CN1895438B - Chinese-medicinal composition for treating cephalagia and its preparation - Google Patents
Chinese-medicinal composition for treating cephalagia and its preparation Download PDFInfo
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Abstract
A Chinese medicine in the form of capsule, pill, tablet, oral liquid, etc for treating various types of headache is prepared from 15 Chinese-medicinal materials including Chuan-xiong rhizome, white peony root, Chinese angelica root, peach kernel, etc. Its preparing process is also disclosed.
Description
Technical field
The present invention relates to a kind of Chinese medicine composition and preparation method thereof and quality determining method, particularly a kind of Chinese medicine composition for the treatment of headache and preparation method thereof and quality determining method.
Background technology
Headache is common clinically disease, is found in multiple acute and chronic diseases.Primary disease is equivalent to the headaches that disease occurred such as migraine, tension headache, cluster headache, chronic paroxysmal hemicrania or infective fever of modern medicine.Chinese medical discrimination is cards such as wind and cold headache, headache due to blood stasis, headache due to deficiency of blood.The present composition cures mainly the headache of card such as wind and cold, blood stasis, blood deficiency, and two more than ten years of clinical practice, determined curative effect, side effect are little, are the Chinese patent medicines that the treatment chronic headache is welcome by the patient deeply.
Summary of the invention
The object of the invention is to provide the preparation method of a kind of Chinese medicine composition and preparation thereof, and another purpose of the present invention is to provide the quality determining method and the purposes of this Chinese medicinal composition preparation.
The present invention seeks to be achieved through the following technical solutions:
The crude drug of Chinese medicine composition of the present invention is composed as follows:
Ramulus Uncariae Cum Uncis 300-360 weight portion Rhizoma Chuanxiong 260-330 weight portion Herba Ephedrae 120-200 weight portion
Herba Asari 120-200 weight portion Radix Aconiti Lateralis Preparata 120-200 weight portion Radix Paeoniae Alba 150-250 weight portion
Rhizoma Et Radix Notopterygii 120-200 weight portion Radix Angelicae Pubescentis 60-150 weight portion Radix Saposhnikoviae 120-200 weight portion
Radix Rehmanniae 120-200 weight portion Radix Angelicae Sinensis 120-200 weight portion Caulis Spatholobi 450-550 weight portion
Semen Persicae 60-150 weight portion Flos Carthami 60-150 weight portion Radix Angelicae Dahuricae 120-200 weight portion.
The preferred weight proportioning of above-mentioned raw materials medicine is as follows:
Ramulus Uncariae Cum Uncis 336 weight portion Rhizoma Chuanxiongs 303 weight portion Herba Ephedraes 168 weight portions
Herba Asari 168 weight portion Radix Aconiti Lateralis Preparatas (system) the 168 weight portion Radix Paeoniae Albas 201 weight portions
Rhizoma Et Radix Notopterygii 168 weight portion Radix Angelicae Pubescentiss 102 weight portion Radix Saposhnikoviaes 168 weight portions
Radix Rehmanniae 168 weight portion Radix Angelicae Sinensis 168 weight portion Caulis Spatholobis 507 weight portions
The Semen Persicae 102 weight portion Flos Carthamis 102 weight portion Radixs Angelicae Dahuricae 168 weight portions
The preferred weight proportioning of above-mentioned raw materials medicine is as follows:
Ramulus Uncariae Cum Uncis 310 weight portion Rhizoma Chuanxiongs 330 weight portion Herba Ephedraes 125 weight portions
The Herba Asari 190 weight portion Radix Aconiti Lateralis Preparatas 130 weight portion Radix Paeoniae Albas 240 weight portions
Rhizoma Et Radix Notopterygii 125 weight portion Radix Angelicae Pubescentiss 150 weight portion Radix Saposhnikoviaes 135 weight portions
Radix Rehmanniae 195 weight portion Radix Angelicae Sinensis 140 weight portion Caulis Spatholobis 545 weight portions
The Semen Persicae 65 weight portion Flos Carthamis 145 weight portion Radixs Angelicae Dahuricae 130 weight portions.
