CN1895408B - Radix saposhnikoviae Tong Sheng capsules, preparation and quality control method thereof - Google Patents
Radix saposhnikoviae Tong Sheng capsules, preparation and quality control method thereof Download PDFInfo
- Publication number
- CN1895408B CN1895408B CN2006100144639A CN200610014463A CN1895408B CN 1895408 B CN1895408 B CN 1895408B CN 2006100144639 A CN2006100144639 A CN 2006100144639A CN 200610014463 A CN200610014463 A CN 200610014463A CN 1895408 B CN1895408 B CN 1895408B
- Authority
- CN
- China
- Prior art keywords
- radix
- extract
- emodin
- chrysophanol
- rhizoma rhei
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
- Medicinal Preparation (AREA)
Abstract
A Chinese medicine 'Tongsheng softgel' is prepared from 17 Chinese-medicinal materials including ledebouriella root, mint, rhubarb, capejasmine fruit, etc, matrix, suspending aid, and lubricant. Its preparing process and its quality control method are also disclosed.
Description
Technical field
The invention belongs to novel form that Chinese medicine compound makes and preparation method thereof, particularly relate to logical holy soft capsule of a kind of Radix Saposhnikoviae and preparation method thereof and method of quality control.
Background technology
The logical sage side of Radix Saposhnikoviae for induce sweat, heat clearing away, the agent of capturing the three and using, former side comes from " Xuanming Lun Fang, Clear Synopsis on Recipes ", is the name side of gold dollar well-known doctor Liu interchannel foundation, is used for the exogenous cold interior-heat, excess in both the exterior and interior, aversion to cold high fever, headache dry pharynx, oliguria with reddish urine, constipation, scrofula is from the beginning of, diseases such as rubella eczema.Because the fangfeng tongsheng pill clinical practice is with a long history, safe and effective, now has been put into the Chinese patent medicine nonprescription drugs.The original dosage form of we is a decoction made from powder, and usefulness is decocted in water for oral dose." Chinese pharmacopoeia one one of version in 2005 discloses the prescription and the preparation method of fangfeng tongsheng pill.Its prescription is Radix Saposhnikoviae 50g, Herba Schizonepetae 25g, Herba Menthae 50g, Herba Ephedrae 50g, Radix Et Rhizoma Rhei 50g, Natrii Sulfas 50g, Fructus Gardeniae 25g, Talcum 300g, Radix Platycodonis 100g, Gypsum Fibrosum 100g, Rhizoma Chuanxiong 50g, Radix Angelicae Sinensis 50g, Radix Paeoniae Alba 50g, Radix Scutellariae 100g, Fructus Forsythiae 50g, Radix Glycyrrhizae 200g, the Rhizoma Atractylodis Macrocephalae (stir-fry) 25g.Its preparation method is above 17 flavors, and except that Natrii Sulfas, Talcum, all the other pulverizing medicinal materials become fine powder, mixing; Natrii Sulfas is dissolved in water, and filters; Pulvis Talci is broken into impalpable powder; Get above-mentioned powder, with the general ball of Natrii Sulfas filtrate, drying is used the Pulvis Talci coating, polishing, and drying, promptly." ministry standard Chinese traditional patent formulation preparation " the 11st discloses the logical holy big honeyed pills of Radix Saposhnikoviae, and the 15th discloses the logical holy concentrated pill of Radix Saposhnikoviae.The preparation method of big honeyed pills is with pulverizing medicinal materials, and mixing, every 100g powder add refined honey 110～120g and make big honeyed pills, promptly.The preparation method of concentrated pill is that Radix Saposhnikoviae, Radix Et Rhizoma Rhei, the Radix Paeoniae Alba, Radix Glycyrrhizae (100g), Rhizoma Chuanxiong, Gypsum Fibrosum, Natrii Sulfas, Pulvis Talci are broken into fine powder, and nine flavors such as all the other Radix Glycyrrhizaes and all the other Herba Schizonepetaes are ground into coarse powder, decoct with water twice, collecting decoction filters, and filtrate is condensed into the thick paste that relative density is 1.30 (20 ℃), with above-mentioned fine powder mixing, oven dry is ground into fine powder, uses water pill, oven dry, polishing, black grey coating, promptly.Except that pill, the domestic report of existing multiple 'Fangfeng Tongsheng ' now is as granule, capsule etc.In the logical sage side of Radix Saposhnikoviae, Herba Menthae, Herba Schizonepetae, Radix Saposhnikoviae and Herba Ephedrae are monarch drug altogether, and Herba Menthae wherein, Herba Schizonepetae contain multiple volatile ingredient.Pill adopts medical material directly to pulverize the method for pill, and technology is original, long term store, and volatile ingredient wherein easily scatters and disappears, and affects the treatment.Though granule, capsule are the preparations through extracting, but still do not solve the problem that volatile ingredient scatters and disappears." Chinese pharmacopoeia version in 2005 reaches 'Fangfeng Tongsheng ' of putting down in writing in " ministry standard " and all has only thin layer to differentiate, and does not have the assay item, and quality standard is low in addition.
Summary of the invention
The objective of the invention is to utilize the logical holy raw material of conventional Radix Saposhnikoviae to form and consumption proportion, under the prerequisite that does not lessen the curative effect, propose logical holy soft capsule of a kind of Radix Saposhnikoviae and preparation method thereof.
Another object of the present invention provides the method for quality control of the logical holy soft capsule of a kind of Radix Saposhnikoviae.Adopt Modern Analytical Instrument and the means content of active component in the logical holy soft capsule of quantitative assay Radix Saposhnikoviae fast and accurately.
The logical holy soft capsule of the Radix Saposhnikoviae that the present invention proposes, comprise capsule liquid, softgel shell, it is characterized in that capsule liquid composition is made up of the recipe quantity extract and the adjuvant of Radix Saposhnikoviae, Herba Schizonepetae, Herba Menthae, Herba Ephedrae, Radix Et Rhizoma Rhei, Natrii Sulfas, Fructus Gardeniae, Talcum, Radix Platycodonis, Gypsum Fibrosum, Rhizoma Chuanxiong, Radix Angelicae Sinensis, the Radix Paeoniae Alba, Radix Scutellariae, Fructus Forsythiae, Radix Glycyrrhizae, the Rhizoma Atractylodis Macrocephalae ten seven flavor medicine materials, adjuvant comprises substrate, suspending agent, wetting agent.
