CN100344320C - Medicinal composition for treating children cold and its prepn. process - Google Patents
Medicinal composition for treating children cold and its prepn. process Download PDFInfo
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- CN100344320C CN100344320C CNB2006100757110A CN200610075711A CN100344320C CN 100344320 C CN100344320 C CN 100344320C CN B2006100757110 A CNB2006100757110 A CN B2006100757110A CN 200610075711 A CN200610075711 A CN 200610075711A CN 100344320 C CN100344320 C CN 100344320C
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Abstract
The present invention discloses a medicine composition, a preparation method thereof and a quality controlling method thereof. The medical composition is prepared from honeysuckle flower, forsythia fruit, isatis root, mint, bupleurum root, great burdock achene, schizonepeta spike, gypsum, baical skullcap root, gardenia, platycodon root, red peony root, reed root, bitter apricot seed, Herba Lophatheri, Fructus Aurantii, Massa Medicata Fermentata, stiff silkorm, ledebouriella root and liquorice. In the preparation method, volatile oil is extracted from the honeysuckle flower, the forsythia fruit, the schizonepeta spike, the mint, the Fructus Aurantii and the bupleurum root of the twenty raw medicinal materials, water solution obtained through distillation is collected in another container, water is added to decoct dregs of decoction and the other fourteen raw medicinal materials, decoction is combined and filtered, effective ingredients are extracted by ethanol, filtrate is concentrated into clear paste, conventional auxiliary materials are added, and an oral liquid preparation is made according to the conventional technique. The present invention also provides the application of the medical composition when the medical composition is used for preparing medicines used for treating infantile common cold.
Description
Technical field
The present invention relates to a kind of pharmaceutical composition and preparation method thereof and method of quality control, particularly a kind of pharmaceutical composition for the treatment of infantile common cold and preparation method thereof and method of quality control.
Background technology
It is department of pediatrics frequently-occurring disease and commonly encountered diseases clinically that cold, fever, acute simple tonsillitis or suppurative tonsillitis merge fever (diseases caused by exogenous pathogenic factor, newborn pretty young woman are suppurated and had heating concurrently).The medicine of generally acknowledging both at home and abroad is an antibiotic at present, domestic many with the penicillin intramuscular injection, and penicillin resistance is growing, the part infant can not be accepted the treatment of this medicine again because of allergy, it is also very painful that a lot of infants are accepted this medicine treatment, therefore, developing the Chinese patent medicine with heat clearing function is very important.
Summary of the invention
The object of the invention is to provide a kind of pharmaceutical composition and preparation method thereof and method of quality control, and another purpose of the present invention is to provide the purposes of this pharmaceutical composition.
The present invention seeks to be achieved through the following technical solutions:
The crude drug of pharmaceutical composition of the present invention consists of:
Flos Lonicerae 10-60 weight portion Fructus Forsythiae 10-60 weight portion Radix Isatidis 10-60 weight portion
Herba Menthae 5-30 weight portion Radix Bupleuri 10-60 weight portion Fructus Arctii 5-30 weight portion
Herba Schizonepetae 5-30 weight portion Gypsum Fibrosum 30-100 weight portion Radix Scutellariae 10-60 weight portion
Fructus Gardeniae 5-30 weight portion Radix Platycodonis 5-30 weight portion Radix Paeoniae Rubra 5-30 weight portion
Rhizoma Phragmitis 10-60 weight portion Semen Armeniacae Amarum 5-30 weight portion Herba Lophatheri 10-60 weight portion
Fructus Aurantii 5-30 weight portion Massa Medicata Fermentata 5-30 weight portion Bombyx Batryticatus 5-30 weight portion
Radix Saposhnikoviae 5-30 weight portion Radix Glycyrrhizae 5-30 weight portion.
The preferred weight proportioning of above-mentioned 20 flavor crude drug is as follows:
Flos Lonicerae 12 weight portion Fructus Forsythiaes 57 weight portion Radix Isatidis 15 weight portions
Herba Menthae 27 weight portion Radix Bupleuri 18 weight portion Fructus Arctiis 24 weight portions
Herba Schizonepetae 6 weight portion Gypsum Fibrosum 99 weight portion Radix Scutellariaes 20 weight portions
Fructus Gardeniae 21 weight portion Radix Platycodoniss 9 weight portion Radix Paeoniae Rubra 20 weight portions
Rhizoma Phragmitis 11 weight portion Semen Armeniacae Amarums 28 weight portion Herba Lophatheris 13 weight portions
Fructus Aurantii 29 weight portion Massa Medicata Fermentatas 10 weight portion Bombyx Batryticatus 25 weight portions
Radix Saposhnikoviae 8 weight portion Radix Glycyrrhizaes 22 weight portions.
The preferred weight proportioning of above-mentioned 20 flavor crude drug is as follows:
Flos Lonicerae 57 weight portion Fructus Forsythiaes 12 weight portion Radix Isatidis 50 weight portions
Herba Menthae 6 weight portion Radix Bupleuri 55 weight portion Fructus Arctiis 10 weight portions
Herba Schizonepetae 27 weight portion Gypsum Fibrosum 33 weight portion Radix Scutellariaes 54 weight portions
Fructus Gardeniae 9 weight portion Radix Platycodoniss 25 weight portion Radix Paeoniae Rubra 8 weight portions
Rhizoma Phragmitis 54 weight portion Semen Armeniacae Amarums 7 weight portion Herba Lophatheris 48 weight portions
Fructus Aurantii 11 weight portion Massa Medicata Fermentatas 24 weight portion Bombyx Batryticatus 6 weight portions
Radix Saposhnikoviae 29 weight portion Radix Glycyrrhizaes 6 weight portions.
The preferred weight proportioning of above-mentioned 20 flavor crude drug is as follows:
Flos Lonicerae 32 weight portion Fructus Forsythiaes 35 weight portion Radix Isatidis 37 weight portions
Herba Menthae 16 weight portion Radix Bupleuri 35 weight portion Fructus Arctiis 20 weight portions
Herba Schizonepetae 18 weight portion Gypsum Fibrosum 65 weight portion Radix Scutellariaes 30 weight portions
Fructus Gardeniae 18 weight portion Radix Platycodoniss 16 weight portion Radix Paeoniae Rubra 18 weight portions
Rhizoma Phragmitis 40 weight portion Semen Armeniacae Amarums 18 weight portion Herba Lophatheris 38 weight portions
Fructus Aurantii 18 weight portion Massa Medicata Fermentatas 15 weight portion Bombyx Batryticatus 18 weight portions
Radix Saposhnikoviae 18 weight portion Radix Glycyrrhizaes 12 weight portions.
Get the above-mentioned composition crude drug, add conventional adjuvant,, make clinical oral liquid, capsule, drop pill, granule, tablet, soft capsule, slow releasing agent or the lyophilized injectable powder accepted according to common process.
The concrete preparation technology of drug composition oral liquid preparation of the present invention is as follows:
Above-mentioned 20 flavor crude drug, extracting honeysuckle, Fructus Forsythiae, Herba Schizonepetae, Herba Menthae, Fructus Aurantii, Radix Bupleuri crude drug, vapor distillation extracts volatile oil, and the aqueous solution after distillation device is in addition collected; Get above-mentioned medicinal residues and all the other 14 flavor crude drug and decoct with water 1-3 time, each 1-2 hour, collecting decoction, filtration, filtrate is condensed into the clear paste that relative density is 1.10-1.20, and it is the clear paste of 1.10-1.20 that precipitate with ethanol, filtrate reconcentration become relative density; Aqueous solution after adding volatile oil and the distillation, fill, sterilization, promptly.
The preferred for preparation technology of drug composition oral liquid preparation of the present invention is as follows:
Above-mentioned 20 flavor crude drug, extracting honeysuckle, Fructus Forsythiae, Herba Schizonepetae, Herba Menthae, Fructus Aurantii, Radix Bupleuri crude drug, vapor distillation extracts volatile oil, and the aqueous solution after distillation device is in addition collected; Get above-mentioned medicinal residues and all the other 14 flavor crude drug and decoct with water 2 times, each 1.5 hours, collecting decoction filtered, and it is 1.15 clear paste that filtrate is condensed into relative density, and it is 1.15 clear paste that precipitate with ethanol, filtrate reconcentration become relative density; Aqueous solution after adding volatile oil and the distillation, fill, sterilization, promptly.
