CN101224245A - Quality controlling method of Chinese traditional medicine for treating gynecology inflammation - Google Patents
Quality controlling method of Chinese traditional medicine for treating gynecology inflammation Download PDFInfo
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Abstract
The invention discloses a quality control method for traditional Chinese medicine preparation, in particular to a quality control method of penyanjing capsule used for treatment of gynecological inflammation. The quality control method of the invention controls the quality of the product effectively by differentiating or assaying one or a plurality of crude medicines of dandelion, rhizoma cibotii and radices paeoniae rubra in the prescription. The invention has the advantages that the differentiation and assay of a plurality of the crude medicines in the prescription guarantees effectively the effect and stability of the penyanjing capsule produced so as to better ensure the safety of medication for sufferers.
Description
Technical field:
The present invention relates to a kind of method of quality control of Chinese medicine preparation, relate in particular to a kind of method of quality control for the treatment of the Chinese medicine preparation of gynecological inflammation.
Background technology:
The United Nations's health organization authority statistical data shows: 75% women, just meet with all kinds of gynaecopathia, wherein especially with all kinds of gynecological inflammations for, gently then cause leucorrhoea grow in quantity, pruritus, variable color, stench, waist abdomen to ache, heavy then cause hysteromyoma, ovarian cyst, infertile, even develop into serious diseases such as cervical cancer.Common pathogenic bacterium have mycete (fungus), virus, chlamydia, infusorian, antibacterial, mycoplasma etc.Just because of this, so occurred the class medication of miscellaneous gynecological on the market.How nature guarantees that the safety of patient's medication has become a problem that can not look down upon with effectiveness and quality controllability.Consider the research that we have carried out at a kind of Chinese medicine preparation for the treatment of gynecological inflammation is the method for quality control of PENYANJING JIAONANG just for this.
Summary of the invention:
The purpose of this invention is to provide a kind of method of quality control for the treatment of the Chinese medicine preparation of gynecological inflammation, it is the method for quality control by the prepared PENYANJING JIAONANG of crude drug Caulis Lonicerae, Caulis Spatholobi, Rhizoma Cibotii, Herba Taraxaci, Herba Leonuri, Herba Plantaginis, Radix Paeoniae Rubra, Rhizoma Chuanxiong, better guarantee the stability of medicine with this, quality controllability makes medication safer, effective.
The objective of the invention is to realize by the following technical solutions, comprise following discriminating and/or assay:
The discriminating of Herba Taraxaci
Get this product, inclining content, porphyrize, get 1-4g, add methanol 15-45ml, reflux 15-45 minute, filter, filtrate is put evaporate to dryness in the water-bath, and residue adds water 10-30ml makes dissolving, put in the separatory funnel, add chloroform and extract secondary, each 10-30ml, combined chloroform liquid, put evaporate to dryness in the water-bath, residue adds chloroform 0.5-1.5ml makes dissolving, as need testing solution; Other gets Herba Taraxaci control medicinal material 1-3g, shines medical material solution in pairs with legal system; Get other medical materials except that Herba Taraxaci in the prescription ratio again, make negative sample, make negative solution with the need testing solution preparation method by preparation technology.According to thin layer chromatography test, draw each 5-15 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with the chloroform, launch, take out, dry, spray 5-15% ethanol solution of sulfuric acid, put 105 ℃ dry by the fire to the speckle colour developing clear.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.Check three batch samples all up to specification, negative solution is noiseless, the results are shown in Figure of description 1.