Radix Saposhnikoviae of the present invention is led to holy soft capsule, and the weight proportion of each component is in the capsule liquid:
Component is proportion in capsule liquid
Medicinal substances extract 36%～53%
Substrate 43%～59%
Suspending agent 2%～7%
Wetting agent 2%～4%
Radix Saposhnikoviae of the present invention is led to holy soft capsule, and the weight proportion of each component is in the comparatively preferred capsule liquid:
Component is proportion in capsule liquid
Medicinal substances extract 42%～47%
Substrate 46%～51%
Suspending agent 2%～5%
Wetting agent 2%～4%
Medicinal substances extract of the present invention is the dry extract that makes through decocting in water, precipitate with ethanol of the medical material of recipe quantity and the mixture of volatile oil; Its prescription is " disclosed fangfeng tongsheng pill prescription of Chinese pharmacopoeia version in 2005: Radix Saposhnikoviae 50g, Herba Schizonepetae 25g, Herba Menthae 50g, Herba Ephedrae 50g, Radix Et Rhizoma Rhei 50g, Natrii Sulfas 50g, Fructus Gardeniae 25g, Talcum 300g, Radix Platycodonis 100g, Gypsum Fibrosum 100g, Rhizoma Chuanxiong 50g, Radix Angelicae Sinensis 50g, Radix Paeoniae Alba 50g, Radix Scutellariae 100g, Fructus Forsythiae 50g, Radix Glycyrrhizae 200g, the Rhizoma Atractylodis Macrocephalae (stir-fry) 25g.Substrate is that vegetable oil comprises: one or more in Semen Maydis oil, salad oil, the Petiolus Trachycarpi oil; Suspending agent is one or more in Cera Flava, aluminum monostearate, the ethyl cellulose; Wetting agent is that fabaceous lecithin, Tweens comprise one or more in Tween-60, the tween 80.
Radix Saposhnikoviae of the present invention is led to holy preparation of soft capsule method, it is characterized in that it comprises following process steps:
(1) get Radix Et Rhizoma Rhei and pulverize, with 6～10 times of amount 60%～80% ethanol extractions, extracting solution reclaims ethanol, concentrate, drying, dry extract, pulverize, sieve, get dry powder;
(2) after all the other ten Six-element pulverizing medicinal materials, the mixing, add 6～10 times of water gagings extractions 1～2 time, it is standby to extract volatile oil simultaneously, and decocting liquid filters, merging, and precipitate with ethanol filters, and filtrate is concentrated, dry, gets dry extract, pulverizes, and gets dry powder;
(3) with above-mentioned two kinds of dry extract mix homogeneously, merge with volatile oil, add adjuvant, make suspension, be filled into soft capsule shell, promptly.
According to described preparation method, wherein Radix Et Rhizoma Rhei adopts 60～80% ethanol refluxing processes to extract in the step (1).
According to described preparation method, wherein Radix Et Rhizoma Rhei adopts 60～80% alcohol dipping methods to extract in the step (1).
According to described preparation method, wherein Radix Et Rhizoma Rhei adopts 60～80% alcohol percolation methods to extract in the step (1).
The method of quality control of the logical holy soft capsule of Radix Saposhnikoviae of the present invention is characterized in that medicinal substances extract adopts emodin and chrysophanol in the quantitative determination of high-performance liquid Radix Et Rhizoma Rhei to comprise:
(1) chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler; Methanol: 0.1% phosphoric acid solution is a mobile phase at 65: 35; Detect wavelength 254nm; Theoretical cam curve is calculated by the emodin peak should be not less than 3000;
(2) preparation of reference substance solution: precision takes by weighing emodin, each 5mg of chrysophanol reference substance, puts respectively in the 50ml measuring bottle, with dissolve with methanol and be diluted to scale and shake up; Precision is measured emodin solution 1ml, chrysophanol solution 2ml respectively, puts respectively in the 25ml measuring bottle, adds methanol to scale, shakes up, and, contains 4 μ g among the every 1ml of emodin that is, contains 8 μ g among the every 1ml of chrysophanol;
(3) preparation of need testing solution: get this product 1g under the weight differential item, the accurate title, decide, and puts in the 50ml conical flask, precision adds methanol 25ml, claims to decide weight, reflux 30 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, filter, precision is measured subsequent filtrate 5ml, put in the 50ml round-bottomed flask, fling to methanol, add 2.5mol/L sulfuric acid solution 10ml, supersound process 5 minutes adds chloroform 10ml again, reflux 1 hour, cooling moves in the separatory funnel, uses the minimum of chloroform washing container, incorporate in the separatory funnel, divide and get chloroform layer, acid solution chloroform extraction 2 times, each about 10ml, combined chloroform liquid is with anhydrous sodium sulfate dehydration, chloroform solution moves in the 100ml conical flask, flings to chloroform, and the residue precision adds methanol 10ml, claim to decide weight, put slight fever dissolved residue in the water-bath, put cold after, claim to decide weight again, supply the weight that subtracts mistake with methanol, shake up, filter, get subsequent filtrate, promptly;
(4) accurate respectively above-mentioned two kinds of reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly; Every of this product contains Radix Et Rhizoma Rhei with emodin (C
15H
10O
5) and chrysophanol (C
15H
10O
4) the total amount meter, must not be less than 0.25mg.
In the fangfeng tongsheng pill prescription: Herba Ephedrae, Herba Schizonepetae, Radix Saposhnikoviae, Herba Menthae dispelling wind to relieve the exterior syndrome, exopathogen is separated from antiperspirant, be monarch drug altogether.Radix Et Rhizoma Rhei, Natrii Sulfas purging heat to relax the bowels, Talcum, Fructus Gardeniae clearing away heat-damp and promoting diuresis make interior-heat just divide from two and disappear; Gypsum Fibrosum, Radix Scutellariae, Fructus Forsythiae, the detoxifcation of Radix Platycodonis clearing away heat-fire are ministerial drug altogether.Radix Angelicae Sinensis, the Radix Paeoniae Alba, Rhizoma Chuanxiong nourish blood and blood; Rhizoma Atractylodis Macrocephalae the spleen strengthening and damp drying is an adjuvant drug.The Radix Glycyrrhizae QI invigorating and in, coordinating the actions of various ingredients in a prescription is messenger drug.All medicines share, and down clear sharp four methods of antiperspirant possess, and play the Tongli that induces sweat altogether, the merit of heat-clearing and toxic substances removing.