The method of quality control of pharmaceutical composition of the present invention comprises following discrimination method and/or content assaying method:
Discrimination method comprises one or more in the following method:
A, get oral liquid 50ml of the present invention, add hydrochloric acid 5ml, shake up, put in the hot bath heating 1 hour, filter with absorbent cotton, filtrate is with benzene extraction 2 times, each 20ml, and combined benzene extracting solution, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Fructus Arctii control medicinal material 1g, and water 50ml shakes up, and puts in the hot bath and heats 1 hour, filters with absorbent cotton, and filtrate is used benzene extraction 2 times, each 20ml, and combined benzene extracting solution, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, makes control medicinal material solution; Test according to thin layer chromatography, draw each 2-5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with 30-60 ℃ of petroleum ether-benzene-ethyl acetate-glacial acetic acid=7-13: 15-25: 5-9: 0.3-0.7 is developing solvent, launch, take out, dry, spray is with the acid 3-7% ferric chloride of hydrochloric acid alcoholic solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on show identical black-and-blue speckle;
B, get oral liquid 10ml of the present invention, add dehydrated alcohol, shake up to 100ml, placed 1 hour, and filtered the filtrate evaporate to dryness, residue adds water 15ml makes dissolving, uses ether extraction 2 times, each 10ml, discard ether solution, reuse ethyl acetate extraction 4 times, each 10-15ml, merge ethyl acetate extraction liquid, evaporate to dryness, residue makes dissolving with methanol 2ml, as need testing solution; Other gets the baicalin reference substance and adds methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, be developing solvent with 30-42% acetic acid, launch, take out, to dry, spray is with 1% ferric chloride alcoholic solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical green speckle;
C, the test of photograph thin layer chromatography, draw need testing solution 10 μ l under the assay item, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-acetonitrile-ammonia=2-6: 0.8-1.6: 1: 0.06-0.14 is developing solvent, launches after saturated 15 minutes, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ were dried by the fire 5 minutes; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
D, get oral liquid 30ml of the present invention, put water-bath and steam near and driedly be thick, residue adds ethanol 10ml makes dissolving, filters or centrifugal, and filtrate is as need testing solution; Other gets Fructus Forsythiae control medicinal material 3g and adds water 50ml, decocts 1 hour, filters, and filtrate is put water bath method, and residue adds ethanol 2ml makes dissolving, filters, and filtrate is medical material solution in contrast; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with chloroform-methanol=15-25: 1 is developing solvent, in temperature is 25 ℃-40 ℃, exhibition launches under the above condition of 13cm, takes out, and dries, spray is 15-25 with acetic anhydride-sulphuric acid: 1 solution, 105 ℃ of bakings 10 minutes, put coldly, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical yellow fluorescence speckle.
Content assaying method in the method for quality control is as follows:
Accurate absorption oral liquid 20ml of the present invention, put in the 100ml measuring bottle, add dehydrated alcohol and be diluted to scale, shake up, placed 20 minutes, supersound process 20 minutes, room temperature was placed 30 minutes, filtered, and discarded filtrate just, the accurate subsequent filtrate 75ml that draws, put evaporate to dryness in the water-bath, residue adds water 20ml dissolving and quantitatively is transferred in the separatory funnel, with 6 each 15-20ml of water saturated n-butanol extraction, merge n-butanol extracting liquid, put evaporate to dryness in the water-bath, residue adds 85% ethanol 5ml, makes dissolving, join 100-150 order neutral alumina and active carbon by 6g: on the pillar of 0.15g mixing, carry out eluting with 85% ethanol with elution speed per minute 3ml, collect eluent 200ml, put evaporate to dryness in the water-bath, residue adds dissolve with methanol and standardize solution in the 5ml measuring bottle, as need testing solution; Other gets the gardenoside reference substance, adds methanol and makes the solution that every 1ml contains 0.75mg, in contrast product solution; According to thin layer chromatography test, the accurate need testing solution 10 μ l that draw, reference substance solution 8 μ l, 4 μ l, respectively the cross point in same be the silica gel G F of binding agent preparation with 0.25% sodium carboxymethyl cellulose
254On the lamellae, with chloroform-methanol-acetonitrile-ammonia=2-6: 0.8-1.6: 1: 0.06-0.14 is developing solvent, saturated 15 minutes, launch, take out, dry, spray is with 5% sulphuric acid ethanol liquid, and it is clear to dry by the fire to the speckle colour developing at 105 ℃, and room temperature was placed after 2 hours, carry out single wavelength zigzag scanning, wavelength X according to the thin layer chromatography thin layer chromatography scanning
s=500nm records test sample trap integrated value and reference substance trap integrated value, calculates with the external standard two-point method, promptly; Contain gardenoside C in the oral liquid of the present invention
17H
240
11Every 1ml must not be less than 0.16mg.
Following experimental example and embodiment are used to further specify but are not limited to the present invention.
Experimental example 1 pharmacodynamic experiment
1, refrigeration function: oral liquid formulations of the present invention is to the rabbit fever models due to the Typhoid And Paratyphoid A, B Vaccine, antipyretic effect is arranged, compare with aspirin and GANMAO TUIRE CHONGJI, the refrigeration function of oral liquid of the present invention relaxes than aspirin, and is strong than GANMAO TUIRE CHONGJI.The oral liquid formulations of the present invention of various dose shows that to the influence of triple vaccine pyrogenicity rabbit body temperature with the increasing of dosage, its refrigeration function strengthens, and good linear relationship is arranged between the dose-effect.
Table 1 oral liquid formulations of the present invention is to the influence of the high fever of fever in rabbit
| The medicine name | Dosage g/kg | Laboratory animal is counted n | The highest intensification value ℃ X ± SD | P |
| Oral liquid GANMAO TUIRE CHONGJI aspirin matched group of the present invention (normal saline) | 71 24 0.30 10ml/kg | 8 8 8 8 | 1.20±0.32 1.48±0.48 1.10±0.26 1.69±0.28 | ＜0.01 ＞0.05 ＜0.01 |
Table 2 oral liquid formulations different time of the present invention is to the influence of fever in rabbit body temperature
| The medicine name | Dosage g/kg | Fervescence value ℃ X ± SD | ||||
| 1h | 2h | 3h | 4h | 5h | ||
| Oral liquid GANMAO TUIRE CHONGJI aspirin matched group of the present invention (normal saline) | 71 24 0.30 10ml/kg | 0.94±0.22 1.04±0.29 0.68±0.12 0.98±0.36 | 1.07±0.26 1.25±0.47 0.81±0.20** 1.32±0.39 | 1.20±0.32** 1.48±0.48 1.10±0.26** 1.69±0.23 | 0.82±0.56* 1.14±0.45 0.72±0.16** 1.44±0.58 | 0.27±0.42* 0.51±0.52 0.36±0.16* 0.81±0.52 |
Annotate: * P＜0.05; * P＜0.01
Table 3 various dose oral liquid formulations of the present invention is to the influence of the high fever of fever in rabbit
| The medicine name | Dosage g/kg | Laboratory animal is counted n | The highest intensification value ℃ X ± SD | P |
| Oral liquid of the present invention oral liquid of the present invention oral liquid matched group of the present invention (normal saline) | 14 43 71 10ml/kg | 8 8 8 8 | 1.53±0.45 1.36±0.29 1.20±0.32 1.69±0.23 | ＞0.05 ＜0.05 ＜0.01 |
2, antiinflammatory immunity function: oral liquid formulations of the present invention has good antiinflammatory action, can resist the acute and formaldehyde chronic animal inflammation of Ovum Gallus domesticus album, onset is very fast, low dose of (40g/kg) antiinflammatory action is similar to sodium salicylate, heavy dose of (80g/kg) antiinflammatory action is better than sodium salicylate, and antiinflammatory action to keep action time longer.Oral liquid of the present invention has the function that strengthens mononuclear phagocyte, improves immunologic function, helps in the inflammatory reaction removing to pathogenic microorganism.Oral liquid of the present invention can effectively suppress the mice local skin vascular permeability that anaphylactogen causes, has and resists allergic effect significantly, shows that oral liquid of the present invention can strengthen humoral immune function.
