CN101195019B - Medicament for treating wet common cold in summer, technique of preparing its preparation and quality control method - Google Patents
Medicament for treating wet common cold in summer, technique of preparing its preparation and quality control method Download PDFInfo
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Abstract
The invention relates to a medicament for curing summer-heat and damp cold, which is characterized in that the invention relates to a process for preparing a traditional Chinese medicine medicament namely ageratum dispersible tablets which are reformed from ageratum granule reagents, and the technical proposal of the invention is that a dispersible tablets technology is optimized and screened, and modernized novel equipment, novel technology, and novel method are adopted by the invention, which are suitable for larger industrial production. The study on quality standard is improved and completed on the basis of an original standard, thin layer identification of medicinal material is modified and newly increased, and a determination method of content is completed and improved, the product quality standard is advanced and controllable, and clinical curative effects are guaranteed.
Description
The invention belongs to field of traditional Chinese, relate to a kind of preparation method for the treatment of the medicine and the preparation thereof of summer-heat damp cold.
Summer-heat damp cold is the commonly encountered diseases in summer, and frequently-occurring disease is different with the common cold pathogeny, and the traditional Chinese medical science thinks that summer-heat damp cold is heat-damp in summer two evil causing a disease, and has the characteristics such as loosing, consume easily impairment of QI Tianjin that rise.Summer, flu showed as summer-heat damp cold more.Fever of the body often appears in patient's diseases caused by summer heat, and micro evil wind is cold, hypohidrosis, the nasal obstruction watery nasal discharge, limb is stranded nose heave, thirsty dry lip, breast gastral cavity painful abdominal mass is vexed, symptoms such as vexed, stool viscous is difficult to resolve, yellowish or reddish urine are violated spleen easily because of damp again, can influence the fortune imbalance of taste, so summer-heat damp cold is always with gastrointestinal symptoms such as abdominal distention, nausea and vomiting, increased borborygmus and diarrheas.Doctor trained in Western medicine claims that summer-heat damp cold is a common cold of gastrointestinal type, think it by due to the multiple virus, and often with symptom of digestive tract, the course of disease is longer, matches with the summer-heat damp cold theory of the traditional Chinese medical science.The burning hot characteristics of the evil existing pathogenic summer-heat of heat-damp in summer have the heavy viscous of damp, touching deadlocked dual pathogenic characteristic again, and have obvious seasonal, and the how critical and fast change of falling ill brings great inconvenience for people's life.Treat this disease at present clinically, doctor trained in Western medicine adopts the antiviral agents treatment usually, but cures the symptoms, not the disease, and side effect is bigger, reduces body immunity.Chinese traditional treatment heat-damp in summer pathogenic factor is followed its pathogenic characteristic usually, with removing dampness induce sweat, lung qi dispersing antidiarrheal is the rule of treatment, carry out determination of treatment based on pathogenesis obtained through differentiation of symptoms and signs, a lot of Chinese medicines have antiviral simultaneously concurrently and conciliate the wet effect of evanescence of heat, the energy treating both the principal and secondary aspects of a disease, the good effect definitely, and the Chinese medicine side effect is less, is convenient to the patient and accepts.Therefore, the Chinese medicine medicine of developing the treatment heat-damp in summer pathogenic factor of safe and effective, taking convenience is of great immediate significance.
In view of the kind of recording in Ministry of Health of the People's Republic of China's standard " ageratum granule ", its reasonable recipe, be based on eliminating evilly, nurse one's health three warmers mechanism of qi and function simultaneously, with legally constituted authority side, run through the wet dissipation that induces sweat, removing dampness by means of aromatics etc. are multiple controls wet method then, rule together inside and outside having embodied, lifting is also transferred the Therapeutic Principle of reinforcing and reducing concurrently, we's the exterior and the interior on the medicine gesture divides before and after up and down and disappears, can reinforcing and reducing on the function can loose and can change, just in patchouli oil, it is warm and separate wind and cold at table both to have got its suffering, change turbid damp again in the lining with its fragrance, and can ward off dirty and in, ascending the clear and descending the turbid is equipped with Folium perillae acutae oil, the hot perfume (or spice) of the Radix Angelicae Dahuricae is dispersed, help the outer dispersing wind and cold of patchouli oil, it is can fragrant removing dampness turbid to hold concurrently; The Rhizoma Pinelliae, Pericarpium Citri Reticulatae dampness stomach function regulating, stopping nausea and vomiting by lowering the adverse flow of QI; Rhizoma Atractylodis, the wet and middle antidiarrheal of Poria spleen invigorating fortune; Cortex Magnoliae Officinalis, Pericarpium Arecae circulation of qi promoting removing dampness remove in smooth full; Rhizoma Zingiberis Recens, the humorous battalion of Radix Glycyrrhizae defend and transfer medicine and in.Comprehensive full side has relieving exterior-interior syndrome, and removing dampness is practised dirty, ascending the clear and descending the turbid, regulate the flow of vital energy and in merit, wind and cold is loose outward, the turbid damp internalization, mechanism of qi is unobstructed, taste are in harmonious proportion, then cold and heat vomiting and diarrhoea spontaneous recovery is medicine first choice of the treatment summer-heat damp cold.Therefore we have carried out further research and development to this kind.