The discriminating of Rhizoma Cibotii
Get this product, inclining content, porphyrize, get 1-4g, add methanol 15-45ml, reflux 15-45 minute, filter, filtrate is put evaporate to dryness in the water-bath, and residue adds water 20ml makes dissolving, put in the separatory funnel, add the ethyl acetate extraction secondary, each 10-30ml, merge ethyl acetate liquid, put evaporate to dryness in the water-bath, residue adds ethyl acetate 1ml makes dissolving, as need testing solution; In addition get other medical materials except that Rhizoma Cibotii, make negative sample, make negative solution with the need testing solution preparation method by preparation technology in the prescription ratio; Get Rhizoma Cibotii control medicinal material 0.5-1.5g again, add water 25-75ml, boiled 15-45 minute, put cold, filter, filtrate adds the ethyl acetate extraction secondary, and each 10-30ml merges ethyl acetate liquid, put evaporate to dryness in the water-bath, residue adds ethyl acetate 0.5-1.5ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography, draw each 2.5-7.5 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction-ethyl acetate-formic acid (2.5-7.5: 1-4: 0.05-0.15) be developing solvent, launch, take out, dry, spray is with the acid ferric chloride alcoholic solution of 2.5-7.5% hydrochloric acid, put 105 ℃ dry by the fire to the speckle colour developing clear.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.Check three batch samples all up to specification, and negative solution is noiseless, the results are shown in Figure of description 2.
Assay
The main constituent of Radix Paeoniae Rubra medical material is a peoniflorin in the PENYANJING JIAONANG, and concrete test method and result are as follows:
(1) instrument and reagent
High performance liquid chromatograph;
(2) reagent
Methanol is chromatorgaphy reagent; Water is redistilled water; Other reagent is analytical pure;
(3) reference substance
Peoniflorin: Nat'l Pharmaceutical ﹠ Biological Products Control Institute provides, and uses (lot number 0736-200116) for assay;
(4) chromatographic condition
Chromatographic column: C
18(Yi Lite 200 * 4.6mm, 5 μ m)
Mobile phase: methanol-water (22: 78)
Detect wavelength: 230nm
Flow velocity: 1.0ml/min
(5) preparation of need testing solution
With reference to " content assaying method of a Radix Paeoniae Rubra medical material of Chinese pharmacopoeia version in 2000, employing methanol is solvent.Because the Radix Paeoniae Rubra medical material is handled through water extract-alcohol precipitation in the finished product preparation, so need not soak for test agent, directly the solubilizer supersound process gets final product, and only extraction time is studied;
Get 10 of this product (021210 batch), inclining content, and accurate the title decides, porphyrize is got three parts of each about 0.25g of fine powder, and accurate the title decides, put in the tool plug triangular flask, the accurate methanol 25ml that adds claims to decide weight, supersound process (power 200W, frequency 40KHz) is 20,40,60 minutes respectively, puts cold, add methanol and supply the weight that subtracts mistake, shake up, filter, get subsequent filtrate, measure, the results are shown in Table 1 by above-mentioned chromatographic condition;
The content comparison sheet of table 1 different extraction times
| Extraction time (min) | 20 | 40 | 60 |
| Content (mg/ grain) | 1.86 | 2.32 | 2.32 |
The above results shows: this product supersound process 40 minutes, peoniflorin are extracted fully substantially, are 40 minutes so determine this product extraction time.The need testing solution compound method is as follows:
Get 10 of this product, inclining content, and accurate the title decides, porphyrize is got the about 0.25g of fine powder, and accurate the title decides, put in the tool plug triangular flask, the accurate methanol 25ml that adds claims to decide weight, supersound process (power 200W, frequency 40KHz) 40 minutes is put cold, add methanol and supply the weight that subtracts mistake, shake up, filter, get subsequent filtrate, promptly;
(6) preparation of negative solution
Take by weighing other medical materials except that Radix Paeoniae Rubra in the prescription ratio, make negative sample, make negative solution by the need testing solution compound method again according to preparation technology;