Table 4 oral liquid formulations of the present invention is to the arthritic effect of the impatient property of rat Ovum Gallus domesticus album
| Group | Dosage g/kg | Cause scorching posterior joint swelling degree (X ± SD, mm) | |||
| 1h | 2h | 4h | 6h | ||
| Matched group oral liquid of the present invention oral liquid salicylic acid of the present invention group | 40 80 0.5 | 7.47±0.51 5.72±0.47** 4.00±0.29** 4.88±0.32** | 6.22±0.29 4.68±0.37** 2.82±0.17** 3.58±0.27** | 5.03±0.15 4.00±0.15** 2.02±0.32** 2.32±0.22** | 4.37±0.44 3.25±0.24** 1.52±0.34** 1.72±0.24** |
Administration group and matched group be * * P＜0.01 relatively
Table 5 oral liquid formulations of the present invention is to the effect of rat formaldehyde chronic arthritis
| Group | Dosage g/kg | Cause scorching back ankle swelling degree (X ± SD, mm) | ||||||
| 1d | 2d | 3d | 4d | 5d | 6d | 7d | ||
| Control group oral liquid formulations of the present invention oral liquid formulations salicylic acid of the present invention group | 40 80 0.3 | 8.00± 0.44 6.73± 0.47** 5.23± 0.22** 6.58± 0.32** | 7.58± 0.47 5.50± 0.32** 4.42± 0.10** 5.17± 0.56** | 7.00± 0.47 4.62± 0.47** 3.77± 0.24** 4.77± 0.25** | 6.18± 0.17 4.10± 0.39** 3.55± 0.20** 4.22± 0.39** | 5.95± 0.37 3.72± 0.32** 2.75± 1.10** 3.60± 0.17** | 5.77± 0.39 343± 0.32** 2.92± 0.39** 3.38± 0.59** | 5.92± 0.49 3.33± 0.34** 2.35± 0.47** 3.00± 1.22** |
Administration group and matched group be * * P＜0.01 relatively
Table 6 oral liquid formulations of the present invention is to the influence of mononuclear phagocyte function
| Group | Dosage (g/kg) | K( X±SD) | α |
| Matched group oral liquid of the present invention oral liquid krestin of the present invention | - 40 80 0.1 | 0.11±0.022 0.015±0.004 0.018±0.004* 0.013±0.003* | 4.34±0.44 4.37±0.57 5.26±1.00* 5.28±0.65* |
*P＜0.01
Table 7 oral liquid formulations of the present invention is to the inhibitory action of mouse skin allergy reaction
| Group | Dosage (g/kg) | Optical density (0D) (X ± SD) | Suppression ratio (%) |
| Matched group oral liquid of the present invention oral liquid hydrochloric acid of the present invention benzene Hai Lamin | - 40 80 0.08 | 0.117±0.059 0.076±0.025 0.028±0.019* 0.028±0.015* | - 35.1 76.1 76.1 |
*P＜0.05
3, antiviral antibacterial action: show that with specific immunity fluorescence method result of the test oral liquid formulations of the present invention can significantly alleviate the pneumonia degree of influenza virus induced mice, and can suppress the proliferative amount of influenza virus in the Mus lung by specificity.External test tube method bacteriostatic test result shows: the oral liquid of the present invention pair antibacterial relevant with respiratory tract infection, staphylococcus aureus, Staphylococcus albus have stronger inhibitory action, minimum inhibitory concentration is 31.25mg/ml, effect to shigella flexneri is also stronger by force, effect to sonne bacillus and Candida albicans is inferior slightly, minimum inhibitory concentration is 62.5mg/ml, and is the most weak to colibacillary action intensity, and minimum inhibitory concentration is 250mg/ml.
Table 8 oral liquid formulations of the present invention is to the exponential effect of mice influenza infection lung
| Group | Dosage (g/kg/d) | Mus number (only) | The lung exponential quantity (M ± SD) | Suppression ratio (%) | P |
| Virus control papova azoles oral liquid of the present invention | 0.00 0.07 66.00 33.00 16.50 | 17 13 10 10 10 | 1.475±0.355 1.041±0.108 1.082±0.317 1.180±0.133 1.229±0.203 | 29.43 26.64 19.97 16.62 | ＜0.01 ＜0.01 ＜0.05 ＞0.05 |
Table 9 oral liquid formulations of the present invention is to the effect of proliferation of influenza virus amount in the mouse lung
| Group | Dosage (g/kg/d) | Specificity fluorescent ratio (%) | Suppression ratio (%) | P |
| Virus control papova azoles oral liquid of the present invention | 0.00 0.07 66.00 33.00 16.50 | 57.34 36.13 41.32 42.68 44.62 | 36.99 27.94 25.56 22.19 | ＜0.01 ＜0.01 ＜0.05 ＜0.05 |
Table 10 oral liquid formulations of the present invention is to the inhibitory action of common pathogen
| Liquor strength (mg/ml) | The gold Portugal | White Portugal | Large intestine | Bai Nian | Fu Shi | In Song |
| 250.00 125.00 62.50 31.25 15.65 | - - - - + | - - - - + | - + + + + | - - - + + | - - - - + | - - - + + |
Experimental example 2 clinical experiments
Select 400 routine infants, male's 221 examples, women's 179 examples, the age minimum is February, and maximum 14 years old, the course of disease is the shortest to be 2 hours, and the longest is 5 days.All infants all have heating, 38.5 ℃ of-39 ℃ of 256 examples wherein, and 39 ℃ of-40 ℃ of 140 examples are greater than 40 ℃ of 4 example.Total white blood cells＜1.0 ten thousand/mm
3183 examples, 1.0 ten thousand-1.5 ten thousand/mm
3164 examples,＞1.5 ten thousand/mm
351 examples.Throat swab antibacterial culturing person 218 examples, its streptococcus intermedius 7 examples, golden yellow staphylococcus 1 example, escherichia coli 1 example, para-influenza Bacillus 1 example, non-pathogenic bacteria 203 examples.Pharyngeal secretion thing virus is separated 261 examples, adenovirus 67 examples wherein, and influenza virus A type 1 example, influenza virus A, Type B 1 example are not isolated viral person's 192 examples.Medium-sized 296 examples of doctor trained in Western medicine typing, heavy 104 examples.Divide treatment group (oral liquid group of the present invention) 300 examples at random.Matched group (XIAOER QINGRE JIEDU KOUFUYE group) 100 examples.Two groups are all adopted oral administration, all do not use antibiotic and other antipyretic at viewing duration.
Table 11 liang 24,48,72 hours body temperature of group is reduced to normal comparison
| Time | The treatment group | Matched group | U | P | ||
| The example number | (％) | The example number | (％) | |||
| 24 hours 48 hours 72 hours | 118 117 32 | 39.33 39.00 10.67 | 21 44 16 | 21.00 44.00 16.00 | 3.333 0.893 1.42 | ＜0.01 ＜0.05 ＜0.05 |
Table 12 liang group body temperature is reduced to normal curative effect relatively
| Group | The example number | The routine number of bringing down a fever | (％) | Fever time X ± SD (h) | T | P |
| Treatment group matched group | 300 100 | 267 81 | 89.00 81.00 | 39.19±17.33 42.09±16.39 | 4.013 | ＜0.001 |
Clinical experiment is the result show: 24 hours extremely normal persons of endosome temperature drop of treatment group and matched group are respectively 118 examples (39.33%) and 21 examples (21.00%), the endosome temperature drop was respectively 267 examples (89.00%) and 81 examples (81.00%) to normal person in 72 hours, and fever time X ± SD (h) is respectively 39.19 ± 17.31 and 42.09 ± 16.39.Two groups at 24 hours endosome temperature drops all there were significant differences to normal required time to normal and 72 hours endosome temperature drops.Treatment group total effective rate is 89.00%, and recovery from illness+obvious effective rate 77.67%, matched group total effective rate are 73.00%, and cure rate+obvious effective rate is 52.00%, two group relatively significant difference, illustrates that the treatment group is better than matched group.
Following embodiment all can realize the described effect of above-mentioned experimental example.
The specific embodiment:
Embodiment 1: the preparation of tablet
Flos Lonicerae 12kg Fructus Forsythiae 57kg Radix Isatidis 15kg
Herba Menthae 27kg Radix Bupleuri 18kg Fructus Arctii 24kg
Herba Schizonepetae 6kg Gypsum Fibrosum 99kg Radix Scutellariae 20kg
Fructus Gardeniae 21kg Radix Platycodonis 9kg Radix Paeoniae Rubra 20kg
Rhizoma Phragmitis 11kg Semen Armeniacae Amarum 28kg Herba Lophatheri 13kg
Fructus Aurantii 29kg Massa Medicata Fermentata 10kg Bombyx Batryticatus 25kg
Radix Saposhnikoviae 8kg Radix Glycyrrhizae 22kg.
Above-mentioned 20 flavor crude drug, Flos Lonicerae, Fructus Forsythiae, Herba Schizonepetae, Herba Menthae, Fructus Aurantii, radix bupleuri extract volatile oil; Medicinal residues and all the other 14 flavor crude drug decoct with water 3 times, and collecting decoction filters, and filtrate is condensed into clear paste, precipitate with ethanol, and filtrate is condensed into clear paste; Add conventional adjuvant granulation, drying, add volatile oil, make tablet.
Embodiment 2: the preparation of capsule
Flos Lonicerae 57kg Fructus Forsythiae 12kg Radix Isatidis 50kg
Herba Menthae 6kg Radix Bupleuri 55kg Fructus Arctii 10kg
Herba Schizonepetae 27kg Gypsum Fibrosum 33kg Radix Scutellariae 54kg
Fructus Gardeniae 9kg Radix Platycodonis 25kg Radix Paeoniae Rubra 8kg
Rhizoma Phragmitis 54kg Semen Armeniacae Amarum 7kg Herba Lophatheri 48kg
Fructus Aurantii 11kg Massa Medicata Fermentata 24kg Bombyx Batryticatus 6kg
Radix Saposhnikoviae 29kg Radix Glycyrrhizae 6kg.
Above-mentioned 20 flavor crude drug, Flos Lonicerae, Fructus Forsythiae, Herba Schizonepetae, Herba Menthae, Fructus Aurantii, radix bupleuri extract volatile oil; Medicinal residues and all the other 14 flavor crude drug decoct with water 3 times, and collecting decoction filters, and filtrate is condensed into clear paste, precipitate with ethanol, and filtrate is condensed into clear paste; Add conventional adjuvant granulation, drying, add volatile oil, make capsule.