The logical holy soft capsule of Radix Saposhnikoviae of the present invention is compared with existing dosage form, has following advantage:
| Dosage form | Pluses and minuses |
| Radix Saposhnikoviae is led to holy soft capsule | Dose little (at every turn taking the suitable and crude drug 6g of 1.74g) easily absorbs, instant effect, and side effect is little, is easy to keep effective ingredient. |
| Fangfeng tongsheng pill | Dose big (take 6g, 2 times on the one, per 20 balls weigh 1g at every turn), it is slow to take effect, and mouthfeel is poor. |
| Radix Saposhnikoviae is led to holy granule | Volatile ingredient scatters and disappears and affects the treatment more, and dose is big, and mouthfeel is poor, takes inconvenience. |
| Radix Saposhnikoviae is led to holy capsule | Dose is few, but effective ingredient is lost many, weak curative effect. |
Radix Saposhnikoviae has multi-flavors such as Herba Menthae, Herba Schizonepetae to contain the volatile oil medical material in the logical sage side, pill is changed system into soft capsule can be dissolved in the volatile oil that proposes in the adjuvant of soft capsule, gel coat sealing inclusion is arranged outward, overcome the weak point of pill, granule and capsule dosage form, made that effective ingredient is able to abundant reservation in the medical material.
Following table is that logical holy soft capsule of Radix Saposhnikoviae and existing dosage form are stored volatile oil content (ml/100g content) comparison after a year:
| Dosage form | Before the storage | After the storage | ||
| Radix Saposhnikoviae is led to holy soft capsule | Sample 1 | 0.33 | Sample 1 | 0.33 |
| Sample 2 | 0.34 | Sample 2 | 0.33 | |
| Sample 3 | 0.33 | Sample 3 | 0.32 | |
| Dosage form | Before the storage | After the storage | ||
| Fangfeng tongsheng pill | Sample 1 | 0.28 | Sample 1 | 0.15 |
| Sample 2 | 0.27 | Sample 2 | 0.13 | |
| Sample 3 | 0.26 | Sample 3 | 0.12 | |
| Radix Saposhnikoviae is led to holy granule | Sample 1 | 0.25 | Sample 1 | 0.15 |
| Sample 2 | 0.26 | Sample 2 | 0.17 | |
| Sample 3 | 0.25 | Sample 3 | 0.16 | |
| Radix Saposhnikoviae is led to holy capsule | Sample 1 | 0.26 | Sample 1 | 0.19 |
| Sample 2 | 0.28 | Sample 2 | 0.20 | |
| Sample 3 | 0.26 | Sample 3 | 0.18 | |
Further specify good effect of the present invention below by pharmacological evaluation and clinical trial.
One, pharmacodynamics test:
To the logical holy soft capsule of Radix Saposhnikoviae carried out analgesic, decorporation just, urinate, antiinflammatory, analgesia, antiallergic, etc. the research of aspect.Result of the test shows:
The logical continuous gastric infusion of holy soft capsule 10.0g crude drug/kg of Radix Saposhnikoviae 5 days can obviously suppress rat fever reaction due to the yeast.2. the logical holy soft capsule 5.0 of Radix Saposhnikoviae, continuous 1 week of gastric infusion of 10.0g crude drug/kg, can shorten mice melena efflux time.3. the logical holy soft capsule 2.5,5.0 of Radix Saposhnikoviae, continuous 1 week of gastric infusion of 10.0g crude drug/kg, can increase after the mice administration feces volume in 4 hours.Can promote the mice excretion of urine, its effect slightly is better than with the dosage fangfeng tongsheng pill, but there was no significant difference.4. the logical holy soft capsule 2.5,5.0 of Radix Saposhnikoviae, continuous 1 week of gastric infusion of 10.0g crude drug/kg, after administration 1,2,3 hour, can obviously suppress rat paw edema reaction due to the chondrus ocellatus Holmes.5. the logical holy soft capsule 2.5,5.0 of Radix Saposhnikoviae, continuous 1 week of gastric infusion of 10.0g crude drug/kg, administration group and matched group ratio can suppress obviously due to low molecular dextran induced mice pruritus, mice models of passive skin irritability of the same race, the histamine that the Cavia porcellus foot is itched, acetic acid induced mice writhing response.Find out thus the logical holy soft capsule of Radix Saposhnikoviae have stronger analgesia, antiinflammatory, analgesic, decorporation just, urinate, anti-allergic effects, cure mainly basically identical with the function of fangfeng tongsheng pill.
Two, toxicology test:
1. chmice acute toxicity:
The logical holy soft capsule of Radix Saposhnikoviae is by the disposable gastric infusion 148.40,185.50,231.88 of mice body weight, 289.38g crude drug/kg, after the administration mice occur autonomic activities reduce, close order, prostrate, breathe reaction such as slow down.Death time of animal is between 0.5-4 hour, and dead animal is dissected perusal immediately and do not seen that internal organs have abnormality.It is normal that surviving animals is recovered after 24 hours fully.The logical holy soft capsule LD50 value of Radix Saposhnikoviae is 231.53g crude drug/kg, is equivalent to 1157.6 times of the clinical consumption of people (12g crude drug/day/people), shows that Radix Saposhnikoviae leads to holy soft capsule clinical drug safety.
2. rat long term toxicity:
Radix Saposhnikoviae is led to holy soft capsule 30,15, three dosage of 7.5g crude drug/kg gastric infusion every day once, and successive administration is 7 days weekly.The rat body weight in 4 weeks of administration and 2 weeks of drug withdrawal increases normal, and the more female Mus of male Mus body weight gain speed is fast, but three dosage group body weight change are compared there was no significant difference with matched group.Each administration group rat urine, defecation, drink water, take the photograph material and general signs and matched group no significant difference.Routine urianlysis: each 4 week of administration group gastric infusion and drug withdrawal eight indexs of 2 all rat urine and matched group be no significant difference relatively.Erythrocyte, hemoglobin, the platelet value of the male Mus low dose group of administration group all were lower than matched group during the hematology measured; But jenny and middle and high dosage group are not seen significant change.Belong to the variation of normal range through analysis-by-synthesis.Other every indexs and matched group are than notable difference is not arranged.After 2 weeks of drug withdrawal, every hematological indices of the female tom of each administration group is all in normal range.In biochemical analysis, the blood glucose of female Mus high dose of administration phase, total protein and creatinine value are lower than matched group, and the albumin value is higher than matched group.Blood urea nitrogen, creatinine and the total bilirubin value of dosage group are lower than matched group in the male Mus, and the blood urea nitrogen value of middle and high dosage group is lower than matched group.More than changing no clinical toxicology meaning, only is significant difference, and other biochemical indicators and matched group are than equal no significant difference.After 2 weeks of drug withdrawal, difference that the measured value of the every biochemical indicator of administration group compares with matched group that there are no significant.In organ coefficient was checked, Radix Saposhnikoviae was led to the uterus ovary of holy soft capsule in administration female Mus low dose group during 4 weeks, middle dosage group liver, kidney, and the kidney of high dose group, adrenal gland, the liver of the middle and high dosage group of male Mus, the organ coefficient of kidney and matched group more all have weightening finish.Other organ coefficients of administration phase and organ weights and matched group relatively there are no significant difference.The organ coefficient of drug withdrawal 2 each administration group of all backs and organ weights and matched group be indifference more also.The above internal organs of binding of pathological morphological observation change the fluctuation that still belongs in normal range.