The objective of the invention is to former granule be carried out rational form improvement, develop the onset time weak point, the fast tablet formulation of performance drug effect at the next anxious characteristics of summer-heat damp cold.Dispersible tablet is a kind of good novel form of developing in recent years, and the good reputation of " Peroral solid dosage form liquid " is arranged.Dispersible tablet can rapid disintegrate and dissolving in the short time after running into saliva, makes medicine be liquid condition, along with swallowing act enters stomach by esophagus, provides convenience for patient especially old man, child and the inconvenient person that fetches water take medicine.
Another object of the present invention is to be optimized on extraction process and to screen, and adopts modern new equipment, new technique, new method at technical elements, has formulated the production technology of reasonable science, is fit to industrialized great production; Adopt advanced extractive technique, as adopt the volatile oil among β-CD inclusion technology the other side to carry out inclusion, can effectively reduce the loss of finished product volatile oil in processes such as storage, and cover the bad smell of volatile oil, improved the mouthfeel when finished product is taken, be convenient to the patient and accept.
Another purpose of the present invention is in dispersible tablet formulation technology, screens by adopting different auxiliary material, preferably is beneficial to the adjuvant of dispersible tablet molding, has guaranteed the stability of tablet formulation.The starting point of dispersible tablet prescription design is that disintegrate became fine particle and forms uniform suspension in the short as far as possible time after tablet was met water.Therefore, quickly disintegrated proper auxiliary materials can be provided is the key that guarantees the dispersible tablet quality in selection.The used adjuvant of this product is filler, disintegrating agent, lubricant.Wherein, filler adopts a kind of in starch, lactose, dextrin, the microcrystalline Cellulose or two kinds or three kinds or four kinds, and its consumption is 40～60%; Disintegrating agent adopts a kind of in carboxymethyl starch sodium, the cross-linking sodium carboxymethyl cellulose or two kinds, and its consumption is 3%～6%, and lubricant is selected from a kind of in magnesium stearate, the sodium lauryl sulphate or two kinds, and its consumption is 0.4%～0.8%.
A further object of the present invention is that preparation has been carried out detailed deep quality standard research, on the basis of primary standard, improve, revised the discriminating of patchouli oil, and increased the thin layer discrimination method of Cortex Magnoliae Officinalis, Radix Glycyrrhizae, the Radix Angelicae Dahuricae, Pericarpium Citri Reticulatae newly, method is all simple and feasible, the feature speckle is obvious, and specificity is strong; By under two appendix items of Chinese Pharmacopoeia to the requirement of dispersible tablet, the dissolution of this product has been carried out relevant research, in quality standard, stipulated this inspection, adopt high effective liquid chromatography for measuring this product dissolution, the result shows that method is simple and feasible.Improved content assaying method, effective ingredient Hesperidin to Pericarpium Citri Reticulatae in the prescription has carried out assay, adopt high performance liquid chromatography, measure Determination of Hesperidin Content in this product, the result shows, method is simple and feasible, has accuracy and precision preferably, can control the quality of this product effectively.
