CN100391532C - Ointment of treating dysmenorrhea, its preparing method and quality control method - Google Patents
Ointment of treating dysmenorrhea, its preparing method and quality control method Download PDFInfo
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Abstract
The present invention provides an ointment for treating dysmenorrhoea, a preparation method and a quality control method of the ointment, and the ointment is prepared from 200g of medicinal evodia fruit, 200g of corydalis tuber, 1000g of dried ginger and 1200g of turmeric root tuber. Compared with the prior art, the ointment of the present invention has the advantages of simple prescription, convenient preparation and use, obvious treatment effect, obvious effect, short course of treatment and no side effect, and furthermore, the ointment is suitable for various patients. The provided quality control method has the advantages of high precision, good reproducibility and exact measurement result, and furthermore, the quality control method effectively guarantees the clinical treatment effect of the ointment.
Description
Technical field:
The present invention relates to a kind of ointment for the treatment of dysmenorrhea and preparation method and method of quality control, belong to technical field of Chinese medicines.
Background technology:
Dysmenorrhea is a common gynecological disease, not only makes the patient suffer misery on the health, but also has influence on patient's work and life.If dysmenorrhea can not get effective treatment, also might cause other body illness.Present therapeutic scheme generally adopts Western medicine or treatment by Chinese herbs, and the western medicine time is short, and curative effect is fast, but western medicine is just at symptom, outbreak repeatedly easily can not thoroughly improve the phenomenon of dysmenorrhea after the treatment, and Western medicine repeatedly use can cause bigger side effect.Treatment by Chinese herbs can be from basic solution dysmenorrhea problem, and side effect is little, thereby is subjected to patient's welcome, but most Chinese medicine is longer the general course of treatment, and taking dose is big, and quality control level is low.
Summary of the invention:
The objective of the invention is to: a kind of ointment for the treatment of dysmenorrhea and preparation method and method of quality control are provided, the present invention is directed to the deficiencies in the prior art, the ointment making that is provided, easy to use, instant effect, the cure rate height, short treating period has no side effect; And its method of quality control is scientific and reasonable, can effectively control and guarantee product quality.
The present invention constitutes like this: it is made by Fructus Evodiae 200g, Rhizoma Corydalis 200g, Rhizoma Zingiberis 1000g and Rhizoma Curcumae Longae 1200g.
The preparation method of ointment for the treatment of dysmenorrhea is: get Rhizoma Zingiberis, Rhizoma Curcumae Longae is extracted volatile oil with steam distillation respectively; It is an amount of that Fructus Evodiae, Rhizoma Corydalis add 85% ethanol respectively, heating and refluxing extraction secondary, 2 hours for the first time, 1 hour for the second time, filter merge extractive liquid,, decolouring, reclaim ethanol, be concentrated into 60～65 ℃ of relative densities and be 1.30～1.32 clear paste, clear paste and emulsion bases are an amount of, grind well the back and add above-mentioned volatile oil, mixing is made ointment; Patch loam cake lining is cut, promptly.
The method of quality control of ointment for the treatment of dysmenorrhea: described method of quality control mainly comprise in character, discriminating, inspection, the assay project partly or entirely; Wherein discriminating is that the thin layer chromatography of Rhizoma Zingiberis, Rhizoma Curcumae Longae, Fructus Evodiae and Rhizoma Corydalis is differentiated; Assay is the assay to Rhizoma Corydalis in the preparation.
The discrimination method of Rhizoma Zingiberis is to be contrast with the oil of Rhizoma Zingiberis Recens reference substance, and with cyclohexane extraction: ether=9: 1 is the thin layer chromatography of developing solvent; The discrimination method of Rhizoma Curcumae Longae is to be contrast with the Rhizoma Curcumae Longae control medicinal material, and with cyclohexane extraction: ether=9: 1 is the thin layer chromatography of developing solvent; The discrimination method of Fructus Evodiae is to be contrast with the Fructus Evodiae control medicinal material, and with n-butyl alcohol: acetic acid: the upper solution of water=2: 1: 1 is the thin layer chromatography of developing solvent; The discrimination method of Rhizoma Corydalis is to be contrast with the tetrahydropalmatine reference substance, and with normal hexane: chloroform: methanol=7.5: 4: 1 is the thin layer chromatography of developing solvent.
Concrete discrimination method comprises the part or all of of following project:
(1) get this ointment 4g, add water 200ml and spirit of vinegar 2ml, connect volatile oil determination apparatus, the heating distillating extracting oil, oil mass no longer increases to the determinator; Divide and get volatile oil, add ethyl acetate and make the solution that every 1ml contains 20 μ l, as need testing solution; Other gets the oil of Rhizoma Zingiberis Recens reference substance, adds ethyl acetate and makes solution that every lml contains 5 μ l product solution in contrast; According to an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: ether=9: 1 be developing solvent, launches, and takes out, and dries, and sprays with the dinitrophenylhydrazine test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(2) get Rhizoma Curcumae Longae control medicinal material 0.5g, the 20ml that adds diethyl ether, supersound process 20 minutes filters, and filtrate volatilizes, and residue adds methanol 1ml makes dissolving, in contrast medical material solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography, draw each the 10 μ l of need testing solution under control medicinal material solution and discriminating (1) item, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: ether=9: 1 is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution of new system, and 105 ℃ to be heated 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;
(3) get this ointment 2g, add spirit of vinegar 15ml, shake well is put water-bath and was placed 15 minutes, filter immediately, filtrate is regulated PH to 8～9 with strong ammonia solution, uses ether 20ml, and jolting is extracted, branch is got ether solution and is volatilized, and residue adds ethanol 1ml makes dissolving, as need testing solution; Other gets Fructus Evodiae control medicinal material 0.2g, adds ethanol 10ml, and supersound process 20 minutes filters, and filtrate is medical material solution in contrast; According to the test of an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with n-butyl alcohol: acetic acid: the upper solution of water=2: 1: 1 is developing solvent, launches, and takes out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
(4) get the tetrahydropalmatine reference substance, add methanol and make the solution that every 1ml contains 0.4mg, in contrast product solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography, draw need testing solution and each 10 μ l of above-mentioned reference substance solution of differentiating under (3) item, put respectively on the silica gel g thin-layer plate of same usefulness 1% sodium hydroxide solution preparation, with normal hexane: chloroform: methanol=7.5: 4: 1 is developing solvent, launch, take out, dry, it is smoked clear to the speckle colour developing to put in the iodine vapor; Inspect under the daylight, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color; After waving the iodine vapor that adsorbs on the most plate, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
The content assaying method of Rhizoma Corydalis is to be contrast with the tetrahydropalmatine reference substance, is that 7.4 phosphate buffer=60: 40 is the high performance liquid chromatography of mobile phase with methanol: PH.