The preferred weight proportioning of above-mentioned raw materials medicine is as follows:
Ramulus Uncariae Cum Uncis 355 weight portion Rhizoma Chuanxiongs 260 weight portion Herba Ephedraes 200 weight portions
The Herba Asari 120 weight portion Radix Aconiti Lateralis Preparatas 185 weight portion Radix Paeoniae Albas 150 weight portions
Rhizoma Et Radix Notopterygii 200 weight portion Radix Angelicae Pubescentiss 60 weight portion Radix Saposhnikoviaes 195 weight portions
Radix Rehmanniae 125 weight portion Radix Angelicae Sinensis 180 weight portion Caulis Spatholobis 450 weight portions
The Semen Persicae 150 weight portion Flos Carthamis 65 weight portion Radixs Angelicae Dahuricae 175 weight portions.
Traditional Chinese medicinal composition raw materials of the present invention adds conventional adjuvant, according to common process, makes clinical acceptable forms, as: capsule, pill, tablet, granule, oral liquid formulations or injection.
Above-mentioned Radix Aconiti Lateralis Preparata can be Radix Aconiti Lateralis Preparata.
The concrete preparation technology of the present composition is as follows:
Get Flos Carthami powder and be broken into fine powder, sieve; Ramulus Uncariae Cum Uncis is ground into coarse powder, uses 60%-80% alcohol dipping 2-4 time, and each 20-30 hour, filter, filtrate recycling ethanol is condensed into thick paste, and drying under reduced pressure below 70 ℃ is ground into thin dried cream powder; 13 flavors such as medicinal residues and all the other Radix Paeoniae Albas decoct with water each 1-3 hour 2-4 time, collect distilled volatile oil simultaneously, decocting liquid filters, and the clear paste that it is 1.05-1.15 that filtrate decompression is concentrated into 80-85 ℃ of relative density adds ethanol and makes and contain the alcohol amount and be 50%-70%, leave standstill, divide and get supernatant, decompression recycling ethanol concentrates, drying is ground into thin dried cream powder; The beta-cyclodextrin inclusion compound that volatile oil is doubly measured with 6-8, with above-mentioned two kinds of thin dried cream powders, Flos Carthami fine powder mix homogeneously, add conventional adjuvant, according to common process, make clinical acceptable forms, as: capsule, pill, tablet, granule, oral liquid or injection.
The preferred for preparation technology of the present composition is as follows:
Get Flos Carthami powder and be broken into fine powder, sieve; Ramulus Uncariae Cum Uncis is ground into coarse powder, with 75% alcohol dipping secondary, and each 24 hours, filter, filtrate recycling ethanol is condensed into thick paste, and drying under reduced pressure below 70 ℃ is ground into thin dried cream powder; 13 flavors such as medicinal residues and all the other Radix Paeoniae Albas decoct with water secondary, each 2 hours, collect distilled volatile oil simultaneously, decocting liquid filters, and it is 1.10 clear paste that filtrate decompression is concentrated into 85 ℃ of relative densities, adds ethanol and makes that to contain the alcohol amount be 60%, leave standstill, divide and get supernatant, decompression recycling ethanol concentrates, drying is ground into thin dried cream powder; Volatile oil with above-mentioned two kinds of thin dried cream powders, Flos Carthami fine powder mix homogeneously, is used 90% alcohol granulation with the beta-cyclodextrin inclusion compound of 7 times of amounts, and drying incapsulates, promptly.