Technical scheme of the present invention is: to the saturating heart, it is an amount of to add Rhizoma Zingiberis, decocts with water twice with cold water soak for the Rhizoma Pinelliae during former ageratum granule is write out a prescription, and 3 hours for the first time, 2 hours for the second time, filtration; Radix Glycyrrhizae, Pericarpium Arecae, Poria decoct with water twice, each 2 hours, filter; Cortex Magnoliae Officinalis, the Radix Angelicae Dahuricae, Rhizoma Atractylodis, Pericarpium Citri Reticulatae add water temperature and soaked 2 hours, extract volatile oil 3 hours, collect standbyly, and medicinal residues decoct with water 2 hours again, filtration.Merge above filtrate, being evaporated to relative density is the clear paste of 1.20～1.25 (60 ℃), drying; pulverize; add right amount of auxiliary materials, granulate, patchouli oil, Folium perillae acutae oil and above-mentioned standby volatile oil are carried out β-CD inclusion; get inclusion complex; with the granule mixing, add right amount of auxiliary materials, mixing; be pressed into 1000, promptly.
In extraction dried particles of the present invention, add 16.5～33g cross-linking sodium carboxymethyl cellulose or carboxymethylstach sodium, mixing sieves, and adds 2.2～4.4g magnesium stearate or sodium lauryl sulphate, mixing, tabletting is tablet of the present invention.
Using method of the present invention: oral, every day 2 times, each 4.Be described in further detail below by the extraction formulation method and the method for quality control of specific embodiment the ageratum dispersible tablet.
Embodiment 1:
With the Rhizoma Pinelliae in the former ageratum granule prescription with cold water soak to the saturating heart, it is an amount of to add Rhizoma Zingiberis, decocts with water twice, 3 hours for the first time, 2 hours for the second time, filters; Radix Glycyrrhizae, Pericarpium Arecae, Poria decoct with water twice, each 2 hours, filter; Cortex Magnoliae Officinalis, the Radix Angelicae Dahuricae, Rhizoma Atractylodis, Pericarpium Citri Reticulatae add water temperature and soaked 2 hours, extract volatile oil 3 hours, collect standbyly, and medicinal residues decoct with water 2 hours again, filtration.Merge above filtrate; being evaporated to relative density is the clear paste of 1.20～1.25 (60 ℃); drying is pulverized, and adding starch and microcrystalline Cellulose are an amount of; granulate; drying is carried out β-CD inclusion with patchouli oil, Folium perillae acutae oil and above-mentioned standby volatile oil, gets inclusion complex; with the granule mixing, be extraction dried particles of the present invention.
Embodiment 2:
With the Rhizoma Pinelliae in the former ageratum granule prescription with cold water soak to the saturating heart, it is an amount of to add Rhizoma Zingiberis, decocts with water twice, 3 hours for the first time, 2 hours for the second time, filters; Radix Glycyrrhizae, Pericarpium Arecae, Poria decoct with water twice, each 2 hours, filter; Cortex Magnoliae Officinalis, the Radix Angelicae Dahuricae, Rhizoma Atractylodis, Pericarpium Citri Reticulatae add water temperature and soaked 2 hours, extract volatile oil 3 hours, collect standbyly, and medicinal residues decoct with water 2 hours again, filtration.Merge above filtrate; being evaporated to relative density is the clear paste of 1.20～1.25 (60 ℃); drying is pulverized, and adding dextrin and starch are an amount of; granulate; drying is carried out β-CD inclusion with patchouli oil, Folium perillae acutae oil and above-mentioned standby volatile oil, gets inclusion complex; with the granule mixing, be extraction dried particles of the present invention.
Embodiment 3:
With the Rhizoma Pinelliae in the former ageratum granule prescription with cold water soak to the saturating heart, it is an amount of to add Rhizoma Zingiberis, decocts with water twice, 3 hours for the first time, 2 hours for the second time, filters; Radix Glycyrrhizae, Pericarpium Arecae, Poria decoct with water twice, each 2 hours, filter; Cortex Magnoliae Officinalis, the Radix Angelicae Dahuricae, Rhizoma Atractylodis, Pericarpium Citri Reticulatae add water temperature and soaked 2 hours, extract volatile oil 3 hours, collect standbyly, and medicinal residues decoct with water 2 hours again, filtration.Merge above filtrate; being evaporated to relative density is the clear paste of 1.20～1.25 (60 ℃); drying is pulverized, and adding lactose and microcrystalline Cellulose are an amount of; granulate; drying is carried out β-CD inclusion with patchouli oil, Folium perillae acutae oil and above-mentioned standby volatile oil, gets inclusion complex; with the granule mixing, be extraction dried particles of the present invention.
