 12 μ l of absorption inject high performance liquid chromatograph, measure peak area, the results are shown in following table, and drawing standard curve, show that arctiin is linear between 1.0ug-6.0ug, its regression equation is:
Area＝632.411382*Amt+19.170517(r＝0.99987)
| Sample size (ug) | 1.0 | 2.0 | 3.0 | 4.0 | 5.0 | 6.0 |
| Peak area | 644.36877 | 1294.01404 | 1934.76135 | 2570.33228 | 3194.13062 | 3777.22559 |
(2) stability test reference substance solution respectively at preparing the back 0,2,4,6,12,24 hour, is measured in accordance with the law, and the result shows that it is basicly stable in 24 hours, the results are shown in following table
| Time (hr) | 0 | 2 | 4 | 6 | 12 | 24 |
| Peak area | 3131.06787 | 3184.60322 | 3157.26355 | 3137.25489 | 3175.03564 | 3136.09851 |
| RSD(％) | 0.711 | |||||
(3) the accurate need testing solution 10 μ l that draw of precision test repeat sample introduction 5 times, try to achieve relative standard deviation＜2%, the results are shown in following table
| Number of times | 1 | 2 | 3 | 4 | 5 |
| Peak area | 2488.12366 | 2485.51865 | 2482.71233 | 2476.12166 | 2479.32166 |
| RSD(％) | 0.193 | ||||
(4) 5 parts in same sample is got in the repeatability test, measures respectively, tries to achieve relative standard deviation＜2%, the results are shown in following table
| Number of times | 1 | 2 | 3 | 4 | 5 |
| Content (mg/ grain) | 3.843 | 3.826 | 3.809 | 3.835 | 3.797 |
| Average content (mg/ grain) | 3.822 | ||||
| RSD(％) | 0.493 | ||||
(5) the recovery test precision take by weighing known content same batch sample 1.0g more respectively precision take by weighing arctiin reference substance 9.0mg, press the preparation method operation of text need testing solution, measure its content, and calculate its response rate, measurement result sees the following form:
| Tested number | Sampling amount (g) | Arctiin in the sample | Add arctiin (mg) | Measure the arctiin amount | The response rate (%) | Average recovery rate (%) | RSD(％) |
| (mg) | (mg) | ||||||
| 1 | 1.0235 | 9.3241 | 9.2 | 18.1062 | 95.46 | 97.59 | 1.587 |
| 2 | 0.9760 | 8.8914 | 9.5 | 18.0922 | 96.85 | ||
| 3 | 1.0424 | 9.4963 | 8.7 | 18.1058 | 98.96 | ||
| 4 | 0.9944 | 9.0590 | 9.2 | 18.0262 | 97.47 | ||
| 5 | 0.9856 | 8.9788 | 8.9 | 17.8085 | 99.21 |
From above result of the test as can be seen, its linear relationship of the content assaying method that medicine of the present invention adopted, stability, precision, repeatability etc. are all good, can effectively control drug quality of the present invention.Following embodiment all can realize the described effect of above-mentioned experimental example
The specific embodiment
Embodiment 1:
Cornu Saigae Tataricae 7.5g Fructus Arctii 240g Semen Sojae Preparatum 150g
Flos Lonicerae 360g Herba Schizonepetae 180g Fructus Forsythiae 360g
Herba Lophatheri 180g Radix Platycodonis 240g Oleum menthae (or Mentholum
0.75g) 15ml Radix Glycyrrhizae 150g
[method for making] above ten flavors, the Cornu Saigae Tataricae file is ground into fine powder, and balloonflower powder is broken into fine powder, Herba Schizonepetae, Fructus Forsythiae extracts volatile oil, adds 10 times of amounts of water, distillation time 5 hours, medicinal residues and medicinal liquid add Flos Lonicerae, Herba Lophatheri, Semen Sojae Preparatum, Fructus Arctii, Radix Glycyrrhizae decocts secondary, adds 8 times of water gagings for the first time, adds 6 times of water gagings for the second time, each 2 hours, collecting decoction filtered, filtrate is concentrated into relative density and is about 1.3 (50～55 ℃), adds Platycodon Root and right amount of auxiliary materials, mixing, make granule, drying is pulverized, and sieves, spray is with Oleum menthae and Herba Schizonepetae, the ethanol dilution liquid of Forsythia volatile oil, add the Cornu Saigae Tataricae fine powder again, mixing incapsulates, make 1000, promptly.