Quality determining method of the present invention comprises following discriminating and/or assay
Discrimination method comprises one or more in the following discriminating:
A. the compositions of getting it filled is put microscopically and observed: pollen grain is ball-type or class is round, three germinal aperatures of tool, and outer wall has dentation;
B. compositions content 5.6g gets it filled, put in the cable type extractor according, moistening with ammonia, 50ml adds diethyl ether, reflux 4 hours, ether solution volatilizes, and residue adds 10% sulfuric acid solution 20ml makes dissolving, more than the reuse ammonia adjust pH to 10, extract with chloroform 20ml, divide and get chloroform solution, steam to about 2ml, as need testing solution; Other is hook taking rattan control medicinal material 4g, add 80% alcohol dipping 24 hours, filter the filtrate evaporate to dryness, residue adds ammonia 2ml dissolving, extract with ether 20ml, divide and get ether solution, volatilize, residue adds 10% sulfuric acid solution 20ml dissolving, press the need testing solution preparation method,, shine medical material solution in pairs with legal system from " more than the reuse ammonia adjust pH to 10 ".An appendix VIB is according to the thin layer chromatography test for Chinese Pharmacopoeia version in 2000, draws each 5 μ l of above-mentioned two kinds of solution, puts respectively on same silica gel g thin-layer plate, with 50: 30: 0.1 chloroform-acetone-ammonia was developing solvent, launched, and took out, dry, spray is with rare bismuth potassium iodide test solution; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
C. the compositions content 5g that gets it filled, it is moistening to add ammonia, adds chloroform 20ml again, and supersound process 20 minutes filters, and filtrate evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Other gets Herba Ephedrae control medicinal material 2g, shines medical material solution in pairs with legal system; Get the ephedrine hydrochloride reference substance again, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution; An appendix VIB is according to the thin layer chromatography test for Chinese Pharmacopoeia version in 2000, drawing each 5 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with 20: 5: 0.1 chloroform-methanol-ammonia, launch, take out, dry, spray is with ninhydrin solution, it is clear to dry by the fire to the speckle colour developing at 105 ℃, in the test sample chromatograph, respectively with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle of same color;
D. the compositions content 5g that gets it filled adds methanol 60ml, and supersound process 10 minutes filters, residue washs with methanol 10ml, and merging filtrate and washing liquid are used 60-90 ℃ of Petroleum ether extraction 2 times, each 50ml, merge petroleum ether liquid, be concentrated into about 2ml, as need testing solution; Other gets Herba Asari control medicinal material 2g, adds methanol 60ml, puts in the water-bath reflux 30 minutes, puts coldly, filters, and filtrate is with 60-90 ℃ of Petroleum ether extraction 2 times, and each 50ml merges petroleum ether liquid, is concentrated into about 2ml, makes control medicinal material solution.According to the 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 60-90 ℃ of 17: 1 petroleum ether-ethyl acetate is developing solvent, launches, and takes out, dry, spray is with 2% vanillin sulfuric acid solution, and it is clear to be heated to speckle colour developing at 100 ℃; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
E. the compositions content 1g that gets it filled adds methanol 30ml, supersound process 15 minutes, filter, filtrate evaporate to dryness, residue add water 50ml dissolving, with chloroform extraction 3 times, each 30ml discards chloroform solution, water layer is with water saturated n-butanol extraction 4 times, each 30ml merges n-butyl alcohol liquid, with the saturated water 50ml washing of n-butyl alcohol, divide and get n-butyl alcohol liquid, evaporate to dryness, residue add water 20ml makes dissolving, filters, the filtrate evaporate to dryness, residue adds ethyl acetate 30ml makes dissolving, filters the filtrate evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution.Other gets Radix Paeoniae Alba control medicinal material 1.5g, adds water 50ml and decocts 1 hour, filters, the saturated n-butanol extraction of filtrate water 3 times, each 30ml merges n-butanol extracting liquid, with the saturated water 50ml washing of n-butyl alcohol, divide and get n-butyl alcohol liquid, evaporate to dryness, residue adds water 20ml makes dissolving, filters the filtrate evaporate to dryness, residue adds ethyl acetate 30ml makes dissolving, filters the filtrate evaporate to dryness, residue adds methanol 1ml makes dissolving, makes control medicinal material solution; Get the peoniflorin reference substance again, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution; According to the thin layer chromatography test, draw each 2 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with 7: 1 ethyl acetate-methanol, launch, take out, to dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to dry by the fire to the speckle colour developing at 105 ℃; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle of same color;
F. the compositions content 5g that gets it filled adds water 20ml, adds 60-90 ℃ of petroleum ether 20ml again, and supersound process 25 minutes is divided and got petroleum ether layer, and evaporate to dryness, residue add chloroform 1ml makes dissolving, as need testing solution; Other gets Radix Angelicae Pubescentis control medicinal material 1g, shines medical material solution in pairs with legal system; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with 60-90 ℃ of 6: 3 petroleum ether-ethyl acetate, launch, take 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.