Embodiment 4:
To add 28g carboxymethylstach sodium and 2.75g sodium lauryl sulphate in any extraction dried particles in the various embodiments described above, mixing, tabletting is tablet of the present invention.
Embodiment 5:
To add 30g cross-linking sodium carboxymethyl cellulose and 3.2g sodium lauryl sulphate in any extraction dried particles in the various embodiments described above, mixing, tabletting is tablet of the present invention.
Embodiment 6:
To add 24g cross-linking sodium carboxymethyl cellulose and 3.4g magnesium stearate in any extraction dried particles in the various embodiments described above, mixing, tabletting is tablet of the present invention.
Embodiment 7:
To add 26g carboxymethylstach sodium and 3.7g magnesium stearate in any extraction dried particles in the various embodiments described above, mixing, tabletting is tablet of the present invention.
Embodiment 8:
In the quality control of the present invention, revise the thin layer of patchouli oil and differentiated, and increased the thin layer discrimination method of Cortex Magnoliae Officinalis, Radix Glycyrrhizae, the Radix Angelicae Dahuricae, Pericarpium Citri Reticulatae newly.
The thin layer of Cortex Magnoliae Officinalis is differentiated as follows: get 7 of this product, porphyrize adds methanol 50ml, supersound process 30 minutes filters the filtrate evaporate to dryness, residue adds hot water 15ml makes dissolving, put coldly, extract 3 times each 15ml with the chloroform jolting, merge chloroform liquid (water liquid is standby), evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Cortex Magnoliae Officinalis control medicinal material 1g, adds methanol 10ml, and supersound process 15 minutes filters, and filtrate is medical material solution in contrast.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution 10 μ l, control medicinal material solution 5 μ l, respectively put in same be on the gel GF 254 plate of adhesive with the sodium carboxymethyl cellulose, with chloroform-benzene-ethyl acetate (5: 4: 1) is developing solvent, take out, dry, put under the ultra-violet lamp (254nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the skin dark stain of same color.
The thin layer of Radix Glycyrrhizae is differentiated as follows: get Cortex Magnoliae Officinalis and differentiate the aqueous solution behind the chloroform extraction under the item, with water saturated n-butanol extraction 3 times, each 15ml, merge n-butyl alcohol liquid, use the saturated water washing of n-butyl alcohol 2 times, each 20ml, discard water liquid, n-butyl alcohol liquid evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution.Extracting liquorice control medicinal material 1g adds methanol 20ml in addition, and supersound process 30 minutes filters, and filtrate evaporate to dryness, residue add methanol 5ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution 5 μ l, control medicinal material solution 3 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with chloroform-methanol-water (40: 10: 1), launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
The thin layer of the Radix Angelicae Dahuricae is differentiated as follows: get Radix Angelicae Dahuricae control medicinal material 1g, porphyrize adds methanol 20ml, and supersound process 30 minutes filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution 8 μ l, control medicinal material solution 10 μ l under the Cortex Magnoliae Officinalis discriminating item, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform-ethanol (17: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (254nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
The thin layer of Pericarpium Citri Reticulatae is differentiated as follows: get 3 of this product, porphyrize adds methanol 20ml, and supersound process 15 minutes filters, and filtrate is as need testing solution.Other gets Pericarpium Citri Reticulatae control medicinal material 0.1g, shines medical material solution in pairs with legal system, and it is an amount of to get the Hesperidin reference substance again, adds methanol and makes the solution that every 1ml contains 0.4mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 4 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ethyl acetate-methanol-water (100: 17: 13) is developing solvent, launches, and takes out, dry, spray is with the aluminum chloride test solution, and hot blast drying is put under the ultra-violet lamp (365nm) and inspected.In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
The thin layer of patchouli oil is differentiated as follows: get 12 of this product, porphyrize adds petroleum ether (60～90 ℃) 30ml, and supersound process 5 minutes filters, and filtrate volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution.Other gets patchouli oil 0.1ml, adds ethyl acetate 10ml and makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution 8 μ l, control medicinal material solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with petroleum ether (60～90 ℃)-ethyl acetate (16: 1) is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
In the quality control of the present invention, stipulated the inspection of dissolution: get this product, according to dissolution method (two appendix XC second methods of Chinese Pharmacopoeia version in 2005), with 0.5% sodium dodecyl sulfate solution 900ml is dissolution medium, and rotating speed is that per minute 100 changes, operation in accordance with the law, in the time of 20 minutes, get solution 2ml, filter, get subsequent filtrate as need testing solution; It is an amount of that other gets the Hesperidin reference substance, and accurate the title decides, and adds methanol and makes the solution that every 10ml contains 2.5mg, and precision is measured 1ml, is diluted to 50ml with dissolution medium, in contrast product solution.Precision is measured need testing solution and each 10 μ l of reference substance solution, injects chromatograph of liquid respectively, and the record chromatogram is by the stripping quantity of external standard method with every of calculated by peak area.