(7) preparation of reference substance solution
It is an amount of that precision takes by weighing the peoniflorin reference substance, adds methanol and make the solution that contains 0.0618mg among every 1ml, shakes up, promptly;
(8) algoscopy
Accurate each the 5 μ l of reference substance solution, negative solution and need testing solution that draw inject chromatograph of liquid, measure, and calculate, promptly;
Measure reference substance solution, negative solution, need testing solution under these conditions, the record chromatogram, the result shows that the separating degree at peoniflorin peak and adjacent chromatographic peak in the test sample is greater than 1.5, number of theoretical plate is greater than 1500 (pressing the peoniflorin peak calculates), and negative solution is interference measurement not, and the result sees Figure of description 3,4,5 respectively;
(9) linear relationship test
Precision takes by weighing peoniflorin reference substance 12.36mg, puts in the 100ml measuring bottle, adds methanol and makes dissolving in right amount, and add methanol to scale, shakes up (0.1236g/ml). Accurate absorption 1,3,5,7,9ml put respectively in the 10ml measuring bottle, add methanol and are diluted to scale, shake up, make the solution of 0.01236mg/ml, 0.03708mg/ml, 0.0618mg/ml, 0.08652mg/ml, a series of concentration of 0.11124mg/ml, get 5 μ l respectively, inject high performance liquid chromatograph, measure, (μ g) is abscissa with sample size, and peak area is a vertical coordinate, the preparation standard curve, regression equation is: Y=18254376.2X+5213.5, r=0.9999.The results are shown in Table 2;
Table 2 linear relationship is investigated table as a result
| Sample size (μ g) | 0.0618 | 0.1854 | 0.309 | 0.4326 | 0.5562 |
| Peak area value | 1134637 | 3366768 | 5651100 | 7954697 | 10121877 |
Peoniflorin is good in 0.0618～0.5562 μ g scope internal linear relation;
(10) precision test
Accurate draw with a need testing solution (lot number: 021210) 5 μ l, inject chromatograph of liquid, replication 5 times the results are shown in Table 3;
Table 3 Precision test result table
Precision is good;
(11) stability test
At room temperature the same a need testing solution (021210) of Fang Zhiing was drawn 5 μ l respectively at 0,2,4,6,10 hour, injected chromatograph of liquid, measured, and the results are shown in Table 4;
Table 4 stability test is table as a result
| Time (h) | 0 | 2 | 4 | 6 | 10 |
| Peak area value | 4954324 | 5009448 | 4977496 | 4959955 | 5023225 |
Need testing solution peak area value in 10 hours does not have change substantially, illustrates that this product solution is stable in 10 hours;
(12) repeatability test
Get same batch sample (021212) and press method under the assay item, measure 5 times (n=2), the results are shown in Table 5;
Table 5 replica test is table as a result
Average content is the 2.3199mg/ grain, i.e. 5.2927mg/g, favorable reproducibility;
(13) recovery test
Precision take by weighing the sample of measuring content (021212 batch, 5.2927mg/g) 0.125g, accurate respectively peoniflorin reference substance solution (0.0695mg/ml) 10ml that adds, be 0.695mg, the accurate again methanol 15ml that adds measures by above-mentioned content assaying method, calculate recovery rate the results are shown in Table 6;
Table 6 determination of recovery rates is table as a result
Average recovery is good;
(14) sample determination result
Measure ten batch samples by the content assaying method of drafting, the results are shown in Table 7;
Table 7 sample size measurement result table
| Lot number | 021210 | 021212 | 021214 | 021216 | 030110 |
| Content (mg/ grain) | 2.36 | 2.32 | 2.36 | 2.30 | 2.41 |
| Lot number | 030112 | 030114 | 040801 | 040803 | 040805 |
| Content (mg/ grain) | 2.35 | 2.37 | 2.81 | 2.84 | 2.82 |
After comparing with reference substance solution, sample peoniflorin peak shape and retention time and reference substance solution are close, and negative sample is noiseless.After " content of different extraction times relatively ", " linear relationship experiment ", " precision experiment ", " stability experiment ", " repeatability test ", " response rate experiment " and " the synthesis measuring tests of ten batch samples ", prove that this method specificity is strong, exactly content of paeoniflorin in the working sample.