Aconitine limit is checked: precision takes by weighing this product content 3.0g, puts in the tool plug conical flask 70ml that adds diethyl ether, jolting 10 minutes, add ammonia solution 10ml again, jolting 30 minutes was placed 2 hours, divided and got ether solution, volatilize, residue adds dehydrated alcohol 2ml makes dissolving, as need testing solution.Other gets the aconitine reference substance, adds dehydrated alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution.Test according to thin layer chromatography (2000 editions appendix VIG of Chinese Pharmacopoeia), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate-dehydrated alcohol-ammonia (15: 5: 1: 0.1) be developing solvent, launch, take out, dry, spray is with bismuth potassium iodide test solution.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, the speckle of appearance should or speckle not occur less than the speckle of reference substance.
Assay in the quality determining method is as follows:
According to high performance liquid chromatography:
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; 20: 80 acetonitrile-waters are mobile phase; The detection wavelength is 230nm; Number of theoretical plate calculates by the peoniflorin peak should be not less than 8000;
The preparation of reference substance solution: it is an amount of to get the peoniflorin reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 0.1mg, shakes up, promptly;
The preparation of need testing solution: the content under the compositions content uniformity of the getting it filled item, mixing is got 2g, the accurate title, decide, and adds water 100ml, claims to decide weight, supersound process 15 minutes is put coldly, claims to decide weight again, water is supplied the weight that subtracts mistake, filters, and measures subsequent filtrate 25ml, add chloroform and extract 2 times, each 20ml discards chloroform solution, water layer is with water saturated n-butanol extraction 4 times, and each 30ml merges n-butanol extracting liquid, sodium chloride solution 10ml washing with saturated divides and gets n-butyl alcohol liquid, adds anhydrous sodium sulfate 8g, jolting filters the filtrate evaporate to dryness, the residue dissolve with methanol, and be transferred in the 10ml measuring bottle, add methanol and be diluted to scale, shake up, promptly; Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly; Every of pharmaceutical composition contains the Radix Paeoniae Alba with peoniflorin C
23H
28O
11Meter must not be less than 1.1mg.
Composition capsule group 101 examples, compositions pill matched group 99 examples are carried out clinical trial.Wherein Chinese medical discrimination belongs to liver-wind syndrome 126 examples (composition capsule group 67 examples, compositions pill matched group 59 examples), blood stasis symptom 73 examples (composition capsule group 33 examples, compositions pill matched group 40 examples).Western medicine diagnose belongs to migraine 119 examples (composition capsule group 56 examples, compositions pill matched group 63 examples), repeated relapsing tension headache 81 examples (composition capsule group 45 examples, compositions pill matched group 36 examples).Experimental result shows: composition capsule treatment headache clinic control rate is 21.78%, and obvious effective rate is 56.43%, and effective percentage is 17.82%, and inefficiency is 3.96%, and total effective rate is 96.03%, does not have significant difference with compositions pill matched group total effects.Clinic control rate+obvious effective rate (78.21%) is better than compositions pill matched group (66.66%).
Following experiment and embodiment are used to further specify but are not limited to the present invention.
Experimental example 1 treatment migraine and repeated relapsing tension headache belong to the clinical efficacy experiment of liver-wind syndrome and blood stasis symptom
One, physical data
Three tame hospitals treat 200 examples altogether, I medicine group (composition capsule group) 101 examples wherein, II medicine group (compositions pill group) 99 examples.Wherein Chinese medical discrimination belongs to liver-wind syndrome 126 examples (I medicine group 67 examples, II medicine group 59 examples), blood stasis symptom 73 examples (I medicine group 33 examples, II medicine group 40 examples).Western medicine diagnose belongs to migraine 119 examples (I medicine group 56 examples, II medicine group 63 examples), repeated relapsing tension headache 81 examples (I medicine group 45 examples, II medicine group 36 examples).
Two, two groups of comparabilities are checked
1, between two groups age and sex relatively see Table 1.The not statistically significant though two groups of ages and sex are variant.
Sick kind, pattern of syndrome are relatively between table 1 liang group
△：t＝1.0321 p＝0.3033
☆：X
2＝0.1624 p＝0.6869
2, sickly between two groups plant, pattern of syndrome relatively see Table 2.Sick kind, pattern of syndrome there was no significant difference between two groups.