Concrete content assaying method is:
According to an appendix VI of Chinese Pharmacopoeia version in 2000 D high effective liquid chromatography for measuring:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol: PH is that 7.4 phosphate buffer=60: 40 is mobile phase; The detection wavelength is 280nm; Number of theoretical plate calculates by the tetrahydropalmatine peak should be not less than 2000;
It is an amount of that the preparation precision of reference substance solution takes by weighing the tetrahydropalmatine reference substance, adds methanol and make the solution that every 1ml contains 0.1mg, promptly;
The preparation of the need testing solution content under the cream content uniformity item of getting it filled, mixing is got 6g, the accurate title, decide, and puts in the conical flask, adds spirit of vinegar 30ml, shake well, ice bath is placed after 30 minutes and is filtered immediately, with ice-cold spirit of vinegar 10ml gradation washing container and residue, filter, merging filtrate is regulated PH to 8～9 with strong ammonia solution, extracts 3 times with the ether jolting, each 20ml, merge ether solution, volatilize, residue adds methanol makes dissolving, put in the 10ml measuring bottle, add methanol and be diluted to scale, shake up, filter, get subsequent filtrate, promptly;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly;
The every 1g of this ointment contains Rhizoma Corydalis with tetrahydropalmatine C
21H
25NO
4Meter must not be less than 0.15mg.
Method of quality control of the present invention comprises:
Character: ointment is the emulsifiable paste of sundown, gas fragrance; Patch is the circular patch of pastille not;
Differentiate: (1) gets this ointment 4g, adds water 200ml and spirit of vinegar 2ml, connects volatile oil determination apparatus, the heating distillating extracting oil, and oil mass no longer increases to the determinator; Divide and get volatile oil, add ethyl acetate and make the solution that every 1ml contains 20 μ l, as need testing solution; Other gets the oil of Rhizoma Zingiberis Recens reference substance, adds ethyl acetate and makes solution that every 1ml contains 5 μ l product solution in contrast; According to an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: ether=9: 1 be developing solvent, launches, and takes out, and dries, and sprays with the dinitrophenylhydrazine test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(2) get Rhizoma Curcumae Longae control medicinal material 0.5g, the 20ml that adds diethyl ether, supersound process 20 minutes filters, and filtrate volatilizes, and residue adds methanol 1ml makes dissolving, in contrast medical material solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography, draw each the 10 μ l of need testing solution under control medicinal material solution and discriminating (1) item, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: ether=9: 1 is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution of new system, and 105 ℃ to be heated 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;
(3) get this ointment 2g, add spirit of vinegar 15ml, shake well is put water-bath and was placed 15 minutes, filter immediately, filtrate is regulated PH to 8～9 with strong ammonia solution, uses ether 20ml, and jolting is extracted, branch is got ether solution and is volatilized, and residue adds ethanol 1ml makes dissolving, as need testing solution; Other gets Fructus Evodiae control medicinal material 0.2g, adds ethanol 10ml, and supersound process 20 minutes filters, and filtrate is medical material solution in contrast; According to the test of an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with n-butyl alcohol: acetic acid: the upper solution of water=2: 1: 1 is developing solvent, launches, and takes out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
(4) get the tetrahydropalmatine reference substance, add methanol and make the solution that every 1ml contains 0.4mg, in contrast product solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography, draw need testing solution and each 10 μ l of above-mentioned reference substance solution of differentiating under (3) item, put respectively on the silica gel g thin-layer plate of same usefulness 1% sodium hydroxide solution preparation, with normal hexane: chloroform: methanol=7.5: 4: 1 is developing solvent, launch, take out, dry, it is smoked clear to the speckle colour developing to put in the iodine vapor; Inspect under the daylight, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color; After waving the iodine vapor that adsorbs on the most plate, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
Check: heavy metal is got this ointment 1.0g, presses an appendix IX of Chinese Pharmacopoeia version in 2000 the E second method inspection, contains heavy metal and must not cross 20/1000000ths;
Other should meet relevant every regulation under an appendix IR of Chinese Pharmacopoeia version in 2000 the ointment item;
Assay: shine an appendix VI of Chinese Pharmacopoeia version in 2000 D high effective liquid chromatography for measuring:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol: PH is that 7.4 phosphate buffer=60: 40 is mobile phase; The detection wavelength is 280nm; Number of theoretical plate calculates by the tetrahydropalmatine peak should be not less than 2000;
It is an amount of that the preparation precision of reference substance solution takes by weighing the tetrahydropalmatine reference substance, adds methanol and make the solution that every 1ml contains 0.1mg, promptly;
The preparation of the need testing solution content under the cream content uniformity item of getting it filled, mixing is got 6g, the accurate title, decide, and puts in the conical flask, adds spirit of vinegar 30ml, shake well, ice bath is placed after 30 minutes and is filtered immediately, with ice-cold spirit of vinegar 10ml gradation washing container and residue, filter, merging filtrate is regulated PH to 8～9 with strong ammonia solution, extracts 3 times with the ether jolting, each 20ml, merge ether solution, volatilize, residue adds methanol makes dissolving, put in the 10ml measuring bottle, add methanol and be diluted to scale, shake up, filter, get subsequent filtrate, promptly;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly;
The every 1g of this ointment contains Rhizoma Corydalis with tetrahydropalmatine C
21H
25NO
4Meter must not be less than 0.15mg.