3. PATHOMORPHOLOGICAL OBSERVATION OF PULLORUM:
Logical high, medium and low three the dosage groups of holy soft capsule of Radix Saposhnikoviae are in 4 weeks of administration and 2 weeks of drug withdrawal the rat main organs be there is no and be subjected to the relevant pathological change of reagent thing toxicity.So show that it is basic security dosage that Radix Saposhnikoviae lead to holy soft capsule 30g crude drug/kg (be equivalent to people's consumption 150 times).
Three, clinical trial:
The logical holy soft capsule of Radix Saposhnikoviae has carried out clinical trial year January in April, 2005 to 2006 at Xiyuan Hospital, Chinese Medicine Academy of China, Hospital No.1 Attached to Tianjin Traditional Chinese Medicine College, No.1 Hospital Attached to Hunan College of Traditional Chinese Medicine, Huaxi Hospital Attached to Sichuan Univ, and the purpose of test is to confirm and estimate the safety and the effectiveness of the logical holy soft capsule treatment of Radix Saposhnikoviae flu, urticaria, eczema.Current effective case 192 examples of clinical trial test group, effective case 192 examples of matched group.Result of the test shows, the logical holy soft capsule treatment of the Radix Saposhnikoviae exogenous cold interior-heat excess in both the exterior and interior type rate 50.00% that throws off a cold, cure-remarkable-effectiveness rate 93.33%; Treatment urticaria cure rate 18.33%, cure-remarkable-effectiveness rate 61.67%; Treatment eczema cure rate 16.13%, cure-remarkable-effectiveness rate 40.32%.During the clinical trial, do not see any untoward reaction, illustrate that this product clinical drug safety is reliable.
The analytical method that the present invention is set up is further described below:
1. instrument and reagent
High performance liquid chromatograph: Waters 2695 high performance liquid chromatographs, Waters 2487 UV-detector, TSKgelODS 100s 150mm chromatographic column.
Reference substance: emodin is available from Nat'l Pharmaceutical ﹠ Biological Products Control Institute (using for assay), lot number: 0756-200110.
Chrysophanol is available from Nat'l Pharmaceutical ﹠ Biological Products Control Institute (using for assay), lot number 0796-200006.
2. chromatographic condition
Chromatographic column: octadecyl silane is a filler; Methanol-0.1% phosphoric acid (65: 35) is mobile phase; Detect wavelength: 254nm; Flow 1.0ml/min; Emodin, chrysophanol and other component can reach baseline separation and meet 2005 editions pharmacopeia separating degrees and require (seeing figure) with this understanding.Number of theoretical plate calculates by chrysophanol and is not less than 3000.
3. the preparation of need testing solution
Get this product 1g under the weight differential item, the accurate title, decide, and puts in the 50ml conical flask, precision adds methanol 25ml, claims to decide weight, reflux 30 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, filter, precision is measured subsequent filtrate 5ml, put in the 50ml round-bottomed flask, fling to methanol, add 2.5mol/L sulfuric acid solution 10ml, supersound process 5 minutes adds chloroform 10ml again, reflux 1 hour, cooling moves in the separatory funnel, uses the minimum of chloroform washing container, incorporate in the separatory funnel, divide and get chloroform layer, acid solution chloroform extraction 2 times, each about 10ml, combined chloroform liquid is with anhydrous sodium sulfate dehydration, chloroform solution moves in the 100ml conical flask, flings to chloroform, and the residue precision adds methanol 10ml, claim to decide weight, put slight fever dissolved residue in the water-bath, put cold after, claim to decide weight again, supply the weight that subtracts mistake with methanol, shake up, filter, get subsequent filtrate, promptly.
4. detect the selection of wavelength
Use ultraviolet spectrophotometer (UV-2100) and measure the uv absorption spectra of emodin and chrysophanol reference substance, determining all has absorption maximum at 254nm, 292nm and 437nm place, and absorb maximum with 254nm wavelength place, this experiment has been carried out sample analysis at this wavelength place, baseline is steady, emodin and chrysophanol peak-to-peak shape are fine, separate fully with impurity peaks, so this experimental selection 254nm is for detecting the wavelength (see figure 1).