Differentiate:
(1) get this product, put microscopically and observe: irregular shape fragment, nearly colourless or light gray, sub-translucent, glossy slightly, accidental sepia pigment granule; Fractionlet is more, shows graininess, and big fragment is evenly distributed with most longitudinal voids that closely are arranged in parallel, space Long Circle, crescent, strip or slit-like; Conduit is scalariform, reticulate pattern and bordered pit vessel, diameter 20～70 μ m;
(2) get 10 of this product, add ethanol 25ml reflux 1 hour, filter, filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets the arctiin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000), draw reference substance solution 1～2ul, sample solution 2～4ul, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water (40: 10: 1) is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and hot blast blows to clear spot; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(3) get this product 5g, add 15% sulphuric acid 20ml, add chloroform 30ml after the jolting, reflux 2 hours is divided and is got chloroform layer, waves to about 1ml, as need testing solution; Other gets Radix Platycodonis control medicinal material 2g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000), draw control medicinal material solution 1～2ul, sample solution 2～4ul, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction-ethyl acetate (2: 0.8) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and hot blast blows to clear spot; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the aubergine speckle of same color;
Assay:
High performance liquid chromatography, chromatographic condition and system suitability test are filler (4.6 * 150mm, 5 μ m) with octadecylsilane chemically bonded silica; Methanol-water solution (1: 1.1) is mobile phase; The detection wavelength is 280nm; Number of theoretical plate calculates by arctiin should be not less than 1500;
The preparation precision of reference substance solution takes by weighing the 5mg arctiin, places the 10ml volumetric flask, adds methanol to scale, shakes up, and filters with microporous filter membrane (0.45 μ m), promptly; (containing arctiin 0.5mg among every 1ml)
The about 2g of powder under this product content uniformity item is got in the preparation of need testing solution, and accurate the title decides, and puts in the tool plug conical flask, precision adds methanol 50ml, claims to decide weight, supersound process (power 250W, frequency 40KHZ) 20 minute, cool, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, get supernatant and filter with microporous filter membrane (0.45 μ m),, promptly;
Accurate respectively reference substance liquid and each the 10 μ l injection chromatograph of liquid of test sample liquid drawn of algoscopy measured, promptly;
Every of this product contains Fructus Arctii with arctiin (C
37H
34O
11) must not be less than 2.30mg.
[function with cure mainly] clearing away heat and expelling pathogen in the exterior.Be used for influenza, the cough due to common cold, dizzy heating, laryngopharynx swelling and pain.
[usage and consumption] is oral, one time 2,2-3 time on the one.
[specification] every dress 0.42g
Embodiment 2: drop pill
Cornu Saigae Tataricae 15g Fructus Arctii 200g Semen Sojae Preparatum 150g
Flos Lonicerae 500g Herba Schizonepetae 200g Fructus Forsythiae 500g
Herba Lophatheri 100g Radix Platycodonis 300g Oleum menthae 30ml
Radix Glycyrrhizae 300g
The Cornu Saigae Tataricae file is ground into fine powder, balloonflower powder is broken into fine powder, Herba Schizonepetae, Fructus Forsythiae extracts volatile oil, adding water 8-12 doubly measures, distillation time 4-7 hour, medicinal residues and medicinal liquid add Flos Lonicerae, Herba Lophatheri, Semen Sojae Preparatum, Fructus Arctii, Radix Glycyrrhizae decocts 2-3 time, add 5-9 times of water gaging at every turn, each 1-3 hour, collecting decoction filters, and filtrate is concentrated into relative density and is about 1.3-1.6 (50～55 ℃), volatile oil with said extracted, the Cornu Saigae Tataricae fine powder, Radix Platycodonis fine powder and water are carried clear paste, with an amount of substrate (can be Macrogol 4000 or 6 000, sodium stearate, any one or two kinds of above mixture in the glycerin gelatine) and the proper amount of surfactant mix homogeneously, insulation (50～70 ℃) splashes in the liquid coolant (5～10 ℃), make drop pill, promptly.