Fructus Evodiae has the soothing the liver therapeutic method to keep the adverse QI flowing downwards in the side, warming spleen and stomach for dispelling cold, dissipating depression of QI pain relieving, stopping nausea and vomiting by lowering the adverse flow of QI, the merit of supporing yang antidiarrheal; Be used for headache, colic, beriberi, dysmenorrhea, abdominal distention, vomiting acid regurgitation, aphtha etc.Rhizoma Corydalis is hot without hesitation, warm, and bitter in the mouth had both been gone into blood system, went into edema caused by disorder of QI again, the gas in can promoting the circulation of blood, and the blood in again can circulation of qi promoting is the good medicine of the promoting the circulation of QI pain relieving of invigorating blood circulation; Be used for costa sternales, epigastric pain, amenorrhea dysmenorrhea, postpartum stagnation, tumbling and swelling.Rhizoma Zingiberis property suffering, heat, warming spleen and stomach for dispelling cold, recuperating depleted YANG is promoted blood circulation, and dry temperature expectorant is used for coldness and pain in the epigastrium, the vomiting diarrhea, the cold extremities faint pulse, phlegm retention is breathed with cough.Rhizoma Curcumae Longae property suffering, hardship, temperature, the removing blood stasis circulation of qi promoting, inducing menstruation to relieve menalgia is used for the blood block up stagnation of QI, the twinge of the breast side of body, amenorrhea stomachache, treating swelling and pain by traumatic injury, rheumatalgia.All medicines share, and are remarkable to the TREATMENT OF DYSMENORRHOEA effect, can alleviate and eliminate symptom rapidly.
The applicant has carried out the method for quality control that pharmaceutical preparation of the present invention is selected in a series of experiments, guaranteeing its science, reasonable, feasible, and guarantees the curative effect of medicine.
Method of quality control research
(1) sample and contrast medicine source
Sample: our company's self-control, lot number is: 050420,050506,050520.
Oil of Rhizoma Zingiberis Recens reference substance (Nat'l Pharmaceutical ﹠ Biological Products Control Institute provides)
Rhizoma Curcumae Longae control medicinal material (Nat'l Pharmaceutical ﹠ Biological Products Control Institute provides)
Fructus Evodiae control medicinal material (Nat'l Pharmaceutical ﹠ Biological Products Control Institute provides)
Tetrahydropalmatine reference substance (Nat'l Pharmaceutical ﹠ Biological Products Control Institute provides)
Other reagent is analytical pure.
(2) content limit
This preparation needs quantitative content's index to adopt high effective liquid chromatography for measuring, and every 1g ointment contains Rhizoma Corydalis with tetrahydropalmatine (C
21H
25NO
4) meter, must not be less than 0.15mg.
(3) character
This preparation is that clear paste and emulsion bases grind well, and adds volatile oil, and mixing is made, and through many batch sample trial-productions, the result shows the emulsifiable paste that is sundown, gas fragrance.Therefore one of character is defined as that " ointment is the emulsifiable paste of sundown, gas fragrance in the ointment for the treatment of dysmenorrhea quality standard; Patch is the circular patch of pastille not.”
(4) differentiate
The present invention increases the specificity thin layer chromatography of having worked out Rhizoma Zingiberis, Rhizoma Curcumae Longae and differentiates.
The preparation sample of need testing solution is put in the determination of volatile oil device, adds water and a small amount of spirit of vinegar (make breakdown of emulsion, avoid bubbling), and heating and refluxing extraction volatile oil divides in separatory funnel and gets volatile oil to fully, adds ethyl acetate and makes dissolving, promptly gets need testing solution.Prepare scarce Rhizoma Zingiberis respectively, lack the negative test liquid of Rhizoma Curcumae Longae with method.
The Rhizoma Zingiberis thin layer chromatography is differentiated Rhizoma Zingiberis thin layer chromatography discriminating employing oil of Rhizoma Zingiberis Recens reference substance.Once used the Rhizoma Zingiberis control medicinal material in the test, add diethyl ether (or ethanol), supersound process (or backflow) is extracted preparation control medicinal material solution, but thin layer chromatography is not seen the corresponding feature speckle of Rhizoma Zingiberis volatile oil.Developing solvent is selected with reference to the regulation under the pharmacopeia Rhizoma Zingiberis discriminating item, and the developing solvent ratio adjusts slightly and is cyclohexane extraction: ether (9: 1), separating effect is better.Once with the colour developing of vanillin test solution, interference was arranged but lack the Rhizoma Zingiberis negative sample.Consider to contain carbonyl compound in the oil of ginger and select the colour developing of dinitrophenylhydrazine test solution, as a result in the test sample chromatograph with the corresponding position of oil of Rhizoma Zingiberis Recens reference substance on, show the speckle of same color (yellow), negative noiseless.
The Rhizoma Curcumae Longae thin layer chromatography is differentiated employing Rhizoma Curcumae Longae control medicinal material, and the supersound process that adds diethyl ether is extracted volatile oil, carefully flings to solvent, and residue adds dissolve with methanol, promptly gets control medicinal material solution.The developing solvent cyclohexane extraction: ether (9: 1), developer 5% vanillin sulphuric acid test solution, 105 ℃ to be heated to speckle colour developing clear, in the test sample chromatograph with the corresponding position of Rhizoma Curcumae Longae control medicinal material on, show the speckle of same color (aubergine), negative noiseless.
(5) check
Heavy metal is got this ointment 1.0g, checks that by an appendix IX of Chinese Pharmacopoeia version in 2000 E second method result is all up to specification.