5. the standard curve and the range of linearity
It is an amount of that precision takes by weighing the emodin reference substance, makes the reference substance solution that contains emodin 0.004mg among every 1ml with methanol.Under above-mentioned chromatographic condition, accurate reference substance solution 5,10,15,20,25, the 30 μ l that draw, sample introduction is measured successively, and the result is as follows:
| Sample size (ug) | 20.35 | 40.70 | 61.05 | 81.4 | 101.75 | 122.1 |
| The peak area integrated value | 72013 | 148966 | 226922 | 305135 | 383851 | 463782 |
Learning by statistics and calculating recurrence side is Y=-7393.13333+3849.368901X, and r=0.9999 illustrates that chrysophanol is linear between 20～120 μ g.With the sample size is abscissa, and peak area value is a vertical coordinate, the drawing standard curve.Attached: emodin standard curve chromatogram (see figure 2)
It is an amount of that precision takes by weighing the chrysophanol reference substance, makes the reference substance solution that contains chrysophanol 0.008mg among every 1ml with methanol.Under above-mentioned chromatographic condition, accurate reference substance solution 5,10,15,20,25, the 30 μ l sample introduction mensuration successively of drawing, the result is as follows:
| Sample size (ug) | 40.8 | 81.6 | 122.4 | 163.2 | 204 | 244.8 |
| The peak area integrated value | 290990 | 610212 | 925717 | 1244946 | 1567656 | 1891149 |
Learning by statistics and calculating recurrence side is Y=-30790.6+7837.7843X, and r=0.9999 illustrates that chrysophanol is linear between 40～240 μ g.With the sample size is abscissa, and peak area value is a vertical coordinate, the drawing standard curve.Attached: chrysophanol standard curve chromatogram (see figure 3)
6. precision and repeatability
The precision test
6.1 get same need testing solution, continuous sample introduction 6 times is measured emodin, chrysophanol absworption peak area, the results are shown in Table 4:
Table 4 emodin Precision test result
| Chrysophanol 638,797 539,905 639,730 641,530 640,302 641894 RSD=0.18% |
| Emodin 349,902 353,018 360,720 366,190 369,205 351125 RSD=2.29% |
6.2 get same reference substance solution, continuous sample introduction 6 times is measured emodin, chrysophanol absworption peak area, the results are shown in Table 4:
| Chrysophanol 287,610 287,365 289,134 289,407 289,512 288944 RSD=0.32% |
| Emodin 70,741 70,601 70,483 71,006 70,890 71499 RSD=0.51% |
The repeatability test
Get 6 parts in same lot number sample, the accurate title, decide, and presses the determination operation.The results are shown in Table 5:
Table 5 reproducible test results
| Sampling amount (g) | Emodin content (mg/g) | Chrysophanol content (mg/g) | Emodin and chrysophanol summation (mg/g)/ |
| 1.0587 1.0412 1.0424 1.0438 1.1421 1.2044 meansigma methods RSD% | 0.4707 0.4640 0.4759 0.4596 0.4815 0.4990 0.4751 2.97 | 0.4937 0.5036 0.5054 0.5160 0.5101 0.5125 0.5069 1.6 | 0.9643 0.9677 0.9812 0.9755 0.9915 1.0115 0.98196 1.77 |
7. test sample stability test
Get same need testing solution, sample introduction in the different time, the stability of observing emodin, chrysophanol in the test sample, measurement result sees Table 6.
Table 6. test sample stability result
| Time (hour) | 0 | 6 | 9 | 12 | 15 | Meansigma methods | RSD(％) |
| Emodin (mg/g) chrysophanol (mg/g) | 29562510744 | 290738 512307 | 291074 513514 | 287539 514386 | 291324 510598 | 290047.4 512309.8 | 0.54 0.33 |
The result shows that the emodin in the test sample, chrysophanol are stable in 15 hours.
8. recovery test
Adopt the application of sample absorption method, get 6 parts in same sample, add a certain amount of emodin, chrysophanol reference substance respectively, measure emodin, the chrysophanol response rate in accordance with the law respectively, the results are shown in Table 7,8.
Table 7. emodin determination of recovery rates result
| Tested number | Sample weighing (g) | The former content of emodin (mg) | Add emodin amount (mg) | Measured value (mg) | The response rate (%) |
| 1 2 3 4 5 6 | 0.5348 0.5019 0.5192 0.5136 0.5397 0.5255 | 0.2541 0.2387 0.2438 0.2435 0.2565 0.2497 | 0.2545 0.2545 0.2545 0.2545 0.2545 0.2545 | 0.50201 0.48329 0.49282 0.49361 0.50039 0.49277 | 97.41 96.10 97.83 98.27 95.83 96.28 |
Average recovery rate 96.95% RSD 1.05%
Table 8. chrysophanol determination of recovery rates result
| Tested number | Sample weighing (g) | The former content of chrysophanol (mg) | Add chrysophanol amount (mg) | Measured value (mg) | Response rate % |
| 1 2 3 4 5 6 | 0.5348 0.5019 0.5192 0.5136 0.5397 0.5255 | 0.2711 0.2544 0.2632 0.2603 0.2736 0.2664 | 0.2545 0.2545 0.2545 0.2545 0.2545 0.2545 | 0.5343 0.5181 0.5285 0.5265 0.5394 0.5294 | 103.42 103.63 104.25 104.58 104.46 103.36 |
Average recovery rate 103.95% RSD 0.52%
9. the mensuration of sample
Get three batch samples respectively, measure in accordance with the law, calculate the content of emodin, chrysophanol, the results are shown in Table 9.
The measurement result of table 9. three batch samples
| Lot number | 050329 | 050330 | 050402 |
| Content (mg/ grain) | 0.5575 | 0.5497 | 0.5365 |
The total amount of emodin and chrysophanol is defined as and is no less than 0.5% in this product raw medicinal material Radix Et Rhizoma Rhei, the suitable 0.0755g Radix Et Rhizoma Rhei of every capsules in the prescription.The yield of this preparation technology conjunction type chrysophanic acid is about 68%, and the emodin in the finished product, chrysophanol content sum should be the 0.26mg/ grain, but considers the difference between pilot scale and big the production, and the content of Radix Et Rhizoma Rhei is with conjunction type emodin (C in tentative this product
15H
10O
5), chrysophanol (C
15H
10O
4) total amount counts per 1 and must not be less than 0.25mg.
Figure of description
Fig. 1 is the uv absorption spectra of emodin and chrysophanol reference substance.
Fig. 2 is an emodin standard curve chromatogram.
Fig. 3 is a chrysophanol standard curve chromatogram.
The specific embodiment
The present invention will be further described below in conjunction with embodiment.
Embodiment 1
(1) get Radix Et Rhizoma Rhei 50g pulverizing, use 60% alcohol reflux, reclaim ethanol, concentrate, drying gets dry extract, pulverizes, and sieves, and gets dry powder;
(2) Radix Saposhnikoviae 50g, Herba Schizonepetae 25g, Herba Menthae 50g, Herba Ephedrae 50g, Natrii Sulfas 50g, Fructus Gardeniae 25g, Talcum 300g, Radix Platycodonis 100g, Gypsum Fibrosum 100g, Rhizoma Chuanxiong 50g, Radix Angelicae Sinensis 50g, Radix Paeoniae Alba 50g, Radix Scutellariae 100g, Fructus Forsythiae 50g, Radix Glycyrrhizae 200g, Rhizoma Atractylodis Macrocephalae 25g ten Six-element medical materials add 6 times of water gagings extractions 1 time, it is standby to extract volatile oil simultaneously, the water extract filters precipitate with ethanol, filter, filtrate is concentrated, dry, get dry extract, pulverize, get dry powder;
(3) with above-mentioned two kinds of dry extract mix homogeneously (dry powder weight accounts for 37% in the capsule liquid), merge with volatile oil, add Semen Maydis oil 200g, ethyl cellulose 27g, fabaceous lecithin 7.73g, make suspension, be filled into soft capsule shell, make 1000.The total amount of emodin and chrysophanol is counted 0.25mg in every.