The PENYANJING JIAONANG that meets quality standard of the present invention has following drug effect:
Have significant antiinflammatory action, and escherichia coli, bacillus pyocyaneus, streptococcus, micrococcus luteus, golden staphylococci and anaerobe, product melanin bacillus are had bacteriostasis, toxicologic study proves that this medicine belongs to avirulence Chinese medicine.PENYANJING JIAONANG can suppress mice auricle swelling and the granulomatous hamartoplasia of rat agar significantly.Because of the Caulis Lonicerae in this medicine, Caulis Spatholobi, Rhizoma Cibotii, Herba Taraxaci, Radix Paeoniae Rubra are broad-spectrum antiseptic Chinese medicine, experimental results show that, PENYANJING JIAONANG can suppress the growth that escherichia coli, bacillus pyocyaneus, streptococcus, micrococcus luteus, golden staphylococci and anaerobe are produced the melanin bacillus, and its MIC is being equivalent to crude drug in whole 6.25-3.12mg/ml.And acute toxicity and long term toxicity test prove that also this medicine belongs to avirulence Chinese medicine,
Concrete experimental result is as follows:
1, long term toxicity test: healthy rat 60 (male and female half and half, body weight 116 ± 12g), continuous use 32 days, rat behavior activity therebetween, diet, defecation are normal, weight increase, the rat eye socket is got hematometry hematology and blood biochemical index after the drug withdrawal, through significance test difference there are no significant meaning, the result shows that successive administration has no side effect to rat;
2, to the inhibitory action of mice auricle swelling: PENYANJING JIAONANG can suppress the swelling of Mice Auricle significantly, and the effect of high dose group and aspirin group are approximate, and its inhibitory action is dose-effect relationship;
3, to the antiinflammatory action of rat granuloma model: PENYANJING JIAONANG can suppress rat agar granulation tissue hyperplasia significantly, and its antiinflammatory action is dose-effect relationship;
4, acute toxicity testing: 20 of healthy mices (male and female half and half, body weight 17-20g), to observe 7 days after the medication, equal healthy survival, hair color, activity, diet and defecation are all normal, weight increase;
5, to pelvic inflammatory disease common pathogen and anaerobe sensitive experiment: PENYANJING JIAONANG is produced the melanin bacillus to escherichia coli, bacillus pyocyaneus, streptococcus, micrococcus luteus, golden staphylococci and anaerobe bacteriostasis, general minimum inhibitory concentration (MIC) 6.25-3.12mg/ml (being equivalent to crude drug in whole).
The invention has the advantages that can be by to the discriminating and the assay of plurality of raw materials medicine in the prescription, guarantees the drug effect and the stability of the PENYANJING JIAONANG produced effectively, thereby can protect the safety of extensive patients medication better.
Specific embodiment
The discriminating of specific embodiment one Herba Taraxaci
Get this product, inclining content, porphyrize, get 3g, add methanol 30ml, reflux 30 minutes, filter, filtrate is put evaporate to dryness in the water-bath, and residue adds water 20ml makes dissolving, put in the separatory funnel, add chloroform and extract secondary, each 20ml, combined chloroform liquid, put evaporate to dryness in the water-bath, residue adds chloroform 1ml makes dissolving, as need testing solution; Other gets Herba Taraxaci control medicinal material 2g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography, drawing each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with the chloroform, launch, take out, dry, spray 10% ethanol solution of sulfuric acid, put 105 ℃ dry by the fire to speckle colour developing clear, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
Check three batch samples all up to specification, negative solution is noiseless.
The discriminating of specific embodiment two Rhizoma Cibotii
Get this product, inclining content, porphyrize, get 3g, add methanol 30ml, reflux 30 minutes, filter, filtrate is put evaporate to dryness in the water-bath, and residue adds water 20ml makes dissolving, put in the separatory funnel, add the ethyl acetate extraction secondary, each 20ml, merge ethyl acetate liquid, put evaporate to dryness in the water-bath, residue adds ethyl acetate 1ml makes dissolving, as need testing solution; Get Rhizoma Cibotii control medicinal material 1g again, add water 50ml, boiled 30 minutes, put coldly, filter, filtrate adds the ethyl acetate extraction secondary, each 20ml merges ethyl acetate liquid, puts evaporate to dryness in the water-bath, residue adds ethyl acetate 1ml makes dissolving, medical material solution according to the thin layer chromatography test, is drawn each 5 μ l of above-mentioned two kinds of solution in contrast, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction-ethyl acetate-formic acid (5: 3: 0.1) is developing solvent, launches, and takes out, dry, spray is with the acid ferric chloride alcoholic solution of 5% hydrochloric acid, put 105 ℃ dry by the fire to the speckle colour developing clear, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
Check three batch samples all up to specification, and negative solution is noiseless.