(6) assay
The content assaying method research of Rhizoma Corydalis:
1, method
(1) instrument and reagent:
Instrument: HP1100 high performance liquid chromatograph, HP chromatographic work station;
Reagent: methanol, ether, spirit of vinegar are analytical pure;
Reference substance: tetrahydropalmatine reference substance (Nat'l Pharmaceutical ﹠ Biological Products Control Institute provides);
Test sample: ointment for the treatment of dysmenorrhea, our company's self-control, lot number is: 050420,050506,050520.
(2) chromatographic condition:
With octadecylsilane chemically bonded silica is filler; Methanol: PH is that 7.4 phosphate buffer=60: 40 is mobile phase; The detection wavelength is 280nm; Number of theoretical plate calculates by the tetrahydropalmatine peak should be not less than 2000.
Chromatographic column model: Hypersil ODS25 μ m φ 4.6 * 200mm.
(3) preparation of reference substance solution:
It is an amount of that precision takes by weighing the tetrahydropalmatine reference substance, adds methanol and make the solution that every 1ml contains 0.1mg, promptly.
(4) preparation of need testing solution:
Content under the cream content uniformity of the getting it filled item, mixing is got 6g, and accurate the title, decide, put in the conical flask, add spirit of vinegar 30ml, shake well, ice bath is placed after 30 minutes and is filtered immediately, with ice-cold spirit of vinegar 10ml gradation washing container and residue, filter, merging filtrate is regulated PH to 8～9 with strong ammonia solution, extract 3 times with the ether jolting, each 20ml merges ether solution, volatilizes, residue adds methanol makes dissolving, puts in the 10ml measuring bottle, adds methanol and is diluted to scale, shakes up, filter, get subsequent filtrate, promptly.
(5) selection of detection wavelength:
Measure the tetrahydropalmatine reference substance solution and measure ultraviolet spectrogram on ultraviolet spectrophotometer, in the interscan of 400～200nm wave-length coverage, the result has maximum absorption band at 280nm wavelength place, so select the detection wavelength of 280nm as this mensuration.
2, the comparison of extracting method
Content under the cream content uniformity of the getting it filled item, mixing is got 6g, and accurate the title, decide, put in the conical flask, add spirit of vinegar 30ml, shake well, ice bath is placed after 30 minutes and is filtered immediately, with ice-cold spirit of vinegar 10ml gradation washing container and residue, filter, merging filtrate is regulated PH to 8～9 with strong ammonia solution, extract 3 times with the ether jolting, each 20ml merges ether solution, volatilizes, residue adds methanol makes dissolving, puts 10, in the l measuring bottle, adds methanol and is diluted to scale, shake up, filter, get subsequent filtrate, promptly.
Other cream 6g that gets it filled, accurate claim fixed, with above-mentioned method chloroform extraction.
Respectively get subsequent filtrate 10 μ l and inject chromatograph of liquid, the record chromatogram.
The comparative result of extracting method
| Method | Content (mg/g) |
| Ether extraction | 0.40 |
| Chloroform extraction | 0.11 |
The result shows that ether extraction is higher than chloroform extraction efficient.Therefore select ether extraction for use.
3, blank assay
Get scarce Rhizoma Corydalis negative sample, according to the preparation of the method under the need testing solution item, by above-mentioned chromatographic condition analysis.With the corresponding position of reference substance on, not having obviously, other peak occurs.The result proves that negative sample is noiseless to this test.
4, linear relationship is investigated
It is an amount of that precision takes by weighing the tetrahydropalmatine reference substance, add methanol and be mixed with reference substance storing solution (0.1008mg/ml), accurate reference substance storing solution 0.5ml, 1ml, 2ml, 3ml, 4ml, the 5ml of drawing is in the 5ml volumetric flask, add methanol constant volume respectively to scale, shake up, accurate respectively each the 10 μ l of above-mentioned reference substance solution that draw inject high performance liquid chromatograph, measure the record result.Concentration with tetrahydropalmatine is abscissa, and peak area is a vertical coordinate, draw standard curve, tetrahydropalmatine is good linear relation between 0.01～0.1mg/ml.
5, precision test: (lot number: 050520), prepare need testing solution as stated above, the accurate 10 μ l that draw repeat sample introduction 5 times, and RSD is 1.32% as a result, shows that precision is good to get this preparation.
6, repeatability test: press 5 parts of test samples of test sample compound method preparation, measure every duplicate samples content respectively, average content is 0.185mg/g as a result, and RSD is 1.45%, shows that repeatability is good.
7, recovery test: precision takes by weighing the test sample (lot number: 050520) 5 parts of a known content, accurate reference substance solution (concentration the is 0.1008mg/ml) 2ml that adds in every part, make need testing solution as stated above, measure, calculate recovery rate, average recovery rate is 99.135%, and RSD=1.80% shows and reclaims well.
8, stability test: (lot number: 050520), prepare the need testing solution portion as stated above, sample introduction is measured at regular intervals, and record chromatogram, results peaks area are stable in 6 hours to get this preparation.Show that this test method is stable, minute can be in 6 hours.
9, the mensuration of sample and content limit determines
Press the compound method of need testing solution, many batch samples are carried out assay, to determine its content limit, the assay of sample the results are shown in following table.
The assay result
| Lot number | 031208 | 031218 | 040414 | 040424 | 040520 | 040608 | 040728 | 040808 | 040920 | 041019 |
| Content | 0.17 | 0.18 | 0.18 | 0.20 | 0.16 | 0.18 | 0.16 | 0.21 | 0.20 | 0.19 |
| Lot number | 041101 | 041128 | 041207 | 050203 | 050220 | 050323 | 050405 | 050420 | 050506 | 050520 |
| Content | 0.16 | 0.18 | 0.19 | 0.20 | 0.17 | 0.21 | 0.16 | 0.18 | 0.18 | 0.19 |
Determine that at last its content limit is that every 1g ointment contains Rhizoma Corydalis with tetrahydropalmatine (C
21H
25NO
4) meter, must not be less than 0.15mg.
Compared with prior art, prescription of the present invention is simple, and making, easy to use is fit to all kinds of patients and uses; Evident in efficacy, instant effect, short treating period has no side effect; The method of quality control precision height that is provided, favorable reproducibility, measurement result is accurate, has guaranteed the clinical efficacy of said preparation effectively.