Embodiment 2
(1) get Radix Et Rhizoma Rhei 50g and pulverize, 70% ethanol percolate extraction,, collect 8 times and measure percolates, reclaim ethanol, concentrate, drying gets dry extract, pulverizes, and sieves, and gets dry powder;
(2) 8 times of water gagings extractions of all the other ten Six-element medical materials (weight is with embodiment 2) are 2 times, and it is standby to extract volatile oil simultaneously, and the filtration of decocting liquid merges, and is concentrated, and precipitate with ethanol filters, and filtrate is concentrated, dry, gets dry extract, pulverizes, and gets dry powder;
(3) with above-mentioned two kinds of dry extract mix homogeneously (dry powder weight accounts for 47% in the capsule liquid), merge with volatile oil, add salad oil 130g, Cera Flava 11.6 g, fabaceous lecithin 15.5g, Petiolus Trachycarpi oil 31g, make suspension, embedding is gone in the soft capsule shell, makes 1000.The total amount of emodin and chrysophanol is counted 0.3mg in every.
Embodiment 3
(1) gets Radix Et Rhizoma Rhei 50g and pulverize, measured 80% alcohol dipping 24 hours for 10 times; Impregnation liquid reclaims ethanol, concentrates, and drying gets dry extract, pulverizes, and sieves, and gets dry powder;
(2) 10 times of water gagings extractions of all the other ten Six-element medical materials (weight is with embodiment 2) are 2 times, and it is standby to extract volatile oil simultaneously, and the filtration of decocting liquid merges, and is concentrated, and precipitate with ethanol filters, and filtrate is concentrated, dry, gets dry extract, pulverizes, and gets dry powder;
(3) with above-mentioned two kinds of dry extract mix homogeneously (dry powder weight accounts for 53% in the capsule liquid), merge with volatile oil, adding Semen Maydis oil 60g, salad oil 100g, Cera Flava 7.73g, fabaceous lecithin 7.73g make suspension, and embedding is gone in the soft capsule shell, promptly.The total amount of emodin and chrysophanol is counted 0.29mg in every.
Embodiment 4
(1) get Radix Et Rhizoma Rhei 50g and pulverize, 60% ethanol percolate extraction is collected 8 times of amount percolates; Extracting solution reclaims ethanol, concentrates, and drying gets dry extract, pulverizes, and sieves, and gets dry powder;
(2) 8 times of water gagings extractions of all the other ten Six-element medical materials (weight is with embodiment 2) are 1 time, and it is standby to extract volatile oil simultaneously, and decocting liquid filters, and is concentrated, and precipitate with ethanol filters, and filtrate is concentrated, dry, gets dry extract, pulverizes, and gets dry powder;
(3) with above-mentioned two kinds of dry extract mix homogeneously (dry powder weight accounts for 42% in the capsule liquid), merge with volatile oil, add salad oil 200g, aluminum monostearate 20g, tween 80 7.73g, make suspension, embedding is gone in the soft capsule shell, promptly get every in the total amount of emodin and chrysophanol count 0.33mg.
Embodiment 5
(1) get Radix Et Rhizoma Rhei 50g and pulverize, measure 80% alcohol reflux for 6 times, extracting solution reclaims ethanol, concentrates, and drying gets dry extract, pulverizes, and sieves, and gets dry powder;
(2) 10 times of water gagings extractions of all the other ten Six-element medical materials (weight is with embodiment 2) are 1 time, and it is standby to extract volatile oil simultaneously, and decocting liquid filters, and is concentrated, and precipitate with ethanol filters, and filtrate is concentrated, dry, gets dry extract, pulverizes, and gets dry powder;
(3) with above-mentioned two kinds of dry extract mix homogeneously (dry powder weight accounts for 42% in the capsule liquid), merge with volatile oil, add salad oil 165g, Petiolus Trachycarpi oil 19.3g, Cera Flava 7.73g, soil temperature-60 11.6g, make suspension, embedding is gone in the soft capsule shell, that is, the total amount of emodin and chrysophanol is counted 0.36mg in every.
Embodiment 6
Emodin, chrysophanol assay:
(1) chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler; Methanol: 0.1% phosphoric acid solution is a mobile phase at 65: 35; Detect wavelength 254nm; Theoretical cam curve is calculated by the emodin peak should be not less than 3000;
(2) preparation of reference substance solution: precision takes by weighing emodin, each 5mg of chrysophanol reference substance, puts respectively in the 50ml measuring bottle, with dissolve with methanol and be diluted to scale and shake up; Precision is measured emodin solution 1ml, chrysophanol solution 2ml respectively, puts respectively in the 25ml measuring bottle, adds methanol to scale, shakes up, and, contains 4 μ g among the every 1ml of emodin that is, contains 8 μ g among the every 1ml of chrysophanol;
(3) preparation of need testing solution: get the soft capsule liquid 1g that embodiment 1 makes, the accurate title, decide, and puts in the 50ml conical flask, precision adds methanol 25ml, claims to decide weight, reflux 30 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, filter, precision is measured subsequent filtrate 5ml, put in the 50ml round-bottomed flask, fling to methanol, add 2.5mol/L sulfuric acid solution 10ml, supersound process 5 minutes adds chloroform 10ml again, reflux 1 hour, cooling moves in the separatory funnel, uses the minimum of chloroform washing container, incorporate in the separatory funnel, divide and get chloroform layer, acid solution chloroform extraction 2 times, each about 10ml, combined chloroform liquid is with anhydrous sodium sulfate dehydration, chloroform solution moves in the 100ml conical flask, flings to chloroform, and the residue precision adds methanol 10ml, claim to decide weight, put slight fever dissolved residue in the water-bath, put cold after, claim to decide weight again, supply the weight that subtracts mistake with methanol, shake up, filter, get subsequent filtrate, promptly;
(4) accurate respectively above-mentioned two kinds of reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly; Every of this product contains Radix Et Rhizoma Rhei with emodin (C
15H
10O
5) and chrysophanol (C
15H
10O
4) the total amount meter, must not be less than 0.25mg.