Sick kind, pattern of syndrome are relatively between table 2 liang group
△：t＝1.3919 p＝0.2381
☆：X
2＝1.1742 p＝0.2785
3, three sick constituent ratios of planting of hospital see Table 3.Three sick constituent ratios of planting of hospital are than there was no significant difference.
Three hospitals of table 3 are sick plants constituent ratio
4, three hospital's syndrome constituent ratios see Table 4.Three hospital's syndrome constituent ratios are than there was no significant difference.
Three hospitals of table 4 syndrome constituent ratio
5, between two groups the course of disease, the state of an illness relatively see Table 5.The course of disease, state of an illness there was no significant difference between two groups.
The course of disease, the state of an illness are relatively between table 5 liang group
Three, efficacy analysis
1, the headache clinical efficacy relatively sees Table 6 between two groups.Have a headache between two groups, I medicine group clinical recovery+obvious effective rate (%) is 78.21%, is better than II medicine group 66.66%.
The comparison of headache clinical efficacy between table 6 liang group
Ridit checks X
2=3.5809 p=0.0584
2, the migraine clinical efficacy relatively sees Table 7 between two groups.There were significant differences for the treatment migraine between two groups, and I medicine group clinical recovery+obvious effective rate (%) is 78.57%, is better than II medicine group 60.32%.
The comparison of headache clinical efficacy between table 7 liang group
Ridit checks X
2=8.5345 p=0.0035
3, repeated relapsing tension headache clinical efficacy relatively sees Table 8 between two groups.
Repeated relapsing tension headache clinical efficacy relatively between table 8 liang group
Ridit checks X
2=0.0296 p=0.8633
4, total syndrome clinical efficacy compares between two groups, sees Table 9.
Syndrome clinical efficacy total between table 9 liang group compares
Ridit checks X
2=0.6436 p=0.4224
5, different syndrome clinical efficacies relatively see Table and treat liver-wind syndrome, blood stasis symptom between 10 liang of groups there are no significant difference between two groups.
Different syndrome clinical efficacies relatively between table 10 liang group
6, clinical symptoms improvement situation sees Table 11 pairs and treats liver-wind syndromes between two groups, and the I medicine has been compared extremely significant difference with II medicine treatment 2,4 all clinical symptoms and before treating.To the treatment blood stasis symptom, before treating 2,4 all clinical symptoms and treat, the I medicine compared extremely significant difference, and the II medicine has been compared significant differences before treating 2 weeks, 4 all clinical symptoms and treatment.
Clinical symptoms is improved situation between table 11 liang group
Four, discussion and conclusion
Three tame hospitals treat 200 examples altogether, I medicine group 101 examples wherein, II medicine group 99 examples, the analysis of comparable result shows between group, physical data between I medicine group and the II medicine group, the course of disease, the state of an illness, and sick the kind, no significant differences such as pattern of syndrome distribution, comparability is better between the prompting group, two groups have harmony. in addition, disease kind between three hospitals, the syndrome constituent ratio is there was no significant difference also, has comparability.
I medicine group and II medicine group treatment headache curative effect there was no significant difference, wherein I medicine group is treated headache clinical recovery 21.78%, produce effects 56.43%, effective percentage 17.82%, total effective rate 96.03%, II medicine group treatment headache clinical recovery 14.14%, produce effects 52.52%, effective percentage 25.25%, total effective rate 91.91%, prompting I medicine and II medicine treatment headache therapeutic equivalence; I medicine group clinical recovery+obvious effective rate (%) is 78.21% simultaneously, is better than II medicine group 66.66%.
I medicine group and II medicine group treatment migraine curative effect have significant difference, wherein I medicine group treatment migraine clinical recovery 23.21%, produce effects 55.36%, effective percentage 17.86%, total effective rate 96.43%, II medicine group treatment migraine clinical recovery 12.70%, produce effects 47.62%, effective percentage 28.57%, total effective rate 88.89%, prompting I medicine treatment migraine curative effect is better than the II medicine. and two groups suitable to repeated relapsing tension headache clinical efficacy.