The specific embodiment:
Embodiments of the invention 1: Fructus Evodiae 200g, Rhizoma Corydalis 200g, Rhizoma Zingiberis 1000g, Rhizoma Curcumae Longae 1200g
Get Rhizoma Zingiberis, Rhizoma Curcumae Longae is extracted volatile oil with steam distillation respectively; It is an amount of that Fructus Evodiae, Rhizoma Corydalis add 85%7 alcohol respectively, heating and refluxing extraction secondary, 2 hours for the first time, 1 hour for the second time, filter merge extractive liquid,, decolouring, reclaim ethanol, be concentrated into 60～65 ℃ of relative densities and be 1.30～1.32 clear paste, clear paste and emulsion bases are an amount of, grind well the back and add above-mentioned volatile oil, mixing is made ointment 1000g; Patch loam cake lining is cut, promptly.The external of this product, 2～3 times on the one; The cream of getting it filled is coated with in right amount into umbilical part, sticks patch again; Other affected part can directly apply.
Embodiments of the invention 2: described method of quality control comprises following content:
Character: ointment is the emulsifiable paste of sundown, gas fragrance; Patch is the circular patch of pastille not;
Differentiate: (1) gets this ointment 4g, adds water 200ml and spirit of vinegar 2ml, connects volatile oil determination apparatus, the heating distillating extracting oil, and oil mass no longer increases to the determinator; Divide and get volatile oil, add ethyl acetate and make the solution that every 1ml contains 20 μ l, as need testing solution; Other gets the oil of Rhizoma Zingiberis Recens reference substance, adds ethyl acetate and makes solution that every 1ml contains 5 μ l product solution in contrast; According to an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: ether=9: 1 be developing solvent, launches, and takes out, and dries, and sprays with the dinitrophenylhydrazine test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(2) get Rhizoma Curcumae Longae control medicinal material 0.5g, the 20ml that adds diethyl ether, supersound process 20 minutes filters, and filtrate volatilizes, and residue adds methanol 1ml makes dissolving, in contrast medical material solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography, draw each the 10 μ l of need testing solution under control medicinal material solution and discriminating (1) item, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: ether=9: 1 is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution of new system, and 105 ℃ to be heated 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;
(3) get this ointment 2g, add spirit of vinegar 15ml, shake well is put water-bath and was placed 15 minutes, filter immediately, filtrate is regulated PH to 8～9 with strong ammonia solution, uses ether 20ml, and jolting is extracted, branch is got ether solution and is volatilized, and residue adds ethanol 1ml makes dissolving, as need testing solution; Other gets Fructus Evodiae control medicinal material 0.2g, adds ethanol 10ml, and supersound process 20 minutes filters, and filtrate is medical material solution in contrast; According to the test of an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with n-butyl alcohol: acetic acid: the upper solution of water=2: 1: 1 is developing solvent, launches, and takes out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
(4) get the tetrahydropalmatine reference substance, add methanol and make the solution that every 1ml contains 0.4mg, in contrast product solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography, draw need testing solution and each 10 μ l of above-mentioned reference substance solution of differentiating under (3) item, put respectively on the silica gel g thin-layer plate of same usefulness 1% sodium hydroxide solution preparation, with normal hexane: chloroform: methanol=7.5: 4: 1 is developing solvent, launch, take out, dry, it is smoked clear to the speckle colour developing to put in the iodine vapor; Inspect under the daylight, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color; After waving the iodine vapor that adsorbs on the most plate, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
Check: heavy metal is got this ointment 1.0g, presses an appendix IX of Chinese Pharmacopoeia version in 2000 the E second method inspection, contains heavy metal and must not cross 20/1000000ths;
Other should meet relevant every regulation under an appendix IR of Chinese Pharmacopoeia version in 2000 the ointment item;
Assay: shine an appendix VI of Chinese Pharmacopoeia version in 2000 D high effective liquid chromatography for measuring:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol: PH is that 7.4 phosphate buffer=60: 40 is mobile phase; The detection wavelength is 280nm; Number of theoretical plate calculates by the tetrahydropalmatine peak should be not less than 2000;
It is an amount of that the preparation precision of reference substance solution takes by weighing the tetrahydropalmatine reference substance, adds methanol and make the solution that every 1ml contains 0.1mg, promptly;
The preparation of the need testing solution content under the cream content uniformity item of getting it filled, mixing is got 6g, the accurate title, decide, and puts in the conical flask, adds spirit of vinegar 30ml, shake well, ice bath is placed after 30 minutes and is filtered immediately, with ice-cold spirit of vinegar 10ml gradation washing container and residue, filter, merging filtrate is regulated PH to 8～9 with strong ammonia solution, extracts 3 times with the ether jolting, each 20ml, merge ether solution, volatilize, residue adds methanol makes dissolving, put in the 10ml measuring bottle, add methanol and be diluted to scale, shake up, filter, get subsequent filtrate, promptly;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly;
The every 1g of this ointment contains Rhizoma Corydalis with tetrahydropalmatine C
21H
25NO
4Meter must not be less than 0.15mg.