Embodiment 3: effervescent
Cornu Saigae Tataricae 18g Fructus Arctii 100g Semen Sojae Preparatum 100g gold
Flos Lonicerae 450g Herba Schizonepetae 150g Fructus Forsythiae 450g phyllostachys nigra (lodd.ex lindl.) munro var.henonis (miff.) spapf et rendle
Leaf 120g Radix Platycodonis 350g Oleum menthae 40ml Radix Glycyrrhizae
350g
The Cornu Saigae Tataricae file is ground into fine powder, and balloonflower powder is broken into fine powder, Herba Schizonepetae, Fructus Forsythiae extracts volatile oil, add 10 times of amounts of water, distillation time 5 hours, medicinal residues and medicinal liquid add Flos Lonicerae, Herba Lophatheri, Semen Sojae Preparatum, Fructus Arctii, Radix Glycyrrhizae decocts secondary, add for the first time 8 times of water gagings, for the second time add 6 times of water gagings, each 2 hours, collecting decoction, filter, filtrate is concentrated into relative density and is about 1.3 (50～55 ℃), adds balloonflower powder, Cornu Saigae Tataricae fine powder and right amount of auxiliary materials, mixing, make granule, drying is pulverized, and sieves, with Oleum menthae and Herba Schizonepetae, the ethanol dilution liquid of Forsythia volatile oil, and sodium bicarbonate, Polyethylene Glycol, alcohol mixeding liquid sprays in the drug particles of above-mentioned preparation granulate, with an amount of citric acid, cyclamate and fumaric acid add, mixing, tabletting, promptly.
Embodiment 4:
Cornu Bubali 7.5g Fructus Arctii 280g Semen Sojae Preparatum 150g Flos Lonicerae
360g Radix Saposhnikoviae 200g Fructus Forsythiae 360g Herba Lophatheri 180g
Radix Platycodonis 240g Oleum menthae (or Mentholum 0.75g) 15ml Radix Glycyrrhizae 250g
This pharmaceutical composition adds conventional adjuvant, makes oral liquid by common process.
Embodiment 5:
Cornu Saigae Tataricae 15g Fructus Arctii 200g Semen Sojae Preparatum 150g Flos Lonicerae 500g
Herba Schizonepetae 200g Fructus Forsythiae 500g Herba Lophatheri 100g Radix Platycodonis 300g
Oleum menthae 30ml Radix Glycyrrhizae 300g
More than ten flavors, Cornu Saigae Tataricae file is ground into fine powder, balloonflower powder is broken into fine powder, Herba Schizonepetae, Fructus Forsythiae extracts volatile oil, adds 10 times of amounts of water, distillation time 5 hours, medicinal residues and medicinal liquid add Flos Lonicerae, Herba Lophatheri, Semen Sojae Preparatum, Fructus Arctii, Radix Glycyrrhizae decocts secondary, adds 8 times of water gagings for the first time, adds 6 times of water gagings for the second time, each 2 hours, collecting decoction filtered, filtrate is concentrated into relative density and is about 1.3 (50～55 ℃), adds Platycodon Root and right amount of auxiliary materials, mixing, make granule, drying is pulverized, and sieves, spray is with Oleum menthae and Herba Schizonepetae, the ethanol dilution liquid of Forsythia volatile oil, add the Cornu Saigae Tataricae fine powder again, mixing incapsulates, make 1000, promptly.
Embodiment 6:
Cornu Saigae Tataricae 18g Fructus Arctii 100g Semen Sojae Preparatum 100g Flos Lonicerae 450g
Herba Schizonepetae 150g Fructus Forsythiae 450g Herba Lophatheri 120g Radix Platycodonis 350g
Oleum menthae 40ml Radix Glycyrrhizae 350g
More than ten flavors, Cornu Saigae Tataricae file is ground into fine powder, balloonflower powder is broken into fine powder, Herba Schizonepetae, Fructus Forsythiae extracts volatile oil, adds 10 times of amounts of water, distillation time 5 hours, medicinal residues and medicinal liquid add Flos Lonicerae, Herba Lophatheri, Semen Sojae Preparatum, Fructus Arctii, Radix Glycyrrhizae decocts secondary, adds 8 times of water gagings for the first time, adds 6 times of water gagings for the second time, each 2 hours, collecting decoction filtered, filtrate is concentrated into relative density and is about 1.3 (50～55 ℃), adds Platycodon Root and right amount of auxiliary materials, mixing, make granule, drying is pulverized, and sieves, spray is with Oleum menthae and Herba Schizonepetae, the ethanol dilution liquid of Forsythia volatile oil, add the Cornu Saigae Tataricae fine powder again, mixing incapsulates, make 1000, promptly.