Specific embodiment three
Assay is according to high effective liquid chromatography for measuring;
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler, is mobile phase with methanol 22 water 78; The detection wavelength is 230nm, and theoretical cam curve is calculated by peoniflorin should be not less than 1500;
The preparation of reference substance solution, it is an amount of to get the peoniflorin reference substance, adds methanol and makes the solution that contains 0.06mg among every 1ml, promptly;
The preparation of need testing solution: get this product, inclining content, and accurate the title decided porphyrize, get the about 0.25g of fine powder, the accurate title, decide, and puts in the tool plug triangular flask, the accurate methanol 25ml that adds claims to decide weight, supersound process, power 200W, frequency 40KHz, 40 minutes, put coldly, add methanol and supply the weight that subtracts mistake, shake up, filter, get subsequent filtrate, promptly;
Algoscopy: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject chromatograph of liquid, measure.
Description of drawings:
1, (1) Fig. 1 is the thin layer chromatography photo of dandelion; 1. negative among the figure, be sample, 4. control medicinal material 2., 3., 5..
(2) Fig. 2 is the thin layer chromatography photo of Rhizoma Cibotii; 1. negative among the figure, be sample, 4. control medicinal material 2., 3., 5..
(3) Fig. 3 is the reference substance sample high performance liquid chromatogram figure that paeoniflorin content is measured in the PENYANJING JIAONANG Radix Paeoniae Rubra.
(4) Fig. 4 is the negative sample high performance liquid chromatogram figure that paeoniflorin content is measured in the PENYANJING JIAONANG Radix Paeoniae Rubra.
(5) the test sample sample high performance liquid chromatogram figure that paeoniflorin content is measured in Fig. 5 PENYANJING JIAONANG Radix Paeoniae Rubra.
2, (1) Fig. 1 and Fig. 2 can show in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color, and negative solution is noiseless, illustrates that this method is feasible, can control drug quality.
(2) Fig. 3, Fig. 4, Fig. 5 show that after comparing with reference substance solution, sample Paeoniflorin peak shape and retention time and reference substance solution are close, and negative sample is noiseless, prove that the method specificity is strong, exactly the content of Paeoniflorin in the working sample.
3, Fig. 1 and Fig. 2 must express with cromogram.
Claims (8)
1. method of quality control for the treatment of the Chinese medicine preparation of gynecological inflammation, this Chinese medicine preparation is prepared by crude drug Caulis Lonicerae, Caulis Spatholobi, Rhizoma Cibotii, Herba Taraxaci, Herba Leonuri, Herba Plantaginis, Radix Paeoniae Rubra, Rhizoma Chuanxiong, it is characterized in that by the thin layer chromatography of Herba Taraxaci and/or Rhizoma Cibotii is differentiated and/or Radix Paeoniae Rubra in the high-efficient liquid phase technique assay of peoniflorin carry out quality control.
2. a kind of method of quality control for the treatment of the Chinese medicine preparation of gynecological inflammation as claimed in claim 1 is characterized in that described Chinese medicine preparation is a PENYANJING JIAONANG.