Embodiments of the invention 3: method of quality control can comprise following content:
Character: ointment is the emulsifiable paste of sundown, gas fragrance; Patch is the circular patch of pastille not;
Differentiate: (1) gets this ointment 4g, adds water 200ml and spirit of vinegar 2ml, connects volatile oil determination apparatus, the heating distillating extracting oil, and oil mass no longer increases to the determinator; Divide and get volatile oil, add ethyl acetate and make the solution that every 1ml contains 20 μ l, as need testing solution; Other gets the oil of Rhizoma Zingiberis Recens reference substance, adds ethyl acetate and makes solution that every 1ml contains 5 μ l product solution in contrast; According to an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: ether=9: 1 be developing solvent, launches, and takes out, and dries, and sprays with the dinitrophenylhydrazine test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(2) get Rhizoma Curcumae Longae control medicinal material 0.5g, the 20ml that adds diethyl ether, supersound process 20 minutes filters, and filtrate volatilizes, and residue adds methanol 1ml makes dissolving, in contrast medical material solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography, draw each the 10 μ l of need testing solution under control medicinal material solution and discriminating (1) item, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: ether=9: 1 is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution of new system, and 105 ℃ to be heated 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;
Assay: shine an appendix VI of Chinese Pharmacopoeia version in 2000 D high effective liquid chromatography for measuring:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol: PH is that 7.4 phosphate buffer=60: 40 is mobile phase; The detection wavelength is 280nm; Number of theoretical plate calculates by the tetrahydropalmatine peak should be not less than 2000;
It is an amount of that the preparation precision of reference substance solution takes by weighing the tetrahydropalmatine reference substance, adds methanol and make the solution that every 1ml contains 0.1mg, promptly;
The preparation of the need testing solution content under the cream content uniformity item of getting it filled, mixing is got 6g, the accurate title, decide, and puts in the conical flask, adds spirit of vinegar 30ml, shake well, ice bath is placed after 30 minutes and is filtered immediately, with ice-cold spirit of vinegar 10ml gradation washing container and residue, filter, merging filtrate is regulated PH to 8～9 with strong ammonia solution, extracts 3 times with the ether jolting, each 20ml, merge ether solution, volatilize, residue adds methanol makes dissolving, put in the 10ml measuring bottle, add methanol and be diluted to scale, shake up, filter, get subsequent filtrate, promptly;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly;
The every 1g of this ointment contains Rhizoma Corydalis with tetrahydropalmatine C
21H
25NO
4Meter must not be less than 0.15mg.
Embodiments of the invention 4: method of quality control can comprise following content:
Character: ointment is the emulsifiable paste of sundown, gas fragrance; Patch is the circular patch of pastille not;
Differentiate: (1) gets this ointment 4g, adds water 200ml and spirit of vinegar 2ml, connects volatile oil determination apparatus, the heating distillating extracting oil, and oil mass no longer increases to the determinator; Divide and get volatile oil, add ethyl acetate and make the solution that every 1ml contains 20 μ l, as need testing solution; Other gets the oil of Rhizoma Zingiberis Recens reference substance, adds ethyl acetate and makes solution that every 1ml contains 5 μ l product solution in contrast; According to an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: ether=9: 1 be developing solvent, launches, and takes out, and dries, and sprays with the dinitrophenylhydrazine test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(2) get this ointment 2g, add spirit of vinegar 15ml, shake well is put water-bath and was placed 15 minutes, filter immediately, filtrate is regulated PH to 8～9 with strong ammonia solution, uses ether 20ml, and jolting is extracted, branch is got ether solution and is volatilized, and residue adds ethanol 1ml makes dissolving, as need testing solution; Other gets Fructus Evodiae control medicinal material 0.2g, adds ethanol 10ml, and supersound process 20 minutes filters, and filtrate is medical material solution in contrast; According to the test of an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with n-butyl alcohol: acetic acid: the upper solution of water=2: 1: 1 is developing solvent, launches, and takes out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
(3) get the tetrahydropalmatine reference substance, add methanol and make the solution that every 1ml contains 0.4mg, in contrast product solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography, draw need testing solution and each 10 μ l of above-mentioned reference substance solution of differentiating under (2) item, put respectively on the silica gel g thin-layer plate of same usefulness 1% sodium hydroxide solution preparation, with normal hexane: chloroform: methanol=7.5: 4: 1 is developing solvent, launch, take out, dry, it is smoked clear to the speckle colour developing to put in the iodine vapor; Inspect under the daylight, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color; After waving the iodine vapor that adsorbs on the most plate, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
Check: heavy metal is got this ointment 1.0g, presses an appendix IX of Chinese Pharmacopoeia version in 2000 the E second method inspection, contains heavy metal and must not cross 20/1000000ths;
Other should meet relevant every regulation under an appendix IR of Chinese Pharmacopoeia version in 2000 the ointment item.
Embodiments of the invention 5: method of quality control can comprise following content:
Character: ointment is the emulsifiable paste of sundown, gas fragrance; Patch is the circular patch of pastille not;
Differentiate: (1) gets this ointment 4g, adds water 200ml and spirit of vinegar 2ml, connects volatile oil determination apparatus, the heating distillating extracting oil, and oil mass no longer increases to the determinator; Divide and get volatile oil, add ethyl acetate and make the solution that every 1ml contains 20 μ l, as need testing solution; Get Rhizoma Curcumae Longae control medicinal material 0.5g, the 20ml that adds diethyl ether, supersound process 20 minutes filters, and filtrate volatilizes, and residue adds methanol 1ml makes dissolving, in contrast medical material solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: ether=9: 1 is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution of new system, and 105 ℃ to be heated 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;
(2) get this ointment 2g, add spirit of vinegar 15ml, shake well is put water-bath and was placed 15 minutes, filter immediately, filtrate is regulated PH to 8～9 with strong ammonia solution, uses ether 20ml, and jolting is extracted, branch is got ether solution and is volatilized, and residue adds ethanol 1ml makes dissolving, as need testing solution; Other gets Fructus Evodiae control medicinal material 0.2g, adds ethanol 10ml, and supersound process 20 minutes filters, and filtrate is medical material solution in contrast; According to the test of an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with n-butyl alcohol: acetic acid: the upper solution of water=2: 1: 1 is developing solvent, launches, and takes out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
Check: heavy metal is got this ointment 1.0g, presses an appendix IX of Chinese Pharmacopoeia version in 2000 the E second method inspection, contains heavy metal and must not cross 20/1000000ths;
Other should meet relevant every regulation under an appendix IR of Chinese Pharmacopoeia version in 2000 the ointment item;
Assay: shine an appendix VI of Chinese Pharmacopoeia version in 2000 D high effective liquid chromatography for measuring:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol: PH is that 7.4 phosphate buffer=60: 40 is mobile phase; The detection wavelength is 280nm; Number of theoretical plate calculates by the tetrahydropalmatine peak should be not less than 2000;
It is an amount of that the preparation precision of reference substance solution takes by weighing the tetrahydropalmatine reference substance, adds methanol and make the solution that every 1ml contains 0.1mg, promptly;
The preparation of the need testing solution content under the cream content uniformity item of getting it filled, mixing is got 6g, the accurate title, decide, and puts in the conical flask, adds spirit of vinegar 30ml, shake well, ice bath is placed after 30 minutes and is filtered immediately, with ice-cold spirit of vinegar 10ml gradation washing container and residue, filter, merging filtrate is regulated PH to 8～9 with strong ammonia solution, extracts 3 times with the ether jolting, each 20ml, merge ether solution, volatilize, residue adds methanol makes dissolving, put in the 10ml measuring bottle, add methanol and be diluted to scale, shake up, filter, get subsequent filtrate, promptly;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly;
The every 1g of this ointment contains Rhizoma Corydalis with tetrahydropalmatine C
21H
25NO
4Meter must not be less than 0.15mg.