Embodiment 3: the preparation of granule
Flos Lonicerae 32kg Fructus Forsythiae 35kg Radix Isatidis 37kg
Herba Menthae 16kg Radix Bupleuri 35kg Fructus Arctii 20kg
Herba Schizonepetae 18kg Gypsum Fibrosum 65kg Radix Scutellariae 30kg
Fructus Gardeniae 18kg Radix Platycodonis 16kg Radix Paeoniae Rubra 18kg
Rhizoma Phragmitis 40kg Semen Armeniacae Amarum 18kg Herba Lophatheri 38kg
Fructus Aurantii 18kg Massa Medicata Fermentata 15kg Bombyx Batryticatus 18kg
Radix Saposhnikoviae 18kg Radix Glycyrrhizae 12kg.
Above-mentioned 20 flavor crude drug, Flos Lonicerae, Fructus Forsythiae, Herba Schizonepetae, Herba Menthae, Fructus Aurantii, radix bupleuri extract volatile oil; Medicinal residues and all the other 14 flavor crude drug decoct with water 3 times, and collecting decoction filters, and filtrate is condensed into clear paste, precipitate with ethanol, and filtrate is condensed into clear paste; Add conventional adjuvant granulation, drying, add volatile oil, make granule.
Embodiment 4: the preparation of oral liquid formulations
Flos Lonicerae 12g Fructus Forsythiae 57g Radix Isatidis 15g
Herba Menthae 27g Radix Bupleuri 18g Fructus Arctii 24g
Herba Schizonepetae 6g Gypsum Fibrosum 99g Radix Scutellariae 20g
Fructus Gardeniae 21g Radix Platycodonis 9g Radix Paeoniae Rubra 20g
Rhizoma Phragmitis 11g Semen Armeniacae Amarum 28g Herba Lophatheri 13g
Fructus Aurantii 29g Massa Medicata Fermentata 10g Bombyx Batryticatus 25g
Radix Saposhnikoviae 8g Radix Glycyrrhizae 22g.
Above-mentioned 20 flavor crude drug, Flos Lonicerae, Fructus Forsythiae, Herba Schizonepetae, Herba Menthae, Fructus Aurantii, radix bupleuri extract volatile oil, the aqueous solution after distillation device is in addition collected; Medicinal residues and all the other 14 flavor crude drug decoct with water 2 times, and collecting decoction filters, and filtrate is condensed into clear paste, precipitate with ethanol, and filtrate is condensed into clear paste; Aqueous solution after adding sweeting agent, volatile oil and the distillation is adjusted to 1000ml, fill, and sterilization, promptly.
Embodiment 5: the preparation of oral liquid formulations
Flos Lonicerae 32g Fructus Forsythiae 35g Radix Isatidis 37g
Herba Menthae 16g Radix Bupleuri 35g Fructus Arctii 20g
Herba Schizonepetae 18g Gypsum Fibrosum 65g Radix Scutellariae 30g
Fructus Gardeniae 18g Radix Platycodonis 16g Radix Paeoniae Rubra 18g
Rhizoma Phragmitis 40g Semen Armeniacae Amarum 18g Herba Lophatheri 38g
Fructus Aurantii 18g Massa Medicata Fermentata 15g Bombyx Batryticatus 18g
Radix Saposhnikoviae 18g Radix Glycyrrhizae 12g.
Above-mentioned 20 flavor crude drug, Flos Lonicerae, Fructus Forsythiae, Herba Schizonepetae, Herba Menthae, Fructus Aurantii, radix bupleuri extract volatile oil, the aqueous solution after distillation device is in addition collected; Medicinal residues and all the other 14 flavor crude drug decoct with water 3 times, and collecting decoction filters, and filtrate is condensed into clear paste, precipitate with ethanol, and filtrate is condensed into clear paste; Aqueous solution after adding sweeting agent, volatile oil and the distillation is adjusted to 1000ml, fill, and sterilization, promptly.
Embodiment 6: the method for quality control of oral liquid formulations
Discrimination method:
A, get embodiment 4 oral liquid 50ml, add hydrochloric acid 5ml, shake up, put in the hot bath heating 1 hour, filter with absorbent cotton, filtrate is with benzene extraction 2 times, each 20ml, and combined benzene extracting solution, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Fructus Arctii control medicinal material 1g, adds water 50ml, shakes up, and puts in the hot bath and heats 1 hour, filters with absorbent cotton, and filtrate is used benzene extraction 2 times, each 20ml, and combined benzene extracting solution, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, makes control medicinal material solution; Test according to thin layer chromatography, draw each 3 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with 45 ℃ of petroleum ether-benzene-ethyl acetate-glacial acetic acid=10: 20: 7: 0.5 was developing solvent, launch, take out, dry, spray is with the acid 5% ferric chloride alcoholic solution of hydrochloric acid, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on show identical black-and-blue speckle;
B, get embodiment 4 oral liquid 10ml, add dehydrated alcohol, shake up to 100ml, placed 1 hour, and filtered the filtrate evaporate to dryness, residue adds water 15ml makes dissolving, uses ether extraction 2 times, each 10ml, discard ether solution, reuse ethyl acetate extraction 4 times, for the first time 15ml, 10ml, 10ml, the 4th 10ml for the third time for the second time, merge ethyl acetate extraction liquid, evaporate to dryness, residue makes dissolving with methanol 2ml, as need testing solution; Other gets the baicalin reference substance and adds methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, be developing solvent with 36% acetic acid, launch, take out, to dry, spray is with 1% ferric chloride alcoholic solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical green speckle;
C, the test of photograph thin layer chromatography, draw need testing solution 10 μ l under the assay item, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-acetonitrile-ammonia=4: 1.2: 1: 0.1 was developing solvent, launches after saturated 15 minutes, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ were dried by the fire 5 minutes; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
D, get embodiment 4 oral liquid 30ml, put water-bath and steam near and driedly be thick, residue adds ethanol 10ml makes dissolving, filters or centrifugal, and filtrate is as need testing solution; Other gets Fructus Forsythiae control medicinal material 3g and adds water 50ml, decocts 1 hour, filters, and filtrate is put water bath method, and residue adds ethanol 2ml makes dissolving, filters, and filtrate is medical material solution in contrast; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, be developing solvent with chloroform-methanol=20: 1, in temperature is 32 ℃, exhibition launches under the above condition of 13cm, takes out, and dries, spray is 20: 1 solution with acetic anhydride-sulphuric acid, 105 ℃ of bakings 10 minutes, put coldly, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical yellow fluorescence speckle.
Embodiment 7: the method for quality control of oral liquid formulations
Content assaying method:
The accurate embodiment 5 oral liquid 20ml that draw, put in the 100ml measuring bottle, add dehydrated alcohol and be diluted to scale, shake up, placed 20 minutes, supersound process 20 minutes, room temperature was placed 30 minutes, filtered, and discarded filtrate just, the accurate subsequent filtrate 75ml that draws, put evaporate to dryness in the water-bath, residue adds water 20ml dissolving and quantitatively is transferred in the separatory funnel, with 6 each 15-20ml of water saturated n-butanol extraction, merge n-butanol extracting liquid, put evaporate to dryness in the water-bath, residue adds 85% ethanol 5ml, makes dissolving, join 100-150 order neutral alumina and active carbon by 6g: on the pillar of 0.15g mixing, carry out eluting with 85% ethanol with elution speed per minute 3ml, collect eluent 200ml, put evaporate to dryness in the water-bath, residue adds dissolve with methanol and standardize solution in the 5ml measuring bottle, as need testing solution; Other gets the gardenoside reference substance, adds methanol and makes the solution that every 1ml contains 0.75mg, in contrast product solution; According to thin layer chromatography test, the accurate need testing solution 10 μ l that draw, reference substance solution 8 μ l, 4 μ l, respectively the cross point in same be the silica gel G F of binding agent preparation with 0.25% sodium carboxymethyl cellulose
254On the lamellae, with chloroform-methanol-acetonitrile-ammonia=4: 1.2: 1: 0.1 was developing solvent, saturated 15 minutes, launch, take out, dry, spray is with 5% sulphuric acid ethanol liquid, and it is clear to dry by the fire to the speckle colour developing at 105 ℃, and room temperature was placed after 2 hours, carry out single wavelength zigzag scanning, wavelength X according to the thin layer chromatography thin layer chromatography scanning
s=500nm records test sample trap integrated value and reference substance trap integrated value, calculates with the external standard two-point method, promptly;
Contain gardenoside C in the oral liquid of the present invention
17H
24O
11Every 1ml must not be less than 0.16mg.