Embodiment 7:
Cornu Bubali 9 weight portion Fructus Arctiis 150 weight portions
Semen Sojae Preparatum 180 weight portion Flos Loniceraes 260 weight portions
Radix Saposhnikoviae 180 weight portion Fructus Forsythiaes 260 weight portions
Light place leaf 200 weight portion Radix Platycodoniss 200 weight portions
Oleum menthae 20 parts by volume Radix Glycyrrhizaes 180 weight portions.
More than ten flavors, Cornu Bubali file is ground into fine powder, balloonflower powder is broken into fine powder, Fructus Forsythiae extracts volatile oil, adds 10 times of amounts of water, distillation time 5 hours, medicinal residues and medicinal liquid add Radix Saposhnikoviae, Flos Lonicerae, Herba Lophatheri, Semen Sojae Preparatum, Fructus Arctii, Radix Glycyrrhizae decocts secondary, adds 8 times of water gagings for the first time, adds 6 times of water gagings for the second time, each 2 hours, collecting decoction filtered, filtrate is concentrated into relative density and is about 1.3 (50～55 ℃), adds Platycodon Root and right amount of auxiliary materials, mixing, make granule, drying is pulverized, and sieves, spray is with Oleum menthae and Herba Schizonepetae, the ethanol dilution liquid of Forsythia volatile oil, add the Cornu Saigae Tataricae fine powder again, mixing incapsulates, make 1000, promptly.
Claims (10)
1, a kind of pharmaceutical composition for the treatment of flu is characterized in that the crude drug of this pharmaceutical composition consists of:
Cornu Bubali 3-25 weight portion Fructus Arctii 100-400 weight portion
Semen Sojae Preparatum 100-400 weight portion Flos Lonicerae 200-500 weight portion
Radix Saposhnikoviae 100-500 weight portion Fructus Forsythiae 200-500 weight portion
Herba Lophatheri 100-400 weight portion Radix Platycodonis 100-400 weight portion
Oleum menthae 5-40 parts by volume Radix Glycyrrhizae 100-400 weight portion.
2, pharmaceutical composition as claimed in claim 1, it is characterized in that in the crude drug composition in this pharmaceutical composition: Cornu Bubali 3-25 weight portion is replaced with Cornu Saigae Tataricae 3-25 weight portion, and Radix Saposhnikoviae 100-500 weight portion is replaced by Herba Schizonepetae 100-500 weight portion.
3, pharmaceutical composition as claimed in claim 2 is characterized in that the crude drug of this pharmaceutical composition consists of:
Cornu Saigae Tataricae 15-20 weight portion Fructus Arctii 100-200 weight portion
Semen Sojae Preparatum 100-200 weight portion Flos Lonicerae 400-500 weight portion
Herba Schizonepetae 100-200 weight portion Fructus Forsythiae 400-500 weight portion
Herba Lophatheri 100-300 weight portion Radix Platycodonis 300-400 weight portion
Oleum menthae 30-50 parts by volume Radix Glycyrrhizae 300-400 weight portion.
4, pharmaceutical composition as claimed in claim 3 is characterized in that the crude drug of this pharmaceutical composition consists of:
Cornu Saigae Tataricae 15 weight portion Fructus Arctiis 200 weight portion Semen Sojae Preparatums 150 weight portions
Flos Lonicerae 500 weight portion Herba Schizonepetae 200 weight portion Fructus Forsythiaes 500 weight portions
Herba Lophatheri 100 weight portion Radix Platycodoniss 300 weight portion Oleum menthae 30 parts by volume
Radix Glycyrrhizae 300 weight portions.
5, pharmaceutical composition as claimed in claim 3 is characterized in that the crude drug of this pharmaceutical composition consists of:
Cornu Saigae Tataricae 18 weight portion Fructus Arctiis 100 weight portion Semen Sojae Preparatums 100 weight portions
Flos Lonicerae 450 weight portion Herba Schizonepetae 150 weight portion Fructus Forsythiaes 450 weight portions
Herba Lophatheri 120 weight portion Radix Platycodoniss 350 weight portion Oleum menthae 40 parts by volume
Radix Glycyrrhizae 350 weight portions.