Claims (7)
1. ointment for the treatment of dysmenorrhea, it is characterized in that: it prepares according to following method with Fructus Evodiae 200g, Rhizoma Corydalis 200g, Rhizoma Zingiberis 1000g and Rhizoma Curcumae Longae 1200g: get Rhizoma Zingiberis, Rhizoma Curcumae Longae is extracted volatile oil with steam distillation respectively; It is an amount of that Fructus Evodiae, Rhizoma Corydalis add 85% ethanol respectively, heating and refluxing extraction secondary, 2 hours for the first time, 1 hour for the second time, filter merge extractive liquid,, decolouring, reclaim ethanol, be concentrated into 60～65 ℃ of relative densities and be 1.30～1.32 clear paste, clear paste and emulsion bases are an amount of, grind well the back and add above-mentioned volatile oil, mixing is made ointment; Patch loam cake lining is cut, promptly.
2. the method for quality control of ointment for the treatment of dysmenorrhea as claimed in claim 1, it is characterized in that: described method of quality control is character, discriminating, inspection and assay project; Wherein discriminating is that the thin layer chromatography of Rhizoma Zingiberis, Rhizoma Curcumae Longae, Fructus Evodiae and Rhizoma Corydalis is differentiated; Assay is the assay to Rhizoma Corydalis in the preparation.
3. according to the method for quality control of the described ointment for the treatment of dysmenorrhea of claim 2, it is characterized in that: the discrimination method of Rhizoma Zingiberis is to be contrast with the oil of Rhizoma Zingiberis Recens reference substance, and with cyclohexane extraction: ether=9: 1 is the thin layer chromatography of developing solvent; The discrimination method of Rhizoma Curcumae Longae is to be contrast with the Rhizoma Curcumae Longae control medicinal material, and with cyclohexane extraction: ether=9: 1 is the thin layer chromatography of developing solvent; The discrimination method of Fructus Evodiae is to be contrast with the Fructus Evodiae control medicinal material, and with n-butyl alcohol: acetic acid: the upper solution of water=2: 1: 1 is the thin layer chromatography of developing solvent; The discrimination method of Rhizoma Corydalis is to be contrast with the tetrahydropalmatine reference substance, and with normal hexane: chloroform: methanol=7.5: 4: 1 is the thin layer chromatography of developing solvent.
4. according to the method for quality control of claim 2 or 3 described ointment for the treatment of dysmenorrhea, it is characterized in that: concrete discrimination method is:
(1) get this ointment 4g, add water 200ml and spirit of vinegar 2ml, connect volatile oil determination apparatus, the heating distillating extracting oil, oil mass no longer increases to the determinator; Divide and get volatile oil, add ethyl acetate and make the solution that every 1ml contains 20 μ l, as need testing solution; Other gets the oil of Rhizoma Zingiberis Recens reference substance, adds ethyl acetate and makes solution that every 1ml contains 5 μ l product solution in contrast; According to an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: ether=9: 1 be developing solvent, launches, and takes out, and dries, and sprays with the dinitrophenylhydrazine test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(2) get Rhizoma Curcumae Longae control medicinal material 0.5g, the 20ml that adds diethyl ether, supersound process 20 minutes filters, and filtrate volatilizes, and residue adds methanol 1ml makes dissolving, in contrast medical material solution; According to the test of an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography,
Draw respectively 10 μ l of control medicinal material solution and discriminating (1) need testing solution down, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: ether=9: 1 is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution of new system, and 105 ℃ to be heated 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;
(3) get this ointment 2g, add spirit of vinegar 15ml, shake well is put water-bath and was placed 15 minutes, filter immediately, filtrate is regulated PH to 8～9 with strong ammonia solution, uses ether 20ml, and jolting is extracted, branch is got ether solution and is volatilized, and residue adds ethanol 1ml makes dissolving, as need testing solution; Other gets Fructus Evodiae control medicinal material 0.2g, adds ethanol 10ml, and supersound process 20 minutes filters, and filtrate is medical material solution in contrast; According to the test of an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with n-butyl alcohol: acetic acid: the upper solution of water=2: 1: 1 is developing solvent, launches, and takes out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
(4) get the tetrahydropalmatine reference substance, add methanol and make the solution that every 1ml contains 0.4mg, in contrast product solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography, draw need testing solution and each 10 μ l of above-mentioned reference substance solution of differentiating under (3) item, put respectively on the silica gel g thin-layer plate of same usefulness 1% sodium hydroxide solution preparation, with normal hexane: chloroform: methanol=7.5: 4: 1 is developing solvent, launch, take out, dry, it is smoked clear to the speckle colour developing to put in the iodine vapor; Inspect under the daylight, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color; After waving the iodine vapor that adsorbs on the most plate, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
5. according to the method for quality control of the described ointment for the treatment of dysmenorrhea of claim 2, it is characterized in that: the content assaying method of Rhizoma Corydalis is to be contrast with the tetrahydropalmatine reference substance, is that 7.4 phosphate buffer=60: 40 is the high performance liquid chromatography of mobile phase with methanol: PH.