3. a kind of method of quality control for the treatment of the Chinese medicine preparation of gynecological inflammation as claimed in claim 1, the thin layer chromatography that it is characterized in that its used Herba Taraxaci are to realize controlling the purpose of drug quality by implementing following concrete discrimination method:
The discriminating of Herba Taraxaci
Get this product, inclining content, porphyrize, get 1-4g, add methanol 15-45ml, reflux 15-45 minute, filter, filtrate is put evaporate to dryness in the water-bath, and residue adds water 10-30ml makes dissolving, put in the separatory funnel, add chloroform and extract secondary, each 10-30ml, combined chloroform liquid, put evaporate to dryness in the water-bath, residue adds chloroform 0.5-1.5ml makes dissolving, as need testing solution; Other gets Herba Taraxaci control medicinal material 1-3g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography, drawing each 5-15 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with the chloroform, launch, take out, dry, spray 5-15% ethanol solution of sulfuric acid, put 105 ℃ dry by the fire to speckle colour developing clear, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
4. a kind of method of quality control for the treatment of the Chinese medicine preparation of gynecological inflammation as claimed in claim 3, the thin layer chromatography that it is characterized in that its used Herba Taraxaci are to realize controlling the purpose of drug quality by implementing following concrete discrimination method:
The discriminating of Herba Taraxaci
Get this product, inclining content, porphyrize, get 3g, add methanol 30ml, reflux 30 minutes, filter, filtrate is put evaporate to dryness in the water-bath, and residue adds water 20ml makes dissolving, put in the separatory funnel, add chloroform and extract secondary, each 20ml, combined chloroform liquid, put evaporate to dryness in the water-bath, residue adds chloroform 1ml makes dissolving, as need testing solution; Other gets Herba Taraxaci control medicinal material 2g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography, drawing each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with the chloroform, launch, take out, dry, spray 10% ethanol solution of sulfuric acid, put 105 ℃ dry by the fire to speckle colour developing clear, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
5. a kind of according to claim 1 method of quality control for the treatment of the Chinese medicine preparation of gynecological inflammation, the thin layer chromatography that it is characterized in that its used Rhizoma Cibotii are by implementing the purpose that following discriminating realizes controlling drug quality:
The discriminating of Rhizoma Cibotii
Get this product, inclining content, porphyrize, get 1-4g, add methanol 15-45ml, reflux 15-45 minute, filter, filtrate is put evaporate to dryness in the water-bath, and residue adds water 20ml makes dissolving, put in the separatory funnel, add the ethyl acetate extraction secondary, each 10-30ml, merge ethyl acetate liquid, put evaporate to dryness in the water-bath, residue adds ethyl acetate 1ml makes dissolving, as need testing solution; Get Rhizoma Cibotii control medicinal material 0.5-1.5g again, add water 25-75ml, boiled 15-45 minute, and put coldly, filter, filtrate adds the ethyl acetate extraction secondary, each 10-30ml merges ethyl acetate liquid, puts evaporate to dryness in the water-bath, residue adds ethyl acetate 0.5-1.5ml makes dissolving, medical material solution according to the thin layer chromatography test, is drawn each 2.5-7.5 μ l of above-mentioned two kinds of solution in contrast, put respectively on same silica gel g thin-layer plate, 0.05-0.15 is developing solvent with cyclohexane extraction 2.5-7.5-ethyl acetate 1-4 formic acid, launches, and takes out, dry, spray is with the acid ferric chloride alcoholic solution of 2.5-7.5% hydrochloric acid, put 105 ℃ dry by the fire to the speckle colour developing clear, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
6. as a kind of method of quality control for the treatment of the Chinese medicine preparation of gynecological inflammation as described in the claim 5, the thin layer chromatography that it is characterized in that its used Rhizoma Cibotii is by implementing the purpose that following discriminating realizes controlling drug quality:
The discriminating of Rhizoma Cibotii