Embodiment 8: the method for quality control of oral liquid formulations
Content assaying method:
The accurate embodiment 5 oral liquid 20ml that draw, put in the 100ml measuring bottle, add dehydrated alcohol and be diluted to scale, shake up, placed 20 minutes, supersound process 20 minutes, room temperature was placed 30 minutes, filtered, and discarded filtrate just, the accurate subsequent filtrate 75ml that draws, put evaporate to dryness in the water-bath, residue adds water 20ml dissolving and quantitatively is transferred in the separatory funnel, with 6 each 13ml of water saturated n-butanol extraction, merge n-butanol extracting liquid, put evaporate to dryness in the water-bath, residue adds 85% ethanol 5ml, makes dissolving, join 100-150 order neutral alumina and active carbon by 6g: on the pillar of 0.15g mixing, carry out eluting with 85% ethanol with elution speed per minute 3ml, collect eluent 200ml, put evaporate to dryness in the water-bath, residue adds dissolve with methanol and standardize solution in the 5ml measuring bottle, as need testing solution; Other gets the gardenoside reference substance, adds methanol and makes the solution that every 1ml contains 0.75mg, in contrast product solution; According to thin layer chromatography test, the accurate need testing solution 10 μ l that draw, reference substance solution 8 μ l, 4 μ l, respectively the cross point in same be the silica gel G F of binding agent preparation with 0.25% sodium carboxymethyl cellulose
254On the lamellae, with chloroform-methanol-acetonitrile-ammonia=5: 0.9: 1: 0.07 was developing solvent, saturated 15 minutes, launch, take out, dry, spray is with 5% sulphuric acid ethanol liquid, and it is clear to dry by the fire to the speckle colour developing at 105 ℃, and room temperature was placed after 2 hours, carry out single wavelength zigzag scanning, wavelength X according to the thin layer chromatography thin layer chromatography scanning
s=500nm records test sample trap integrated value and reference substance trap integrated value, calculates with the external standard two-point method, promptly;
Contain gardenoside C in the oral liquid of the present invention
17H
24O
11Every 1ml must not be less than 0.16mg.
Embodiment 9: the method for quality control of oral liquid formulations
Discrimination method:
A, get embodiment 5 oral liquid 50ml, add hydrochloric acid 5ml, shake up, put in the hot bath heating 1 hour, filter with absorbent cotton, filtrate is with benzene extraction 2 times, each 20ml, and combined benzene extracting solution, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Fructus Arctii control medicinal material 1g, adds water 50ml, shakes up, and puts in the hot bath and heats 1 hour, filters with absorbent cotton, and filtrate is used benzene extraction 2 times, each 20ml, and combined benzene extracting solution, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, makes control medicinal material solution; Test according to thin layer chromatography, draw each 3 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with 45 ℃ of petroleum ether-benzene-ethyl acetate-glacial acetic acid=8: 24: 6: 0.6 was developing solvent, launch, take out, dry, spray is with the acid 4% ferric chloride alcoholic solution of hydrochloric acid, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on show identical black-and-blue speckle;
B, get embodiment 5 oral liquid 10ml, add dehydrated alcohol, shake up to 100ml, placed 1 hour, and filtered the filtrate evaporate to dryness, residue adds water 15ml makes dissolving, uses ether extraction 2 times, each 10ml, discard ether solution, reuse ethyl acetate extraction 4 times, for the first time 13ml, 13ml, 12ml, the 4th 10ml for the third time for the second time, merge ethyl acetate extraction liquid, evaporate to dryness, residue makes dissolving with methanol 2ml, as need testing solution; Other gets the baicalin reference substance and adds methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, be developing solvent with 31% acetic acid, launch, take out, to dry, spray is with 1% ferric chloride alcoholic solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical green speckle;
C, the test of photograph thin layer chromatography, draw need testing solution 10 μ l under the assay item, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-acetonitrile-ammonia=3: 1.5: 1: 0.07 was developing solvent, launches after saturated 15 minutes, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ were dried by the fire 5 minutes; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Embodiment 10: the method for quality control of oral liquid formulations
Discrimination method:
B, get embodiment 4 oral liquid 10ml, add dehydrated alcohol, shake up to 100ml, placed 1 hour, and filtered the filtrate evaporate to dryness, residue adds water 15ml makes dissolving, uses ether extraction 2 times, each 10ml, discard ether solution, reuse ethyl acetate extraction 4 times, for the first time 11ml, 11ml, 14ml, the 4th 15ml for the third time for the second time, merge ethyl acetate extraction liquid, evaporate to dryness, residue makes dissolving with methanol 2ml, as need testing solution; Other gets the baicalin reference substance and adds methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, be developing solvent with 41% acetic acid, launch, take out, to dry, spray is with 1% ferric chloride alcoholic solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical green speckle;
C, the test of photograph thin layer chromatography, draw need testing solution 10 μ l under the assay item, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-acetonitrile-ammonia=5: 0.9: 1: 0.13 was developing solvent, launches after saturated 15 minutes, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ were dried by the fire 5 minutes; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
D, get embodiment 4 oral liquid 30ml, put water-bath and steam near and driedly be thick, residue adds ethanol 10ml makes dissolving, filters or centrifugal, and filtrate is as need testing solution; Other gets Fructus Forsythiae control medicinal material 3g and adds water 50ml, decocts 1 hour, filters, and filtrate is put water bath method, and residue adds ethanol 2ml makes dissolving, filters, and filtrate is medical material solution in contrast; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, be developing solvent with chloroform-methanol=24: 1, in temperature is 32 ℃, exhibition launches under the above condition of 13cm, takes out, and dries, spray is 16: 1 solution with acetic anhydride-sulphuric acid, 105 ℃ of bakings 10 minutes, put coldly, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical yellow fluorescence speckle.
Embodiment 11: the method for quality control of oral liquid formulations
Discrimination method:
A, get embodiment 4 oral liquid 50ml, add hydrochloric acid 5ml, shake up, put in the hot bath heating 1 hour, filter with absorbent cotton, filtrate is with benzene extraction 2 times, each 20ml, and combined benzene extracting solution, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Fructus Arctii control medicinal material 1g, adds water 50ml, shakes up, and puts in the hot bath and heats 1 hour, filters with absorbent cotton, and filtrate is used benzene extraction 2 times, each 20ml, and combined benzene extracting solution, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, makes control medicinal material solution; Test according to thin layer chromatography, draw each 3 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with 45 ℃ of petroleum ether-benzene-ethyl acetate-glacial acetic acid=10: 20: 7: 0.5 was developing solvent, launch, take out, dry, spray is with the acid 5% ferric chloride alcoholic solution of hydrochloric acid, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on show identical black-and-blue speckle;
B, get embodiment 4 oral liquid 10ml, add dehydrated alcohol, shake up to 100ml, placed 1 hour, and filtered the filtrate evaporate to dryness, residue adds water 15ml makes dissolving, uses ether extraction 2 times, each 10ml, discard ether solution, reuse ethyl acetate extraction 4 times, for the first time 15ml, 10ml, 10ml, the 4th 10ml for the third time for the second time, merge ethyl acetate extraction liquid, evaporate to dryness, residue makes dissolving with methanol 2ml, as need testing solution; Other gets the baicalin reference substance and adds methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, be developing solvent with 36% acetic acid, launch, take out, to dry, spray is with 1% ferric chloride alcoholic solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical green speckle;
C, the test of photograph thin layer chromatography, draw need testing solution 10 μ l under the assay item, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-acetonitrile-ammonia=4: 1.2: 1: 0.1 was developing solvent, launches after saturated 15 minutes, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ were dried by the fire 5 minutes; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
D, get embodiment 4 oral liquid 30ml, put water-bath and steam near and driedly be thick, residue adds ethanol 10ml makes dissolving, filters or centrifugal, and filtrate is as need testing solution; Other gets Fructus Forsythiae control medicinal material 3g and adds water 50ml, decocts 1 hour, filters, and filtrate is put water bath method, and residue adds ethanol 2ml makes dissolving, filters, and filtrate is medical material solution in contrast; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, be developing solvent with chloroform-methanol=20: 1, in temperature is 32 ℃, exhibition launches under the above condition of 13cm, takes out, and dries, spray is 20: 1 solution with acetic anhydride-sulphuric acid, 105 ℃ of bakings 10 minutes, put coldly, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical yellow fluorescence speckle.
Content assaying method:
The accurate embodiment 4 oral liquid 20ml that draw, put in the 100ml measuring bottle, add dehydrated alcohol and be diluted to scale, shake up, placed 20 minutes, supersound process 20 minutes, room temperature was placed 30 minutes, filtered, and discarded filtrate just, the accurate subsequent filtrate 75ml that draws, put evaporate to dryness in the water-bath, residue adds water 20ml dissolving and quantitatively is transferred in the separatory funnel, with 6 each 11ml of water saturated n-butanol extraction, merge n-butanol extracting liquid, put evaporate to dryness in the water-bath, residue adds 85% ethanol 5ml, makes dissolving, join 100-150 order neutral alumina and active carbon by 6g: on the pillar of 0.15g mixing, carry out eluting with 85% ethanol with elution speed per minute 3ml, collect eluent 200ml, put evaporate to dryness in the water-bath, residue adds dissolve with methanol and standardize solution in the 5ml measuring bottle, as need testing solution; Other gets the gardenoside reference substance, adds methanol and makes the solution that every 1ml contains 0.75mg, in contrast product solution; According to thin layer chromatography test, the accurate need testing solution 10 μ l that draw, reference substance solution 8 μ l, 4 μ l, respectively the cross point in same be the silica gel G F of binding agent preparation with 0.25% sodium carboxymethyl cellulose
254On the lamellae, with chloroform-methanol-acetonitrile-ammonia=3: 1.5: 1: 0.07 was developing solvent, saturated 15 minutes, launch, take out, dry, spray is with 5% sulphuric acid ethanol liquid, and it is clear to dry by the fire to the speckle colour developing at 105 ℃, and room temperature was placed after 2 hours, carry out single wavelength zigzag scanning, wavelength X according to the thin layer chromatography thin layer chromatography scanning
s=500nm records test sample trap integrated value and reference substance trap integrated value, calculates with the external standard two-point method, promptly;
Contain gardenoside C in the oral liquid of the present invention
17H
24O
11Every 1ml must not be less than 0.16mg.