6, as the described preparation of drug combination method of claim 2-5, it is characterized in that this method is: the Cornu Saigae Tataricae file is ground into fine powder, balloonflower powder is broken into fine powder, Herba Schizonepetae, Fructus Forsythiae extracts volatile oil, adds water 8-12 and doubly measures, distillation time 4-7 hour, medicinal residues and medicinal liquid add Flos Lonicerae, Herba Lophatheri, Semen Sojae Preparatum, Fructus Arctii, Radix Glycyrrhizae decocts 2-3 time, adds 5-9 times of water gaging at every turn, each 1-3 hour, collecting decoction, filter, filtrate is concentrated into relative density and is about 1.3-1.6 (50～55 ℃), adds Platycodon Root and right amount of auxiliary materials, mixing, make granule, drying is pulverized, sieve, spray is with Oleum menthae and Herba Schizonepetae, the ethanol dilution liquid of Forsythia volatile oil adds the Cornu Saigae Tataricae fine powder, mixing again, incapsulate, promptly.
7, preparation of drug combination method as claimed in claim 6, it is characterized in that this method is: the Cornu Saigae Tataricae file is ground into fine powder, balloonflower powder is broken into fine powder, Herba Schizonepetae, Fructus Forsythiae extracts volatile oil, adds 10 times of amounts of water, distillation time 5 hours, medicinal residues and medicinal liquid add Flos Lonicerae, Herba Lophatheri, Semen Sojae Preparatum, Fructus Arctii, Radix Glycyrrhizae decocts secondary, adds 8 times of water gagings for the first time, adds 6 times of water gagings for the second time, each 2 hours, collecting decoction filters, and filtrate is concentrated into relative density and is about 1.3 (50～55 ℃), add Platycodon Root and right amount of auxiliary materials, mixing is made granule, drying, pulverize, sieve, spray is with Oleum menthae and Herba Schizonepetae, the ethanol dilution liquid of Forsythia volatile oil adds the Cornu Saigae Tataricae fine powder again, mixing incapsulates promptly.
8,, it is characterized in that this method of quality control comprises one or more in following discrimination method and/or the assay as the method for quality control of the described pharmaceutical composition of claim 1-5:
Differentiate:
A. get pharmaceutical composition solid preparation of the present invention, put microscopically and observe: irregular shape fragment, nearly colourless or light gray, sub-translucent, glossy slightly, accidental sepia pigment granule; Fractionlet is more, shows graininess, and big fragment is evenly distributed with most longitudinal voids that closely are arranged in parallel, space Long Circle, crescent, strip or slit-like; Conduit is scalariform, reticulate pattern and bordered pit vessel, diameter 20～70 μ m;
B, get the drug combination preparation of the present invention that is equivalent to crude drug 18-25g, add ethanol 25ml reflux 0.8-1.5 hour, filter, filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets the arctiin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to the thin layer chromatography test, draw reference substance solution 1～2ul, sample solution 2～4ul, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water (35-45: 8-12: 1) be developing solvent, launch, take out, dry, spray is with 4-6% vanillin sulfuric acid solution, and hot blast blows to clear spot; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
C, get and be equivalent to crude drug 18-25g drug combination preparation of the present invention, add 15% sulphuric acid 20ml, add chloroform 30ml after the jolting, reflux 1-3 hour, divide and get chloroform layer, evaporate into about 1ml, as need testing solution; Other gets Radix Platycodonis control medicinal material 2g, shines medical material solution in pairs with legal system; According to the thin layer chromatography test, draw control medicinal material solution 1～2ul, sample solution 2～4ul, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction-ethyl acetate (1-4: 0.5-1) be developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and hot blast blows to clear spot; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the aubergine speckle of same color;
Assay:
High performance liquid chromatography, chromatographic condition and system suitability test are filler (4.6 * 150mm, 5 μ m) with octadecylsilane chemically bonded silica; Methanol-water solution (1: 1-2) be mobile phase; The detection wavelength is 280nm; Number of theoretical plate calculates by arctiin should be not less than 1500;
The preparation of reference substance solution: precision takes by weighing the 5mg arctiin, places the 10ml volumetric flask, adds methanol to scale, shakes up, and filters with microporous filter membrane (0.45 μ m), promptly; The preparation of (containing arctiin 0.5mg among every 1ml) need testing solution: get the about 2g of powder under the drug combination preparation content uniformity item of the present invention, the accurate title, decide, and puts in the tool plug conical flask, precision adds methanol 50ml, claims to decide weight, supersound process (power 250W, frequency 40KHZ) 15-25 minute, cool, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, get supernatant and filter with microporous filter membrane (0.45 μ m),, promptly;
Algoscopy: accurate respectively reference substance liquid and each 10 μ l injection chromatograph of liquid of test sample liquid drawn, measure, promptly; Be equivalent to crude drug 1.5-2.5g drug combination preparation of the present invention and contain Fructus Arctii with arctiin (C
37H
34O
11) must not be less than 2.30mg.