Syndrome between two groups (liver-wind syndrome, blood stasis symptom) does not have significant difference though clinical efficacy is compared, and compares before and after the treatment, and to the treatment liver-wind syndrome, I medicine and II medicine were treated for 2 weeks (course of treatment), 4 weeks (two courses of treatment) clinical symptoms extremely that significance improves; To the treatment blood stasis symptom, I medicine treatment 2,4 all clinical symptoms also have extremely significance improvement.The II medicine treated for 2 weeks, 4 all clinical symptoms with the treatment before compared the highly significant property improvement.Prompting I medicine and II medicine have significant curative effect for improving the liver-wind syndrome headache clinical symptoms, and therapeutic equivalence, are better than the II medicine slightly and headache due to blood stasis I medicine is improved the clinical symptoms effect.
Security inspection shows, I medicine group or II medicine group treatment front and back, and routine blood test, electrocardiogram, liver, renal function does not all have obvious influence, does not see that untoward reaction takes place yet.Dry mouth with bitter taste occurs after having 1 routine patient to take medicine 2 days in I medicine group 101 examples, handling employing need not drug withdrawal.Illustrate that pharmaceutical composition has no side effect substantially, safe and reliable.
Can think that to sum up I medicine and II medicine treatment headache all has better curative effect, I medicine treatment migraine curative effect is better than the II medicine, to repeated relapsing tension headache therapeutic equivalence; I medicine and II medicine have significant curative effect for improving the liver-wind syndrome headache clinical symptoms, and therapeutic equivalence, are better than the II medicine slightly and headache due to blood stasis I medicine is improved the clinical symptoms effect.
The clinical efficacy experiment of experimental example 2 treatment cervical vertebra headaches
One, physical data,
This research has qualified experimenter's 60 examples, I medicine group 30 examples, II medicine group 30 examples.Differential diagnosis in tcm is the headache due to blood stasis card, and Western medicine diagnose is the cervical vertebra headache.Outpatient's 20 examples, inpatient's 40 examples.
Two, comparability inspection before the treatment:
1, two groups of preceding sex ratios of treatment
Sex ratio before the table 12 liang group treatment
X2＝0.268 P＝0.605
Two groups of sex ratios, no significant difference (P＞0.05).
2, two groups of preceding ages of treatment relatively
Age comparison before the table 13 liang group treatment (year)
X2＝1.352 P＝0.509
Two groups of age ratios, no significant difference.
3, two groups of preceding courses of disease of treatment distribute relatively
The course of disease distributes relatively (moon) before the table 14 liang group treatment
X
2＝0.857 P＝0.836
Two groups of courses of disease compare there was no significant difference.
4, two groups of preceding pulse ratios of treatment
The comparison of pulse before the table 15 liang group treatment
Treat preceding pulse ratios, no significant difference for two groups.
5, two groups of preceding blood pressures of treatment relatively
The comparison of blood pressure before the table 16 liang group treatment
X
2＝1.714 P＝0.190
Previously treat comparison, there was no significant difference for two groups.
6, previously treat relatively before two groups of treatments
The previously comparison of treatment before the table 17 liang group treatment
X2＝1.714 P＝0.190
Previously treat comparison, there was no significant difference for two groups.
7, before two groups of treatments the state of an illness relatively see Table 17-1
Treatment front pain pain intensity, seizure frequency, the comparison of persistent period between two groups of 17-1 of table
Two groups of headache pain intensities, seizure frequency, persistent period are compared no significant difference.
Headache character and characteristics are relatively before two groups of treatments of table 17-2
X2＝4.650 P＝0.325
The characteristics of two groups of headache character compare there was no significant difference.
Feel sick the comparison of symptoms such as poor appetite before two groups of treatments of table 17-3
Feel sick before two groups of treatments, poor appetite, phonophobia, photophobia, aversion to wind, aversion to cold, the aggravation of chance wind, local tenderness, feeling of numbness, restriction of neck motion system, other symptom comparison such as dizzy, no significant difference.
8, the comparison of two groups of preceding symptom integral of treatment
The comparison of symptom integral before the table 18 liang group treatment
Two groups of symptom integral compare there was no significant difference.
9, two groups of preceding body of the tongues of treatment relatively
Body of the tongue relatively before the table 19 liang group treatment
X
2＝1.740 P＝0.783
Two groups of body of the tongues compare no significant difference.
10, two groups of preceding tongue furs of treatment relatively
Tongue fur relatively before the table 20 liang group treatment
X
2＝0.661 P＝0.719
Two groups of tongue furs compare no significant difference.