Claims (12)
1, a kind of pharmaceutical composition for the treatment of infantile common cold is characterized in that the crude drug of this pharmaceutical composition consists of:
Flos Lonicerae 10-60 weight portion Fructus Forsythiae 10-60 weight portion Radix Isatidis 10-60 weight portion
Herba Menthae 5-30 weight portion Radix Bupleuri 10-60 weight portion Fructus Arctii 5-30 weight portion
Herba Schizonepetae 5-30 weight portion Gypsum Fibrosum 30-100 weight portion Radix Scutellariae 10-60 weight portion
Fructus Gardeniae 5-30 weight portion Radix Platycodonis 5-30 weight portion Radix Paeoniae Rubra 5-30 weight portion
Rhizoma Phragmitis 10-60 weight portion Semen Armeniacae Amarum 5-30 weight portion Herba Lophatheri 10-60 weight portion
Fructus Aurantii 5-30 weight portion Massa Medicata Fermentata 5-30 weight portion Bombyx Batryticatus 5-30 weight portion
Radix Saposhnikoviae 5-30 weight portion Radix Glycyrrhizae 5-30 weight portion.
2, pharmaceutical composition as claimed in claim 1 is characterized in that the crude drug of this pharmaceutical composition consists of:
Flos Lonicerae 12 weight portion Fructus Forsythiaes 57 weight portion Radix Isatidis 15 weight portions
Herba Menthae 27 weight portion Radix Bupleuri 18 weight portion Fructus Arctiis 24 weight portions
Herba Schizonepetae 6 weight portion Gypsum Fibrosum 99 weight portion Radix Scutellariaes 20 weight portions
Fructus Gardeniae 21 weight portion Radix Platycodoniss 9 weight portion Radix Paeoniae Rubra 20 weight portions
Rhizoma Phragmitis 11 weight portion Semen Armeniacae Amarums 28 weight portion Herba Lophatheris 13 weight portions
Fructus Aurantii 29 weight portion Massa Medicata Fermentatas 10 weight portion Bombyx Batryticatus 25 weight portions
Radix Saposhnikoviae 8 weight portion Radix Glycyrrhizaes 22 weight portions.
3, pharmaceutical composition as claimed in claim 1 is characterized in that the crude drug of this pharmaceutical composition consists of:
Flos Lonicerae 57 weight portion Fructus Forsythiaes 12 weight portion Radix Isatidis 50 weight portions
Herba Menthae 6 weight portion Radix Bupleuri 55 weight portion Fructus Arctiis 10 weight portions
Herba Schizonepetae 27 weight portion Gypsum Fibrosum 33 weight portion Radix Scutellariaes 54 weight portions
Fructus Gardeniae 9 weight portion Radix Platycodoniss 25 weight portion Radix Paeoniae Rubra 8 weight portions
Rhizoma Phragmitis 54 weight portion Semen Armeniacae Amarums 7 weight portion Herba Lophatheris 48 weight portions
Fructus Aurantii 11 weight portion Massa Medicata Fermentatas 24 weight portion Bombyx Batryticatus 6 weight portions
Radix Saposhnikoviae 29 weight portion Radix Glycyrrhizaes 6 weight portions.
4, pharmaceutical composition as claimed in claim 1 is characterized in that the crude drug of this pharmaceutical composition consists of:
Flos Lonicerae 32 weight portion Fructus Forsythiaes 35 weight portion Radix Isatidis 37 weight portions
Herba Menthae 16 weight portion Radix Bupleuri 35 weight portion Fructus Arctiis 20 weight portions
Herba Schizonepetae 18 weight portion Gypsum Fibrosum 65 weight portion Radix Scutellariaes 30 weight portions
Fructus Gardeniae 18 weight portion Radix Platycodoniss 16 weight portion Radix Paeoniae Rubra 18 weight portions
Rhizoma Phragmitis 40 weight portion Semen Armeniacae Amarums 18 weight portion Herba Lophatheris 38 weight portions
Fructus Aurantii 18 weight portion Massa Medicata Fermentatas 15 weight portion Bombyx Batryticatus 18 weight portions
Radix Saposhnikoviae 18 weight portion Radix Glycyrrhizaes 12 weight portions.
5, as claim 1,2,3 or 4 described pharmaceutical compositions, it is characterized in that getting this pharmaceutical composition crude drug, add conventional adjuvant,, make oral liquid, capsule, drop pill, granule, tablet, soft capsule, slow releasing agent or lyophilized injectable powder according to common process.
6, as claim 1,2,3 or 4 described preparation of drug combination methods, the preparation method that it is characterized in that oral liquid is: extracting honeysuckle, Fructus Forsythiae, Herba Schizonepetae, Herba Menthae, Fructus Aurantii, Radix Bupleuri crude drug, vapor distillation extracts volatile oil, and the aqueous solution after distillation device is in addition collected; Get above-mentioned medicinal residues and all the other 14 flavor crude drug and decoct with water 1-3 time, each 1-2 hour, collecting decoction, filtration, filtrate is condensed into the clear paste that relative density is 1.10-1.20, and it is the clear paste of 1.10-1.20 that precipitate with ethanol, filtrate reconcentration become relative density; Aqueous solution after adding volatile oil and the distillation, fill, sterilization, promptly.
7, as claim 1,2,3 or 4 described preparation of drug combination methods, the preparation method that it is characterized in that oral liquid is: extracting honeysuckle, Fructus Forsythiae, Herba Schizonepetae, Herba Menthae, Fructus Aurantii, Radix Bupleuri crude drug, vapor distillation extracts volatile oil, and the aqueous solution after distillation device is in addition collected; Get above-mentioned medicinal residues and all the other 14 flavor crude drug and decoct with water 2 times, each 1.5 hours, collecting decoction filtered, and it is 1.15 clear paste that filtrate is condensed into relative density, and it is 1.15 clear paste that precipitate with ethanol, filtrate reconcentration become relative density; Aqueous solution after adding volatile oil and the distillation, fill, sterilization, promptly.
8, the method for quality control of pharmaceutical composition as claimed in claim 5 is characterized in that this method comprises following discriminating and/or assay:
Differentiate: A, get oral liquid 50ml, add hydrochloric acid 5ml, shake up, put in the hot bath heating 1 hour, filter with absorbent cotton, filtrate is with benzene extraction 2 times, each 20ml, and combined benzene extracting solution, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Fructus Arctii control medicinal material 1g, adds water 50ml, shakes up, and puts in the hot bath and heats 1 hour, filters with absorbent cotton, and filtrate is used benzene extraction 2 times, each 20ml, and combined benzene extracting solution, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, makes control medicinal material solution; Test according to thin layer chromatography, draw each 2-5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with 30-60 ℃ of petroleum ether-benzene-ethyl acetate-glacial acetic acid=7-13: 15-25: 5-9: 0.3-0.7 is developing solvent, launch, take out, dry, spray is with the acid 3-7% ferric chloride of hydrochloric acid alcoholic solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on show identical black-and-blue speckle;
B, get oral liquid 10ml, add dehydrated alcohol, shake up to 100ml, placed 1 hour, and filtered the filtrate evaporate to dryness, residue adds water 15ml makes dissolving, uses ether extraction 2 times, each 10ml, discard ether solution, reuse ethyl acetate extraction 4 times, each 10-15ml, merge ethyl acetate extraction liquid, evaporate to dryness, residue makes dissolving with methanol 2ml, as need testing solution; Other gets the baicalin reference substance and adds methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, be developing solvent with 30-42% acetic acid, launch, take out, to dry, spray is with 1% ferric chloride alcoholic solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical green speckle;
C, the test of photograph thin layer chromatography, draw need testing solution 10 μ l under the assay item, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-acetonitrile-ammonia=2-6: 0.8-1.6: 1: 0.06-0.14 is developing solvent, launches after saturated 15 minutes, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ were dried by the fire 5 minutes; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
D, get oral liquid 30ml, put water-bath and steam near and driedly be thick, residue adds ethanol 10ml makes dissolving, filters or centrifugal, and filtrate is as need testing solution; Other gets Fructus Forsythiae control medicinal material 3g and adds water 50ml, decocts 1 hour, filters, and filtrate is put water bath method, and residue adds ethanol 2ml makes dissolving, filters, and filtrate is medical material solution in contrast; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with chloroform-methanol=15-25: 1 is developing solvent, in temperature is 25 ℃-40 ℃, exhibition launches under the above condition of 13cm, takes out, and dries, spray is 15-25 with acetic anhydride-sulphuric acid: 1 solution, 105 ℃ of bakings 10 minutes, put coldly, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical yellow fluorescence speckle;
Assay: the accurate oral liquid 20ml that draws, put in the 100ml measuring bottle, add dehydrated alcohol and be diluted to scale, shake up, placed 20 minutes, supersound process 20 minutes, room temperature was placed 30 minutes, filtered, and discarded filtrate just, the accurate subsequent filtrate 75ml that draws, put evaporate to dryness in the water-bath, residue adds water 20ml dissolving and quantitatively is transferred in the separatory funnel, with 6 each 15-20ml of water saturated n-butanol extraction, merge n-butanol extracting liquid, put evaporate to dryness in the water-bath, residue adds 85% ethanol 5ml, makes dissolving, join 100-150 order neutral alumina and active carbon by 6g: on the pillar of 0.15g mixing, carry out eluting with 85% ethanol with elution speed per minute 3ml, collect eluent 200ml, put evaporate to dryness in the water-bath, residue adds dissolve with methanol and standardize solution in the 5ml measuring bottle, as need testing solution; Other gets the gardenoside reference substance, adds methanol and makes the solution that every 1ml contains 0.75mg, in contrast product solution; According to thin layer chromatography test, the accurate need testing solution 10 μ l that draw, reference substance solution 8 μ l, 4 μ l, respectively the cross point in same be the silica gel G F of binding agent preparation with 0.25% sodium carboxymethyl cellulose
254On the lamellae, with chloroform-methanol-acetonitrile-ammonia=2-6: 0.8-1.6: 1: 0.06-0.14 is developing solvent, saturated 15 minutes, launch, take out, dry, spray is with 5% sulphuric acid ethanol liquid, and it is clear to dry by the fire to the speckle colour developing at 105 ℃, and room temperature was placed after 2 hours, carry out single wavelength zigzag scanning, wavelength X according to the thin layer chromatography thin layer chromatography scanning
S=500nm records test sample trap integrated value and reference substance trap integrated value, calculates with the external standard two-point method, promptly; Contain gardenoside C in the oral liquid
17H
24O
11Every 1ml must not be less than 0.16mg.