9, the method for quality control of pharmaceutical composition as claimed in claim 8 is characterized in that this method of quality control comprises one or more in following discrimination method and/or the assay:
Differentiate:
A, get pharmaceutical composition solid preparation of the present invention, put microscopically and observe: irregular shape fragment, nearly colourless or light gray, sub-translucent, glossy slightly, accidental sepia pigment granule; Fractionlet is more, shows graininess, and big fragment is evenly distributed with most longitudinal voids that closely are arranged in parallel, space Long Circle, crescent, strip or slit-like; Conduit is scalariform, reticulate pattern and bordered pit vessel, diameter 20～70 μ m;
B, get the drug combination preparation of the present invention that is equivalent to crude drug 18-25g, add ethanol 25ml reflux 1 hour, filter, filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets the arctiin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to the thin layer chromatography test, draw reference substance solution 1～2ul, sample solution 2～4ul, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water (40: 10: 1) is developing solvent, launches, and takes out, dry, spray is with 5% vanillin sulfuric acid solution, and hot blast blows to clear spot; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
C, get and be equivalent to crude drug 18-25g drug combination preparation of the present invention, add 15% sulphuric acid 20ml, add chloroform 30ml after the jolting, reflux 2 hours is divided and is got chloroform layer, waves to about 1ml, as need testing solution; Other gets Radix Platycodonis control medicinal material 2g, shines medical material solution in pairs with legal system; According to the thin layer chromatography test, draw control medicinal material solution 1～2ul, sample solution 2～4ul, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction-ethyl acetate (2: 0.8) is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and hot blast blows to clear spot; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the aubergine speckle of same color;
Assay:
High performance liquid chromatography, chromatographic condition and system suitability test are filler (4.6 * 150mm, 5 μ m) with octadecylsilane chemically bonded silica; Methanol-water solution (1: 1.1) is mobile phase; The detection wavelength is 280nm; Number of theoretical plate calculates by arctiin should be not less than 1500;
The preparation precision of reference substance solution takes by weighing the 5mg arctiin, places the 10ml volumetric flask, adds methanol to scale, shakes up, and filters with microporous filter membrane (0.45 μ m), promptly; The about 2g of powder under the drug combination preparation content uniformity item of the present invention is got in the preparation of (containing arctiin 0.5mg among every 1ml) need testing solution, and accurate the title decides, and puts in the tool plug conical flask, precision adds methanol 50ml, claims to decide weight, supersound process (power 250W, frequency 40KHZ) 20 minute, cool, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, get supernatant and filter with microporous filter membrane (0.45 μ m),, promptly;
Algoscopy, accurate respectively reference substance liquid and each 10 μ l injection chromatograph of liquid of test sample liquid drawn measured, promptly;
Be equivalent to crude drug 1.5-2.5g drug combination preparation of the present invention and contain Fructus Arctii with arctiin (C
37H
34O
11) must not be less than 2.30mg.