In the quality control of the present invention, perfect Determination of Hesperidin Content mensuration:, be filler with the octadecylsilane chemically bonded silica according to high effective liquid chromatography for measuring; With acetonitrile-0.05mol/L phosphate sodium dihydrogen buffer solution (phosphoric acid is regulated pH value to 3.0) (24: 76) is mobile phase; The detection wavelength is 284nm.Number of theoretical plate calculates by the Hesperidin peak should be not less than 2000.Get the about 5mg of Hesperidin reference substance, the accurate title, decide, and puts in the 10ml measuring bottle, adds dissolve with methanol and be diluted to scale, shakes up, and precision is measured 1ml, puts in the 10ml measuring bottle, adds methanol to scale, shakes up, and promptly gets (every 1ml contains Hesperidin 50 μ g).Get this product under the weight differential item, porphyrize is got about 0.4g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, supersound process (power 100W, frequency 40kHz) 30 minutes, put coldly, claim to decide weight again, supply the weight that subtracts mistake with methanol, shake up, filter, get subsequent filtrate as need testing solution.Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly.
Below by test the adjuvant in the above-mentioned dispersible tablet formulation process is further screened and optimizes.
Test example 1: the screening of different auxiliary material
Get the granule that makes, add magnesium stearate, sodium lauryl sulphate, micropowder silica gel respectively in 0.5% ratio respectively, 5% carboxymethylstach sodium, low-substituted hydroxypropyl cellulose, cross-linking sodium carboxymethyl cellulose, mixing, tabletting the results are shown in Table 1 respectively.
Table 1 different auxiliary material is to the influence of dispersible tablet
The result shows that preferred magnesium stearate, sodium lauryl sulphate are lubricant, and cross-linking sodium carboxymethyl cellulose, carboxymethylstach sodium are that disintegrating agent carries out the different proportion combination, and tablet appearance is better.
Test example 2: the investigation of different auxiliary material addition
At first the consumption of sodium lauryl sulphate is investigated
Get the granule that makes, add sodium lauryl sulphate in 0.3%, 0.4%, 0.5%, 0.8% ratio respectively, 5% carboxymethylstach sodium, mixing, tabletting the results are shown in Table 2 respectively.
Table 2 sodium lauryl sulphate addition is to the influence of dispersible tablet
The sodium lauryl sulphate addition is 0.3% o'clock, and tablet weight variation is bigger, and 1 overrun is arranged; Consumption is 0.4% and 0.8% o'clock, and the gained tablet surface is smooth, and is smooth, no sliver phenomenon.Therefore determine that the sodium lauryl sulphate consumption is 0.4～0.8%.
Further the consumption of carboxymethylstach sodium is investigated.
Get the granule that makes, add carboxymethylstach sodium in 2%, 3%, 4%, 6% ratio respectively, add 0.5% sodium lauryl sulphate, mixing, tabletting the results are shown in Table 3 respectively.
Table 3 carboxymethylstach sodium addition is to the influence of dispersible tablet
According to result of the test, select for use the carboxymethylstach sodium of 0.4～0.8% sodium lauryl sulphate and 3～6% good as the dispersible tablet quality that adjuvant makes.