9, the method for quality control of pharmaceutical composition as claimed in claim 6 is characterized in that this method comprises following discriminating and/or assay:
Differentiate: A, get oral liquid 50ml, add hydrochloric acid 5ml, shake up, put in the hot bath heating 1 hour, filter with absorbent cotton, filtrate is with benzene extraction 2 times, each 20ml, and combined benzene extracting solution, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Fructus Arctii control medicinal material 1g, adds water 50ml, shakes up, and puts in the hot bath and heats 1 hour, filters with absorbent cotton, and filtrate is used benzene extraction 2 times, each 20ml, and combined benzene extracting solution, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, makes control medicinal material solution; Test according to thin layer chromatography, draw each 2-5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with 30-60 ℃ of petroleum ether-benzene-ethyl acetate-glacial acetic acid=7-13: 15-25: 5-9: 0.3-0.7 is developing solvent, launch, take out, dry, spray is with the acid 3-7% ferric chloride of hydrochloric acid alcoholic solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on show identical black-and-blue speckle;
B, get oral liquid 10ml, add dehydrated alcohol, shake up to 100ml, placed 1 hour, and filtered the filtrate evaporate to dryness, residue adds water 15ml makes dissolving, uses ether extraction 2 times, each 10ml, discard ether solution, reuse ethyl acetate extraction 4 times, each 10-15ml, merge ethyl acetate extraction liquid, evaporate to dryness, residue makes dissolving with methanol 2ml, as need testing solution; Other gets the baicalin reference substance and adds methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, be developing solvent with 30-42% acetic acid, launch, take out, to dry, spray is with 1% ferric chloride alcoholic solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical green speckle;
C, the test of photograph thin layer chromatography, draw need testing solution 10 μ l under the assay item, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-acetonitrile-ammonia=2-6: 0.8-1.6: 1: 0.06-0.14 is developing solvent, launches after saturated 15 minutes, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ were dried by the fire 5 minutes; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
D, get oral liquid 30ml, put water-bath and steam near and driedly be thick, residue adds ethanol 10ml makes dissolving, filters or centrifugal, and filtrate is as need testing solution; Other gets Fructus Forsythiae control medicinal material 3g and adds water 50ml, decocts 1 hour, filters, and filtrate is put water bath method, and residue adds ethanol 2ml makes dissolving, filters, and filtrate is medical material solution in contrast; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with chloroform-methanol=15-25: 1 is developing solvent, in temperature is 25 ℃-40 ℃, exhibition launches under the above condition of 13cm, takes out, and dries, spray is 15-25 with acetic anhydride-sulphuric acid: 1 solution, 105 ℃ of bakings 10 minutes, put coldly, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical yellow fluorescence speckle;
Assay: the accurate oral liquid 20ml that draws, put in the 100ml measuring bottle, add dehydrated alcohol and be diluted to scale, shake up, placed 20 minutes, supersound process 20 minutes, room temperature was placed 30 minutes, filtered, and discarded filtrate just, the accurate subsequent filtrate 75ml that draws, put evaporate to dryness in the water-bath, residue adds water 20ml dissolving and quantitatively is transferred in the separatory funnel, with 6 each 15-20ml of water saturated n-butanol extraction, merge n-butanol extracting liquid, put evaporate to dryness in the water-bath, residue adds 85% ethanol 5ml, makes dissolving, join 100-150 order neutral alumina and active carbon by 6g: on the pillar of 0.15g mixing, carry out eluting with 85% ethanol with elution speed per minute 3ml, collect eluent 200ml, put evaporate to dryness in the water-bath, residue adds dissolve with methanol and standardize solution in the 5ml measuring bottle, as need testing solution; Other gets the gardenoside reference substance, adds methanol and makes the solution that every 1ml contains 0.75mg, in contrast product solution; According to thin layer chromatography test, the accurate need testing solution 10 μ l that draw, reference substance solution 8 μ l, 4 μ l, respectively the cross point in same be the silica gel G F of binding agent preparation with 0.25% sodium carboxymethyl cellulose
254On the lamellae, with chloroform-methanol-acetonitrile-ammonia=2-6: 0.8-1.6: 1: 0.06-0.14 is developing solvent, saturated 15 minutes, launch, take out, dry, spray is with 5% sulphuric acid ethanol liquid, and it is clear to dry by the fire to the speckle colour developing at 105 ℃, and room temperature was placed after 2 hours, carry out single wavelength zigzag scanning, wavelength X according to the thin layer chromatography thin layer chromatography scanning
S=500nm records test sample trap integrated value and reference substance trap integrated value, calculates with the external standard two-point method, promptly; Contain gardenoside C in the oral liquid
17H
24O
11Every 1ml must not be less than 0.16mg.