Claims (7)
1. the logical holy soft capsule of Radix Saposhnikoviae comprises capsule liquid, softgel shell, it is characterized in that the percentage by weight of each component in the capsule liquid is:
Medicinal substances extract 36%～53%
Substrate 43%～59%
Suspending agent 2%～7%
Wetting agent 2%～4%;
Wherein said substrate is one or more in Semen Maydis oil, salad oil, the Petiolus Trachycarpi oil; Suspending agent is one or more in Cera Flava, aluminum monostearate, the ethyl cellulose; Wetting agent is one or more in fabaceous lecithin, Tween-60, the tween 80;
Described medicinal substances extract is that Radix Et Rhizoma Rhei 50g, Radix Saposhnikoviae 50g, Herba Schizonepetae 25g, Herba Menthae 50g, Herba Ephedrae 50g, Natrii Sulfas 50g, Fructus Gardeniae 25g, Talcum 300g, Radix Platycodonis 100g, Gypsum Fibrosum 100g, Rhizoma Chuanxiong 50g, Radix Angelicae Sinensis 50g, Radix Paeoniae Alba 50g, Radix Scutellariae 100g, Fructus Forsythiae 50g, Radix Glycyrrhizae 200g, Rhizoma Atractylodis Macrocephalae 25g make through following method:
(1) get Radix Et Rhizoma Rhei and pulverize, with 6～10 times of amount 60%～80% ethanol extractions, extracting solution reclaims ethanol, concentrate, drying, dry extract, pulverize, sieve, get dry powder;
(2) after all the other ten Six-element pulverizing medicinal materials, the mixing, water extraction, it is standby to extract volatile oil simultaneously, and decocting liquid filters, merging, precipitate with ethanol filters, and filtrate is concentrated, dry, gets dry extract, pulverizes, and gets dry powder;
(3) above-mentioned two kinds of dry extract mix homogeneously and volatile oil combination system are got.
2. soft capsule as claimed in claim 1 is characterized in that the weight proportion of each component in the capsule liquid is:
Medicinal substances extract 42%～47%
Substrate 46%～51%
Suspending agent 2%～5%
Wetting agent 2%～4%.
Wherein said medicinal substances extract is that Radix Et Rhizoma Rhei 50g, Radix Saposhnikoviae 50g, Herba Schizonepetae 25g, Herba Menthae 50g, Herba Ephedrae 50g, Natrii Sulfas 50g, Fructus Gardeniae 25g, Talcum 300g, Radix Platycodonis 100g, Gypsum Fibrosum 100g, Rhizoma Chuanxiong 50g, Radix Angelicae Sinensis 50g, Radix Paeoniae Alba 50g, Radix Scutellariae 100g, Fructus Forsythiae 50g, Radix Glycyrrhizae 200g, Rhizoma Atractylodis Macrocephalae 25g make through following method:
(1) get Radix Et Rhizoma Rhei and pulverize, 70% ethanol percolate extraction is collected 8 times and is measured percolates, reclaims ethanol, concentrates, and drying gets dry extract, pulverizes, and sieves, and gets dry powder;
(2) after all the other ten Six-element pulverizing medicinal materials, the mixing, water extraction, it is standby to extract volatile oil simultaneously, and decocting liquid filters, merging, precipitate with ethanol filters, and filtrate is concentrated, dry, gets dry extract, pulverizes, and gets dry powder;
(3) above-mentioned two kinds of dry extract mix homogeneously and volatile oil combination system are got.
3. one kind prepares the method that the described Radix Saposhnikoviae of claim 1 is led to holy soft capsule, it is characterized in that comprising following process steps:
(1) get Radix Et Rhizoma Rhei and pulverize, with 6～10 times of amount 60%～80% ethanol extractions, extracting solution reclaims ethanol, concentrate, drying, dry extract, pulverize, sieve, get dry powder;
(2) after all the other ten Six-element pulverizing medicinal materials, the mixing, add 6～10 times of water gagings extractions 1～2 time, it is standby to extract volatile oil simultaneously, and decocting liquid filters, merging, and precipitate with ethanol filters, and filtrate is concentrated, dry, gets dry extract, pulverizes, and gets dry powder;
(3) with above-mentioned two kinds of dry extract mix homogeneously, merge with volatile oil, add adjuvant, make suspension, be filled into soft capsule shell, promptly.
4. preparation method as claimed in claim 3, wherein Radix Et Rhizoma Rhei adopts 60～80% ethanol refluxing processes to extract in the step (1).
5. preparation method as claimed in claim 3, wherein Radix Et Rhizoma Rhei adopts 60～80% alcohol dipping methods to extract in the step (1).
6. preparation method as claimed in claim 3, wherein Radix Et Rhizoma Rhei adopts 60～80% alcohol percolation methods to extract in the step (1).
7. the described Radix Saposhnikoviae of claim 1 is led to the content assaying method of holy soft capsule, it is characterized in that medicinal substances extract adopts emodin and chrysophanol in the quantitative determination of high-performance liquid Radix Et Rhizoma Rhei to comprise:
(1) chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler; Methanol: 0.1% phosphoric acid solution is a mobile phase at 65: 35; Detect wavelength 254nm; Theoretical cam curve is calculated by the emodin peak should be not less than 3000;
(2) preparation of reference substance solution: precision takes by weighing emodin, each 5mg of chrysophanol reference substance, puts respectively in the 50ml measuring bottle, with dissolve with methanol and be diluted to scale and shake up; Precision is measured emodin solution 1ml, chrysophanol solution 2ml respectively, puts respectively in the 25ml measuring bottle, adds methanol to scale, shakes up, and, contains 4 μ g among the every 1ml of emodin that is, contains 8 μ g among the every 1ml of chrysophanol;
(3) preparation of need testing solution: get this product 1g under the weight differential item, the accurate title, decide, and puts in the 50ml conical flask, precision adds methanol 25ml, claims to decide weight, reflux 30 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, filter, precision is measured subsequent filtrate 5ml, put in the 50ml round-bottomed flask, fling to methanol, add 2.5mol/L sulfuric acid solution 10ml, supersound process 5 minutes adds chloroform 10ml again, reflux 1 hour, cooling moves in the separatory funnel, uses the minimum of chloroform washing container, incorporate in the separatory funnel, divide and get chloroform layer, acid solution chloroform extraction 2 times, each about 10ml, combined chloroform liquid is with anhydrous sodium sulfate dehydration, chloroform solution moves in the 100ml conical flask, flings to chloroform, and the residue precision adds methanol 10ml, claim to decide weight, put slight fever dissolved residue in the water-bath, put cold after, claim to decide weight again, supply the weight that subtracts mistake with methanol, shake up, filter, get subsequent filtrate, promptly;