6. according to the method for quality control of claim 2 or 5 described ointment for the treatment of dysmenorrhea, it is characterized in that: concrete content assaying method is:
According to an appendix VI of Chinese Pharmacopoeia version in 2000 D high effective liquid chromatography for measuring:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol: PH is that 7.4 phosphate buffer=60: 40 is mobile phase; The detection wavelength is 280nm; Number of theoretical plate calculates by the tetrahydropalmatine peak should be not less than 2000;
It is an amount of that the preparation precision of reference substance solution takes by weighing the tetrahydropalmatine reference substance, adds methanol and make the solution that every 1ml contains 0.1mg, promptly;
The 6g content is got in the preparation of need testing solution, mixing, and accurate the title, decide, and puts in the conical flask, add spirit of vinegar 30ml, shake well, ice bath is placed after 30 minutes and is filtered immediately, with ice-cold spirit of vinegar 10ml gradation washing container and residue, filter, merging filtrate is regulated PH to 8～9 with strong ammonia solution, extracts 3 times with the ether jolting, each 20ml merges ether solution, volatilizes, and residue adds methanol makes dissolving, put in the 10ml measuring bottle, add methanol and be diluted to scale, shake up, filter, get subsequent filtrate, promptly;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly;
The every 1g of this ointment contains Rhizoma Corydalis with tetrahydropalmatine C
21H
25NO
4Meter must not be less than 0.15mg.
7. according to the method for quality control of the described ointment for the treatment of dysmenorrhea of claim 2, it is characterized in that: described method of quality control is: character, discriminating, inspection and assay project; Concrete grammar is:
Character: ointment is the emulsifiable paste of sundown, gas fragrance; Patch is the circular patch of pastille not;
Differentiate: (1) gets this ointment 4g, adds water 200ml and spirit of vinegar 2ml, connects volatile oil determination apparatus, the heating distillating extracting oil, and oil mass no longer increases to the determinator; Divide and get volatile oil, add ethyl acetate and make the solution that every 1ml contains 20 μ l, as need testing solution; Other gets the oil of Rhizoma Zingiberis Recens reference substance, adds ethyl acetate and makes solution that every 1ml contains 5 μ l product solution in contrast; According to an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: ether=9: 1 be developing solvent, launches, and takes out, and dries, and sprays with the dinitrophenylhydrazine test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(2) get Rhizoma Curcumae Longae control medicinal material 0.5g, the 20ml that adds diethyl ether, supersound process 20 minutes filters, and filtrate volatilizes, and residue adds methanol 1ml makes dissolving, in contrast medical material solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography, draw each the 10 μ l of need testing solution under control medicinal material solution and discriminating (1) item, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: ether=9: 1 is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution of new system, and 105 ℃ to be heated 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;
(3) get this ointment 2g, add spirit of vinegar 15ml, shake well is put water-bath and was placed 15 minutes, filter immediately, filtrate is regulated PH to 8～9 with strong ammonia solution, uses ether 20ml, and jolting is extracted, branch is got ether solution and is volatilized, and residue adds ethanol 1ml makes dissolving, as need testing solution; Other gets Fructus Evodiae control medicinal material 0.2g, adds ethanol 10ml, and supersound process 20 minutes filters, and filtrate is medical material solution in contrast; According to the test of an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with n-butyl alcohol: acetic acid: the upper solution of water=2: 1: 1 is developing solvent, launches, and takes out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
(4) get the tetrahydropalmatine reference substance, add methanol and make the solution that every 1ml contains 0.4mg, in contrast product solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography, draw need testing solution and each 10 μ l of above-mentioned reference substance solution of differentiating under (3) item, put respectively on the silica gel g thin-layer plate of same usefulness 1% sodium hydroxide solution preparation, with normal hexane: chloroform: methanol=7.5: 4: 1 is developing solvent, launch, take out, dry, it is smoked clear to the speckle colour developing to put in the iodine vapor; Inspect under the daylight, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color; After waving the iodine vapor that adsorbs on the most plate, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
Check: heavy metal is got this ointment 1.0g, presses an appendix IX of Chinese Pharmacopoeia version in 2000 the E second method inspection, contains heavy metal and must not cross 20/1000000ths;
Other should meet relevant every regulation under an appendix IR of Chinese Pharmacopoeia version in 2000 the ointment item;
Assay: shine an appendix VI of Chinese Pharmacopoeia version in 2000 D high effective liquid chromatography for measuring:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol: PH is that 7.4 phosphate buffer=60: 40 is mobile phase; The detection wavelength is 280nm; Number of theoretical plate calculates by the tetrahydropalmatine peak should be not less than 2000;
It is an amount of that the preparation precision of reference substance solution takes by weighing the tetrahydropalmatine reference substance, adds methanol and make the solution that every 1ml contains 0.1mg, promptly;
The 6g content is got in the preparation of need testing solution, mixing, and accurate the title, decide, and puts in the conical flask, add spirit of vinegar 30ml, shake well, ice bath is placed after 30 minutes and is filtered immediately, with ice-cold spirit of vinegar 10ml gradation washing container and residue, filter, merging filtrate is regulated PH to 8～9 with strong ammonia solution, extracts 3 times with the ether jolting, each 20ml merges ether solution, volatilizes, and residue adds methanol makes dissolving, put in the 10ml measuring bottle, add methanol and be diluted to scale, shake up, filter, get subsequent filtrate, promptly;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly;
The every 1g of this ointment contains Rhizoma Corydalis with tetrahydropalmatine C
21H
25NO
4Meter must not be less than 0.15mg.
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| 延胡索渗漉提取工艺的优选. 桑彤，谢培德.基层中药杂志，第14卷第3期. 2000 * |
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