Claims (5)
1. Chinese medicine preparation for the treatment of summer-heat damp cold, it is characterized in that its preparation method be with the Rhizoma Pinelliae in the former ageratum granule prescription with cold water soak to the saturating heart, it is an amount of to add Rhizoma Zingiberis, decocts with water twice, 3 hours for the first time, 2 hours for the second time, filters; Radix Glycyrrhizae, Pericarpium Arecae, Poria decoct with water twice, each 2 hours, filter; Cortex Magnoliae Officinalis, the Radix Angelicae Dahuricae, Rhizoma Atractylodis, Pericarpium Citri Reticulatae adds water temperature and soaked 2 hours, extracted volatile oil 3 hours, collect standby, medicinal residues decoct with water 2 hours again, filter, and merge above filtrate, being evaporated to and measuring relative densities at 60 ℃ is 1.20～1.25 clear paste, drying is pulverized, and granulates, with patchouli oil, Folium perillae acutae oil and above-mentioned standby volatile oil carry out β-CD inclusion, get inclusion complex,, add right amount of auxiliary materials with the granule mixing, be pressed into 1000, that is, wherein said adjuvant comprises filler, disintegrating agent and lubricant, wherein filler is selected from starch, dextrin, lactose, a kind of in the microcrystalline Cellulose or two kinds or three kinds or four kinds; Disintegrating agent is selected from a kind of in cross-linking sodium carboxymethyl cellulose, the carboxymethylstach sodium or two kinds; Lubricant is selected from a kind of in magnesium stearate, the sodium lauryl sulphate or two kinds.
2. the described a kind of Chinese medicine preparation for the treatment of summer-heat damp cold of claim 1, it is characterized in that in the dispersible tablet formulation process being starch, dextrin, lactose, microcrystalline Cellulose as filler, its consumption is 40～60%, as disintegrating agent is cross-linking sodium carboxymethyl cellulose, carboxymethylstach sodium, its consumption is 3%～6%, as lubricant be magnesium stearate, sodium lauryl sulphate, its consumption is 0.4%～0.8%.
3. the described a kind of Chinese medicine preparation for the treatment of summer-heat damp cold of claim 1, it is characterized in that in the dispersible tablet formulation process as filler be starch and microcrystalline Cellulose, its consumption is respectively 27% and 23%; As disintegrating agent be carboxymethylstach sodium, its consumption is 5%, as lubricant be sodium lauryl sulphate, its consumption is 0.5%.
4. the described a kind of Chinese medicine preparation for the treatment of summer-heat damp cold of claim 1 is characterized in that in the dispersible tablet formulation process as the lactose that is of filler, its consumption is 54%; As disintegrating agent be cross-linking sodium carboxymethyl cellulose, its consumption is 5.5%, as lubricant be magnesium stearate, its consumption is 0.7%.
5. the described a kind of Chinese medicine preparation for the treatment of summer-heat damp cold of claim 1 is characterized in that its quality control index is:
Thin layer is differentiated as follows:
The thin layer of Cortex Magnoliae Officinalis is differentiated as follows: get 7 of this product, porphyrize adds methanol 50ml, supersound process 30 minutes, filter, filtrate evaporate to dryness, residue add hot water 15ml makes dissolving, put cold, extract 3 times with the chloroform jolting, each 15ml, water liquid is standby, merge chloroform liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution, other gets Cortex Magnoliae Officinalis control medicinal material 1g, add methanol 10ml, supersound process 15 minutes filters, filtrate is medical material solution in contrast, according to the thin layer chromatography test of an appendix VI of Chinese Pharmacopoeia version in 2005 B, draw need testing solution 10 μ l, control medicinal material solution 5 μ l, put respectively in same be on the gel GF 254 plate of adhesive with the sodium carboxymethyl cellulose, be that chloroform-benzene-ethyl acetate of 5: 4: 1 is developing solvent with ratio, take out, dry, put under the ultra-violet lamp that wavelength is 254nm and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the skin dark stain of same color;
The thin layer of Radix Glycyrrhizae is differentiated as follows: get the aqueous solution after Cortex Magnoliae Officinalis is differentiated a following chloroform extraction, and with water saturated n-butanol extraction 3 times, 15ml at every turn, merge n-butyl alcohol liquid, use the saturated water washing of n-butyl alcohol 2 times, each 20ml, discard water liquid, n-butyl alcohol liquid evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution, other is extracting liquorice control medicinal material 1g, add methanol 20ml, supersound process 30 minutes filters, the filtrate evaporate to dryness, residue adds methanol 5ml makes dissolving, and medical material solution is tested according to the thin layer chromatography of an appendix VI of Chinese Pharmacopoeia version in 2005 B in contrast, draw need testing solution 5 μ l, control medicinal material solution 3 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be that chloroform-methanol-water of 40: 10: 1 is developing solvent with ratio, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear to be heated to speckle colour developing at 105 ℃, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