(4) accurate respectively above-mentioned two kinds of reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly; Every of this product contains Radix Et Rhizoma Rhei with emodin (C
15H
10O
5) and chrysophanol (C
15H
10O
4) the total amount meter, must not be less than 0.25mg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2006100144639A CN1895408B (en) | 2006-06-27 | 2006-06-27 | Radix saposhnikoviae Tong Sheng capsules, preparation and quality control method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2006100144639A CN1895408B (en) | 2006-06-27 | 2006-06-27 | Radix saposhnikoviae Tong Sheng capsules, preparation and quality control method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1895408A CN1895408A (en) | 2007-01-17 |
| CN1895408B true CN1895408B (en) | 2010-06-30 |
Family
ID=37608147
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2006100144639A Expired - Fee Related CN1895408B (en) | 2006-06-27 | 2006-06-27 | Radix saposhnikoviae Tong Sheng capsules, preparation and quality control method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1895408B (en) |
Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101480484B (en) * | 2008-01-11 | 2012-05-30 | 曾雄辉 | Method for preparing miraculous powder preparation of ledebouriella |
| CN101757188B (en) * | 2010-03-07 | 2012-02-01 | 杜贵胜 | Quick-healing paste for treating damp-heat type eczema and preparation method thereof |
| CN102894212B (en) * | 2012-08-27 | 2014-02-12 | 广东海大集团股份有限公司 | Anti-heat-stress Chinese herbal medicine composite feedstuff additive for meat duck |
| CN103142823A (en) * | 2013-03-20 | 2013-06-12 | 滨州医学院附属医院 | Chinese herbal medicine for treating eczema |
| CN103610796A (en) * | 2013-11-22 | 2014-03-05 | 安徽天恒药业有限公司 | Traditional Chinese medicinal composition for treating exfoliative inflammation of lips |
| CN104435231A (en) * | 2014-11-05 | 2015-03-25 | 烟台天正药业有限公司 | Method for preparing medicine preparation named Fangfengtongsheng |
| CN105617120A (en) * | 2016-03-31 | 2016-06-01 | 杨登新 | Traditional Chinese medicine preparation for treating external cold and internal heat type cold and preparation method of traditional Chinese medicine preparation |
| CN105675765A (en) * | 2016-04-15 | 2016-06-15 | 广西壮族自治区梧州食品药品检验所 | Determination method for prim-O-glucosylcimifugin and 5-O-methylvisammioside in radix saposhnikoviae |
| CN105929087A (en) * | 2016-04-15 | 2016-09-07 | 广西壮族自治区梧州食品药品检验所 | Method for separating prim-o-glucosylcimifugin and 5-o-methylvisammioside from saposhnikovia divaricata |
| CN105699542A (en) * | 2016-04-22 | 2016-06-22 | 广西壮族自治区梧州食品药品检验所 | Method for measuring cimicifugoside, cimifugin, sec-o-glucosylhamaudol and 5-O-methylvisammioside in divaricate saposhnikovia roots |
| CN105929089A (en) * | 2016-04-22 | 2016-09-07 | 广西壮族自治区梧州食品药品检验所 | Method for extracting cimicifugoside, cimicifugin, sec-o-glucosylhamaudol and 5-O-methylvisammioside in divaricate saposhnikovia root |
| CN114252532B (en) * | 2021-01-26 | 2023-12-26 | 山东祥隆医药研究院有限公司 | Method for establishing fingerprint of Fangfengsheng particles and fingerprint thereof |
-
2006
- 2006-06-27 CN CN2006100144639A patent/CN1895408B/en not_active Expired - Fee Related
Non-Patent Citations (3)
| Title |
|---|
| 国家药典委员会.国家药品标准 中药成方制剂第15册.国家药典委员会,1998,78. * |
| 范碧亭.中药药剂学 1997年版.上海科学技术出版社,1997,355-358. |
| 范碧亭.中药药剂学 1997年版.上海科学技术出版社,1997,355-358. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1895408A (en) | 2007-01-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1895408B (en) | Radix saposhnikoviae Tong Sheng capsules, preparation and quality control method thereof | |
| CN102657823B (en) | Traditional Chinese medicine composition with anticancer effect and preparation method and detection method thereof | |
| CN102091168A (en) | Quality control method for Chinese medicine preparation Xuefuzhuyu capsule | |
| CN100581582C (en) | Compound oral taking preparation of cantharis, and preparation method | |
| CN101496870B (en) | Chinese medicinal composition for resolving phlegm and suppressing cough as well as preparation method and quality control method thereof | |
| CN102749401A (en) | Quality inspection method of traditional Chinese medicine composition twenty-five-ingredient lung disease preparation | |
| CN100475239C (en) | Quality control method of heart pulse free flow oral preparation | |
| CN102539599B (en) | Method for detecting liver-enhancing medicine | |
| CN101690757B (en) | Method for preparing bezoar supernatant preparations | |
| CN102068598B (en) | Quality control method of Yangrong Baicao Wan for treating irregular menses caused by hemophthisis | |
| CN103191289A (en) | Synchronous preparation method of four effective parts in medicine pair of common anemarrhena rhizome and amur corktree bark and application thereof | |
| CN102688336A (en) | Bezoar supernatant composite and preparation method thereof | |
| CN103099788A (en) | Traditional Chinese medicine composite decoration from powder, preparation and decoction methods and dosage relation thereof | |
| CN101342230A (en) | Radix astragali particle and quality control method thereof | |
| CN1857445B (en) | Quality control method for Desheng preparation | |
| CN102357131A (en) | Method for preparing astragalus polysaccharide glucose-lowering capsule | |
| CN102590423B (en) | Fingerprint spectrum determination method of ligusticum wallichii tea-blending granular preparation | |
| CN101642492B (en) | Drug for treating chronic pelvic inflammatory disease and preparation method thereof | |
| CN101716270A (en) | Method for detecting quality of traditional Chinese herbal medicament compound preparation for invigorating blood and regulating menses | |
| CN107648424A (en) | A kind of preparation method of Lycium-rehmannia preparation | |
| CN100432670C (en) | Method for inspecting Chinese-medicinal preparation Kaiyinwan | |
| CN1970070A (en) | Oral administered formulation for reducing fat and expelling toxins, preparation process and quality control method thereof | |
| CN101444571A (en) | Jiuweiqianghuo soft capsule and preparation method thereof | |
| CN100515476C (en) | Compound capsule with pseudo-ginseng and Chinese fanpalm seed, its preparation process and quality control method | |
| CN103316074A (en) | Medicine composite of halenia corni extract, astragalus extract and liquorice extract as well as preparation and application of medicine composite |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20100630 Termination date: 20120627 |