11, two groups of preceding pulse conditions of treatment relatively
Pulse condition relatively before the table 21 liang group treatment
X2＝4.342 P＝0.362
Two groups of pulse conditions compare no significant difference.
Comparability detects and shows before the above-mentioned treatment: two groups of sexes, age, the course of disease, pulse, blood pressure, the pasts treat, headache pain intensity, seizure frequency, persistent period, headache character and characteristics, feel sick, poor appetite, phonophobia, photophobia, aversion to wind, aversion to cold, the aggravation of chance wind, local tenderness, feeling of numbness, restriction of neck motion system, symptom such as dizzy, aspects such as symptom integral and body of the tongue, tongue fur, pulse condition relatively, difference there are no significant meaning; The principal element that prompting influences two groups of curative effects has harmony, shows that two groups have comparability.
Three, efficacy analysis
1, total effects analysis
This research has qualified experimenter's 60 examples, I medicine group 30 examples, II medicine group 30 examples.The curative effect of treatment cervical spondylosis headache is as follows
Table 22 liang group total effects relatively
I medicine group II medicine group compares: U=1.189 P=0.234
Above result shows: after around the treatment, I medicine group clinic control rate is 16.67%, and obvious effective rate is 33.33%, and effective percentage is 13.33%, and inefficiency is: 6.67; II medicine group clinic control rate is 16.67%, and obvious effective rate is: 20.0%, and effective percentage is 43.33%, inefficiency is 20.0%.Credit is analysed by statistics, clinical efficacy there was no significant difference between two groups, and prompting I medicine group curative effect is suitable with II medicine group.
2, two groups of treatment back state of an illness relatively
Two groups of treatments of table 22-1 back pain pain intensity, seizure frequency, the comparison of persistent period
Two groups treat two weeks, all around after, headache pain intensity, seizure frequency, persistent period, difference that there are no significant
Table 22-2 two groups of treatment backs headache character and characteristics are relatively
Two groups treat two weeks, all around after, headache character and characteristics relatively, there was no significant difference.
The comparison of transference cure rates (%) such as table 22-3 feels sick two groups of treatment backs, poor appetite
Two groups of two weeks of treatment back, compare all around, remove around the local tenderness after, I medicine group is improved and is better than II medicine group and has outside the significant difference, all the other symptoms relatively, difference that there are no significant.
3, two groups of treatment back symptom integral relatively sees Table 23-1
The comparison of two groups of treatment backs of table 23-1 symptom integral
In two groups of treatment two weeks of back, compare the symptom integral there was no significant difference all around.
The comparison of symptom integral before and after two groups of treatments of table 23-2
In two weeks before and after two groups of treatments, self compares all around, and symptom integral all has significant difference
4, the comparison of two groups of pain relieving onset times sees Table 24
The comparison of table 24 liang group pain relieving onset time (my god)
Relatively there is significant difference two groups of onset times, and I medicine group onset time is fast than II medicine group.
5, two groups of treatment front and back body of the tongues relatively
Body of the tongue relatively before and after the table 25 liang group treatment
Body of the tongue compares difference that there are no significant before and after two groups of treatments.
6, two groups of treatment front and back tongue furs relatively
Tongue fur relatively before and after the table 26 liang group treatment
Tongue fur compares difference that there are no significant before and after two groups of treatments.
7, two groups of treatment front and back pulse conditions relatively
Pulse condition relatively before and after the table 27 liang group treatment
Pulse condition compares difference that there are no significant before and after two groups of treatments.
Four, discussion and conclusion
This research has qualified experimenter's 60 examples, I medicine group 30 examples, and II medicine group 30 examples, Chinese medical discrimination is the headache due to blood stasis card, Western medicine diagnose is the cervical vertebra headache. outpatient's 20 examples, inpatient's 40 examples.
Comparability detects: treat preceding two groups of sexes, age, the course of disease, pulsation, blood pressure, previously treatment, headache pain intensity, seizure frequency, persistent period, headache character and characteristics, feel sick poor appetite, phonophobia, photophobia, aversion to wind, aversion to cold is met the wind aggravation, local tenderness, feeling of numbness, restriction of neck motion system, symptom such as dizzy, symptom integral and body of the tongue, tongue fur, aspects such as pulse condition relatively, difference there are no significant meaning, the principal element that prompting influences two groups of curative effects has harmony, shows that two groups have comparability.