10, the method for quality control of pharmaceutical composition as claimed in claim 7 is characterized in that this method comprises following discriminating and/or assay:
Differentiate: A, get oral liquid 50ml, add hydrochloric acid 5ml, shake up, put in the hot bath heating 1 hour, filter with absorbent cotton, filtrate is with benzene extraction 2 times, each 20ml, and combined benzene extracting solution, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Fructus Arctii control medicinal material 1g, adds water 50ml, shakes up, and puts in the hot bath and heats 1 hour, filters with absorbent cotton, and filtrate is used benzene extraction 2 times, each 20ml, and combined benzene extracting solution, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, makes control medicinal material solution; Test according to thin layer chromatography, draw each 2-5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with 30-60 ℃ of petroleum ether-benzene-ethyl acetate-glacial acetic acid=7-13: 15-25: 5-9: 0.3-0.7 is developing solvent, launch, take out, dry, spray is with the acid 3-7% ferric chloride of hydrochloric acid alcoholic solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on show identical black-and-blue speckle;
B, get oral liquid 10ml, add dehydrated alcohol, shake up to 100ml, placed 1 hour, and filtered the filtrate evaporate to dryness, residue adds water 15ml makes dissolving, uses ether extraction 2 times, each 10ml, discard ether solution, reuse ethyl acetate extraction 4 times, each 10-15ml, merge ethyl acetate extraction liquid, evaporate to dryness, residue makes dissolving with methanol 2ml, as need testing solution; Other gets the baicalin reference substance and adds methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, be developing solvent with 30-42% acetic acid, launch, take out, to dry, spray is with 1% ferric chloride alcoholic solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical green speckle;
C, the test of photograph thin layer chromatography, draw need testing solution 10 μ l under the assay item, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-acetonitrile-ammonia=2-6: 0.8-1.6: 1: 0.06-0.14 is developing solvent, launches after saturated 15 minutes, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ were dried by the fire 5 minutes; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
D, get oral liquid 30ml, put water-bath and steam near and driedly be thick, residue adds ethanol 10ml makes dissolving, filters or centrifugal, and filtrate is as need testing solution; Other gets Fructus Forsythiae control medicinal material 3g and adds water 50ml, decocts 1 hour, filters, and filtrate is put water bath method, and residue adds ethanol 2ml makes dissolving, filters, and filtrate is medical material solution in contrast; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with chloroform-methanol=15-25: 1 is developing solvent, in temperature is 25 ℃-40 ℃, exhibition launches under the above condition of 13cm, takes out, and dries, spray is 15-25 with acetic anhydride-sulphuric acid: 1 solution, 105 ℃ of bakings 10 minutes, put coldly, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical yellow fluorescence speckle;
Assay: the accurate oral liquid 20ml that draws, put in the 100ml measuring bottle, add dehydrated alcohol and be diluted to scale, shake up, placed 20 minutes, supersound process 20 minutes, room temperature was placed 30 minutes, filtered, and discarded filtrate just, the accurate subsequent filtrate 75ml that draws, put evaporate to dryness in the water-bath, residue adds water 20ml dissolving and quantitatively is transferred in the separatory funnel, with 6 each 15-20ml of water saturated n-butanol extraction, merge n-butanol extracting liquid, put evaporate to dryness in the water-bath, residue adds 85% ethanol 5ml, makes dissolving, join 100-150 order neutral alumina and active carbon by 6g: on the pillar of 0.15g mixing, carry out eluting with 85% ethanol with elution speed per minute 3ml, collect eluent 200ml, put evaporate to dryness in the water-bath, residue adds dissolve with methanol and standardize solution in the 5ml measuring bottle, as need testing solution; Other gets the gardenoside reference substance, adds methanol and makes the solution that every 1ml contains 0.75mg, in contrast product solution; According to thin layer chromatography test, the accurate need testing solution 10 μ l that draw, reference substance solution 8 μ l, 4 μ l, respectively the cross point in same be the silica gel G F of binding agent preparation with 0.25% sodium carboxymethyl cellulose
254On the lamellae, with chloroform-methanol-acetonitrile-ammonia=2-6: 0.8-1.6: 1: 0.06-0.14 is developing solvent, saturated 15 minutes, launch, take out, dry, spray is with 5% sulphuric acid ethanol liquid, and it is clear to dry by the fire to the speckle colour developing at 105 ℃, and room temperature was placed after 2 hours, carry out single wavelength zigzag scanning, wavelength X according to the thin layer chromatography thin layer chromatography scanning
S=500nm records test sample trap integrated value and reference substance trap integrated value, calculates with the external standard two-point method, promptly; Contain gardenoside C in the oral liquid
17H
24O
11Every 1ml must not be less than 0.16mg.
11,, it is characterized in that this method comprises following discriminating and/or assay as the method for quality control of claim 8,9 or 10 described pharmaceutical compositions:
Discrimination method: A, get oral liquid 50ml, add hydrochloric acid 5ml, shake up, put in the hot bath heating 1 hour, filter with absorbent cotton, filtrate is used benzene extraction 2 times, each 20ml, combined benzene extracting solution, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Fructus Arctii control medicinal material 1g, adds water 50ml, shakes up, and puts in the hot bath and heats 1 hour, filters with absorbent cotton, and filtrate is used benzene extraction 2 times, each 20ml, and combined benzene extracting solution, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, makes control medicinal material solution; Test according to thin layer chromatography, draw each 3 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with 45 ℃ of petroleum ether-benzene-ethyl acetate-glacial acetic acid=10: 20: 7: 0.5 was developing solvent, launch, take out, dry, spray is with the acid 5% ferric chloride alcoholic solution of hydrochloric acid, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on show identical black-and-blue speckle;
B, get oral liquid 10ml, add dehydrated alcohol, shake up to 100ml, placed 1 hour, and filtered the filtrate evaporate to dryness, residue adds water 15ml makes dissolving, uses ether extraction 2 times, each 10ml, discard ether solution, reuse ethyl acetate extraction 4 times, for the first time 15ml, 10ml, 10ml, the 4th 10ml for the third time for the second time, merge ethyl acetate extraction liquid, evaporate to dryness, residue makes dissolving with methanol 2ml, as need testing solution; Other gets the baicalin reference substance and adds methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, be developing solvent with 36% acetic acid, launch, take out, to dry, spray is with 1% ferric chloride alcoholic solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical green speckle;
C, the test of photograph thin layer chromatography, draw need testing solution 10 μ l under the assay item, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-acetonitrile-ammonia=4: 1.2: 1: 0.1 was developing solvent, launches after saturated 15 minutes, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ were dried by the fire 5 minutes; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
D, get oral liquid 30ml, put water-bath and steam near and driedly be thick, residue adds ethanol 10ml makes dissolving, filters or centrifugal, and filtrate is as need testing solution; Other gets Fructus Forsythiae control medicinal material 3g and adds water 50ml, decocts 1 hour, filters, and filtrate is put water bath method, and residue adds ethanol 2ml makes dissolving, filters, and filtrate is medical material solution in contrast; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, be developing solvent with chloroform-methanol=20: 1, in temperature is 32 ℃, exhibition launches under the above condition of 13cm, takes out, and dries, spray is 20: 1 solution with acetic anhydride-sulphuric acid, 105 ℃ of bakings 10 minutes, put coldly, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical yellow fluorescence speckle;
Content assaying method: the accurate oral liquid 20ml that draws, put in the 100ml measuring bottle, add dehydrated alcohol and be diluted to scale, shake up, placed 20 minutes, supersound process 20 minutes, room temperature was placed 30 minutes, filtered, and discarded filtrate just, the accurate subsequent filtrate 75ml that draws, put evaporate to dryness in the water-bath, residue adds water 20ml dissolving and quantitatively is transferred in the separatory funnel, with 6 each 11ml of water saturated n-butanol extraction, merge n-butanol extracting liquid, put evaporate to dryness in the water-bath, residue adds 85% ethanol 5ml, makes dissolving, join 100-150 order neutral alumina and active carbon by 6g: on the pillar of 0.15g mixing, carry out eluting with 85% ethanol with elution speed per minute 3ml, collect eluent 200ml, put evaporate to dryness in the water-bath, residue adds dissolve with methanol and standardize solution in the 5ml measuring bottle, as need testing solution; Other gets the gardenoside reference substance, adds methanol and makes the solution that every 1ml contains 0.75mg, in contrast product solution; According to thin layer chromatography test, the accurate need testing solution 10 μ l that draw, reference substance solution 8 μ l, 4 μ l, respectively the cross point in same be the silica gel G F of binding agent preparation with 0.25% sodium carboxymethyl cellulose
254On the lamellae, with chloroform-methanol-acetonitrile-ammonia=3: 1.5: 1: 0.07 was developing solvent, saturated 15 minutes, launch, take out, dry, spray is with 5% sulphuric acid ethanol liquid, and it is clear to dry by the fire to the speckle colour developing at 105 ℃, and room temperature was placed after 2 hours, carry out single wavelength zigzag scanning, wavelength X according to the thin layer chromatography thin layer chromatography scanning
S=500nm records test sample trap integrated value and reference substance trap integrated value, calculates with the external standard two-point method, promptly; Contain gardenoside C in the oral liquid
17H
24O
11Every 1ml must not be less than 0.16mg.
12, as claim 1,2, the application of 3 or 4 described pharmaceutical compositions in the medicine of preparation treatment infantile common cold.
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| CN101301383B (en) * | 2008-07-08 | 2011-12-28 | 邯郸摩罗丹药业股份有限公司 | Quality control method of formulation for clearing wind-heat of children |
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| CN101474372B (en) * | 2009-02-01 | 2011-04-27 | 贾翠菊 | Method for preparing Chinese medicine for treating children's wind-heat cold |
| CN102475835B (en) * | 2010-11-25 | 2013-12-11 | 北京东方运嘉科技发展有限公司 | Pharmaceutical composition for treating common cold or cough caused by common cold in children and preparation method thereof |
| WO2012075646A1 (en) * | 2010-12-11 | 2012-06-14 | 深圳金活利生药业有限公司 | Traditional chinese medicine composition for treating infection of influenza a virus subtype and preparation method thereof |
| CN102600378B (en) * | 2011-01-19 | 2014-01-22 | 邯郸摩罗丹药业股份有限公司 | Method for preparing medicament composition by adopting ultrafiltration process |
| CN102526517B (en) * | 2011-12-21 | 2014-06-04 | 南方医科大学珠江医院 | Traditional Chinese medicinal composition for treating influenzas and preparation method thereof |
| CN103330853B (en) * | 2013-06-27 | 2014-09-24 | 张彩英 | Traditional Chinese medicine composition for treating chronic pharyngitis |
| CN104825639B (en) * | 2015-05-27 | 2017-10-03 | 长春人民药业集团有限公司 | It is a kind of to treat children and catch cold the preparation method of Chinese medicine composition |
| CN105998804A (en) * | 2016-06-24 | 2016-10-12 | 王立丽 | Pharmaceutical composition for treating pediatric chill cold |
| CN114652782A (en) * | 2022-03-24 | 2022-06-24 | 国药集团新疆制药有限公司 | Preparation process of children Chailian oral liquid |
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