The thin layer of the Radix Angelicae Dahuricae is differentiated as follows: get Radix Angelicae Dahuricae control medicinal material 1g, porphyrize, add methanol 20ml, supersound process 30 minutes, filter, the filtrate evaporate to dryness, residue adds methanol 1ml makes dissolving, and medical material solution is tested according to the thin layer chromatography of an appendix VI of Chinese Pharmacopoeia version in 2005 B in contrast, draw the need testing solution 8 μ l under the Cortex Magnoliae Officinalis discriminating item, control medicinal material solution 10 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be that chloroform-ethanol of 17: 1 is developing solvent with ratio, launch, take out, dry, put under the ultra-violet lamp that wavelength is 254nm and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
The thin layer of Pericarpium Citri Reticulatae is differentiated as follows: get 3 of this product, porphyrize, add methanol 20ml, supersound process 15 minutes, filter, filtrate is as need testing solution, and other gets Pericarpium Citri Reticulatae control medicinal material 0.1g, shines medical material solution in pairs with legal system, it is an amount of to get the Hesperidin reference substance again, add methanol and make the solution that every 1ml contains 0.4mg, product solution is tested according to the thin layer chromatography of an appendix VIB of Chinese Pharmacopoeia version in 2005 in contrast, draw each 4 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be that ethyl acetate-methanol-water of 100: 17: 13 is developing solvent with ratio, launch, take out, dry, spray is with aluminum chloride test solution, hot blast drying, put under the ultra-violet lamp that wavelength is 365nm and inspect, in the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
The thin layer of patchouli oil is differentiated as follows: get 12 of this product, porphyrize, add boiling range and be 60～90 ℃ petroleum ether 30ml, supersound process 5 minutes filters, and filtrate volatilizes, residue adds ethyl acetate 1ml makes dissolving, as need testing solution, other gets patchouli oil 0.1ml, adds ethyl acetate 10ml and makes dissolving, medical material solution in contrast, according to the thin layer chromatography test of an appendix VI of Chinese Pharmacopoeia version in 2005 B, draw need testing solution 8 μ l, control medicinal material solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with ratio is that 16: 1 boiling range is that 60～90 ℃ petroleum ether-ethyl acetate is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
The inspection of dissolution is as follows: get this product, dissolution method according to two appendix X of Chinese Pharmacopoeia version in 2005 C, second method, with 0.5% sodium dodecyl sulfate solution 900ml is dissolution medium, rotating speed is that per minute 100 changes, operation in the time of 20 minutes, is got solution 2ml in accordance with the law, filter, get subsequent filtrate as need testing solution; It is an amount of that other gets the Hesperidin reference substance, the accurate title, decide, add methanol and make the solution that every 10ml contains 2.5mg, precision is measured 1ml, is diluted to 50ml with dissolution medium, in contrast product solution, precision is measured need testing solution and each 10 μ l of reference substance solution, inject chromatograph of liquid respectively, the record chromatogram is by the stripping quantity of external standard method with every of calculated by peak area;
Determination of Hesperidin Content is measured as follows: according to high effective liquid chromatography for measuring, be filler with the octadecylsilane chemically bonded silica; Phosphate sodium dihydrogen buffer solution with acetonitrile-regulate pH value to 3.0 with the phosphoric acid of 0.05mol/L is a mobile phase, and ratio is 24: 76; The detection wavelength is 284nm, and number of theoretical plate calculates by the Hesperidin peak should be not less than 2000, gets the about 5mg of Hesperidin reference substance, the accurate title, decide, and puts in the 10ml measuring bottle, adds dissolve with methanol and be diluted to scale, shake up, precision is measured 1ml, puts in the 10ml measuring bottle, add methanol to scale, shake up, promptly get the reference substance solution that every 1ml contains Hesperidin 50 μ g, get this product under the weight differential item, porphyrize is got about 0.4g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, at power 100W, supersound process is 30 minutes under the frequency 40kHz condition, puts coldly, claims to decide weight again, supply the weight that subtracts mistake with methanol, shake up, filter, get subsequent filtrate as need testing solution, accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
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| CN109991359B (en) * | 2018-01-02 | 2021-07-13 | 苏州玉森新药开发有限公司 | Quality control method of Chinese medicinal composition with cough relieving and phlegm eliminating effects |
| CN110927322B (en) * | 2019-11-07 | 2022-05-17 | 石药集团中奇制药技术（石家庄）有限公司 | Detection method of Huoxiang Zhengqi mixture |
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