Get this product, inclining content, porphyrize, get 3g, add methanol 30ml, reflux 30 minutes, filter, filtrate is put evaporate to dryness in the water-bath, and residue adds water 20ml makes dissolving, put in the separatory funnel, add the ethyl acetate extraction secondary, each 20ml, merge ethyl acetate liquid, put evaporate to dryness in the water-bath, residue adds ethyl acetate 1ml makes dissolving, as need testing solution; Get Rhizoma Cibotii control medicinal material 1g again, add water 50ml, boiled 30 minutes, put coldly, filter, filtrate adds the ethyl acetate extraction secondary, each 20ml merges ethyl acetate liquid, puts evaporate to dryness in the water-bath, residue adds ethyl acetate 1ml makes dissolving, medical material solution according to the thin layer chromatography test, is drawn each 5 μ l of above-mentioned two kinds of solution in contrast, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction-ethyl acetate-formic acid (5: 3: 0.1) is developing solvent, launches, and takes out, dry, spray is with the acid ferric chloride alcoholic solution of 5% hydrochloric acid, put 105 ℃ dry by the fire to the speckle colour developing clear, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
7. as the described a kind of method of quality control for the treatment of the Chinese medicine preparation of gynecological inflammation of claim 1-6, it is characterized in that it adopts following method to realize to content of paeoniflorin mensuration in the Radix Paeoniae Rubra:
Assay is according to high effective liquid chromatography for measuring;
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler, is mobile phase with methanol 12～32-water 68～88; The detection wavelength is 220～240nm, and theoretical cam curve is calculated by the peoniflorin peak should be not less than 1500;
The preparation of reference substance solution: it is an amount of to get the peoniflorin reference substance, adds methanol and makes the solution that contains 0.01～0.1mg among every 1ml, promptly;
The preparation of need testing solution: get this product, inclining content, and accurate the title decided porphyrize, get the about 0.1～0.5g of fine powder, the accurate title, decide, and puts in the tool plug triangular flask, the accurate methanol 10～50ml that adds claims to decide weight, supersound process, power 200W, frequency 40KHz, 30～50 minutes, put coldly, add methanol and supply the weight that subtracts mistake, shake up, filter, get subsequent filtrate, promptly;
Algoscopy: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject chromatograph of liquid, measure.
8. a kind of method of quality control for the treatment of the Chinese medicine preparation of gynecological inflammation as claimed in claim 7 is characterized in that it adopts following method that content of paeoniflorin in the Radix Paeoniae Rubra is measured:
Assay is according to high effective liquid chromatography for measuring;
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler, is mobile phase with methanol 22-water 78; The detection wavelength is 230nm, and theoretical cam curve is calculated by the peoniflorin peak should be not less than 1500;
The preparation of reference substance solution, it is an amount of to get the peoniflorin reference substance, adds methanol and makes the solution that contains 0.06mg among every 1ml, promptly;
The preparation of need testing solution: get this product, inclining content, and accurate the title decided porphyrize, get the about 0.25g of fine powder, the accurate title, decide, and puts in the tool plug triangular flask, the accurate methanol 25ml that adds claims to decide weight, supersound process, power 200W, frequency 40KHz, 40 minutes, put coldly, add methanol and supply the weight that subtracts mistake, shake up, filter, get subsequent filtrate, promptly;
Algoscopy: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject chromatograph of liquid, measure.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102846870A (en) * | 2012-08-23 | 2013-01-02 | 何兆辉 | External anti-inflammatory drug from the Miao nationality and production process thereof |
| CN103149319A (en) * | 2013-03-05 | 2013-06-12 | 西安碑林药业股份有限公司 | Quality detection method for Chinese herbal preparation with effects of stimulating circulation of blood and causing muscles and joints to relax and activating blood circulation and dissipating blood stasis |
| CN105424833A (en) * | 2015-11-23 | 2016-03-23 | 江苏康缘药业股份有限公司 | Component test method of FKIV granules |
| CN106420974A (en) * | 2016-09-23 | 2017-02-22 | 毛里夏里甫·哈帕 | Fumigation preparation for treating gynopathy, preparing method and application method |
-
2007
- 2007-10-29 CN CNA2007100359832A patent/CN101224245A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102846870A (en) * | 2012-08-23 | 2013-01-02 | 何兆辉 | External anti-inflammatory drug from the Miao nationality and production process thereof |
| CN103149319A (en) * | 2013-03-05 | 2013-06-12 | 西安碑林药业股份有限公司 | Quality detection method for Chinese herbal preparation with effects of stimulating circulation of blood and causing muscles and joints to relax and activating blood circulation and dissipating blood stasis |
| CN105424833A (en) * | 2015-11-23 | 2016-03-23 | 江苏康缘药业股份有限公司 | Component test method of FKIV granules |
| CN106420974A (en) * | 2016-09-23 | 2017-02-22 | 毛里夏里甫·哈帕 | Fumigation preparation for treating gynopathy, preparing method and application method |
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