10, the method for quality control of pharmaceutical composition as claimed in claim 9 is characterized in that this method of quality control comprises following method:
Choose following medicine and make capsule:
Cornu Saigae Tataricae 7.5g Fructus Arctii 240g Semen Sojae Preparatum 150g Flos Lonicerae 360g Herba Schizonepetae 180g Fructus Forsythiae 360g Herba Lophatheri 180g Radix Platycodonis 240g Oleum menthae (or Mentholum 0.75g) 15ml Radix Glycyrrhizae 150g;
The Cornu Saigae Tataricae file is ground into fine powder, and balloonflower powder is broken into fine powder, Herba Schizonepetae, Fructus Forsythiae extracts volatile oil, add 10 times of amounts of water, distillation time 5 hours, medicinal residues and medicinal liquid add Flos Lonicerae, Herba Lophatheri, Semen Sojae Preparatum, Fructus Arctii, Radix Glycyrrhizae decocts secondary, add for the first time 8 times of water gagings, add 6 times of water gagings, each 2 hours for the second time, collecting decoction filters, and filtrate is concentrated into relative density and is about 1.3 (50～55 ℃), add Platycodon Root and right amount of auxiliary materials, mixing is made granule, drying, pulverize, sieve, spray is with Oleum menthae and Herba Schizonepetae, the ethanol dilution liquid of Forsythia volatile oil adds the Cornu Saigae Tataricae fine powder again, mixing, incapsulate, make 1000, promptly; Method of quality control comprises to be differentiated and assay:
Differentiate:
A, get this product, put microscopically and observe: irregular shape fragment, nearly colourless or light gray, sub-translucent, glossy slightly, accidental sepia pigment granule; Fractionlet is more, shows graininess, and big fragment is evenly distributed with most longitudinal voids that closely are arranged in parallel, space Long Circle, crescent, strip or slit-like; Conduit is scalariform, reticulate pattern and bordered pit vessel, diameter 20～70 μ m;
B, get 10 of this product, add ethanol 25ml reflux 1 hour, filter, filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets the arctiin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to the thin layer chromatography test, draw reference substance solution 1～2ul, sample solution 2～4ul, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water (40: 10: 1) is developing solvent, launches, and takes out, dry, spray is with 5% vanillin sulfuric acid solution, and hot blast blows to clear spot; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color; C, get this product 5g, add 15% sulphuric acid 20ml, add chloroform 30ml after the jolting, reflux 2 hours is divided and is got chloroform layer, waves to about 1ml, as need testing solution; Other gets Radix Platycodonis control medicinal material 2g, shines medical material solution in pairs with legal system; According to the thin layer chromatography test, draw control medicinal material solution 1～2ul, sample solution 2～4ul, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction-ethyl acetate (2: 0.8) is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and hot blast blows to clear spot; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the aubergine speckle of same color;
Assay:
High performance liquid chromatography, chromatographic condition and system suitability test are filler (4.6 * 150mm, 5 μ m) with octadecylsilane chemically bonded silica; Methanol-water solution (1: 1.1) is mobile phase; The detection wavelength is 280nm; Number of theoretical plate calculates by arctiin should be not less than 1500;
The preparation precision of reference substance solution takes by weighing the 5mg arctiin, places the 10ml volumetric flask, adds methanol to scale, shakes up, and filters with microporous filter membrane (0.45 μ m), promptly; The about 2g of powder under this product content uniformity item is got in the preparation of (containing arctiin 0.5mg among every 1ml) need testing solution, and accurate the title decides, and puts in the tool plug conical flask, precision adds methanol 50ml, claims to decide weight, supersound process (power 250W, frequency 40KHZ) 20 minute, cool, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, get supernatant and filter with microporous filter membrane (0.45 μ m),, promptly; Algoscopy, accurate respectively reference substance liquid and each 10 μ l injection chromatograph of liquid of test sample liquid drawn measured, promptly; Every of this product contains Fructus Arctii with arctiin (C
37H
34O
11) must not be less than 2.30mg.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102451401A (en) * | 2010-11-01 | 2012-05-16 | 深圳市佳泰药业股份有限公司 | Prescription of vitamin C honeysuckle and forsythia |
| CN104873815A (en) * | 2015-05-27 | 2015-09-02 | 南京同仁堂药业有限责任公司 | Traditional Chinese medicine for treating common cold and preparing method of traditional Chinese medicine |
| CN106581174A (en) * | 2017-02-13 | 2017-04-26 | 佛山市腾瑞医药科技有限公司 | Traditional Chinese medicinal composition for treating wind-heat type common colds, and preparation method thereof |
| CN106729140A (en) * | 2016-12-15 | 2017-05-31 | 贵州恒和制药有限公司 | A kind of compound preparation for treating influenza and preparation method thereof |
-
2007
- 2007-02-01 CN CNB2007100634524A patent/CN100571756C/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102451401A (en) * | 2010-11-01 | 2012-05-16 | 深圳市佳泰药业股份有限公司 | Prescription of vitamin C honeysuckle and forsythia |
| CN104873815A (en) * | 2015-05-27 | 2015-09-02 | 南京同仁堂药业有限责任公司 | Traditional Chinese medicine for treating common cold and preparing method of traditional Chinese medicine |
| CN106729140A (en) * | 2016-12-15 | 2017-05-31 | 贵州恒和制药有限公司 | A kind of compound preparation for treating influenza and preparation method thereof |
| CN106581174A (en) * | 2017-02-13 | 2017-04-26 | 佛山市腾瑞医药科技有限公司 | Traditional Chinese medicinal composition for treating wind-heat type common colds, and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN100571756C (en) | 2009-12-23 |
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