Clinical efficacy: after around the treatment, I medicine clinic control rate is 16.67%, and obvious effective rate is 33.33%, and effective percentage is 43.33%, and inefficiency is 6.67%; II medicine group clinic control rate is 16.67%, and obvious effective rate is 20.0%, effective percentage 43.33%, and inefficiency is 20.0%.Credit is analysed by statistics, clinical efficacy there was no significant difference between two groups, and prompting I medicine group curative effect is suitable with II medicine group.
Symptom, sign curative effect:
Two groups treat two weeks, all around after, headache pain intensity, seizure frequency, persistent period, headache character and characteristics relatively, difference that there are no significant;
Two groups of two weeks of treatment back, compare all around, improve except that back I medicine group around the local tenderness and be better than the II medicine group, all the other symptoms relatively, difference that there are no significant.
In two groups of treatment two weeks of back, compare the symptom integral there was no significant difference all around; Two weeks before and after two groups of treatments, all around self relatively, symptom integral all has significant difference.
Body of the tongue, tongue fur, pulse condition compare difference that there are no significant before and after two groups of treatments.
Above symptom, Signs efficacy result prompting I medicine group curative effect are fast than II medicine group.
Can think that to sum up I medicine and II medicine treatment cervical vertebra headache all has better curative effect, can significantly improve clinical symptoms, the two therapeutic equivalence, clinical practice safety.I medicine pain relieving onset time is fast than the II medicine.
Experimental example 3 paeoniflorin content determination experiments
Instrument and reagent:
High performance liquid chromatograph: Waters-510 type pump, U6K injector, 486 UV-detector
Acetonitrile: chromatographic grade, water: ultra-pure water, other reagent are analytical pure, and assay is provided by Nat'l Pharmaceutical ﹠ Biological Products Control Institute with the peoniflorin reference substance.
Chromatographic column: Dalian Chemistry and Physics Institute country chromatograph center μ Bondapak C18 post, 4.6 * 200mm, filler granularity 10 μ m flow velocity: 1ml/ minute, detect wavelength: be dissolved in measured result in the mobile phase according to bibliographical information and peoniflorin, be defined as 230nm.See Fig. 1.
Elution requirement: acetonitrile-water (20: 80), with this understanding, peoniflorin can effectively separate with adjacent chromatographic peak.
1, the linear investigation:
The preparation precision of standard solution takes by weighing peoniflorin reference substance 10.5mg, places in the 100ml measuring bottle, adds methanol to scale, shakes up.Promptly.
Regression equation calculation is got above-mentioned standard solution 4,6,8,10,12 μ l and is injected high performance liquid chromatograph, measure peoniflorin reference substance peak integrated value by above-mentioned chromatographic condition, with the integrated value is vertical coordinate, and the reference substance amount of injection is an abscissa, sees Fig. 2 as standard curve:
2, stability test:
After the need testing solution preparation finishes, every the certain hour sample introduction once, record peoniflorin peak integrated value.
Result of the test shows that need testing solution is all stable in a couple of days.
Table 28
3, precision test:
Get same need testing solution, continuous sample introduction five times, record peoniflorin peak integrated value.Result of the test shows that this method has good precision.
Table 29
4, repeatability test:
Get lot number and be 20020503 composition capsule sample, be equipped with need testing solution, repeat five times by [assay] below legal system.Get each 10 μ l of need testing solution of five preparations respectively, inject high performance liquid chromatograph, calculate content.Result of the test shows that this method has good repeatability.
Table 30
5, recovery test:
Take the application of sample absorption method.It is 20020503 composition capsule (content is the 1.34mg/ grain) the about 1.0g of content that precision takes by weighing lot number, add every ml and contain 1.05mg peoniflorin methanol solution 2.5ml, rise and operate from " the accurate title decides ... " down according to [assay] item as method, calculate the peoniflorin total amount, and by the following formula calculate recovery rate, the result shows in the table, and this method has the good response rate.
Table 31
6, sample test result:
Get ten batch samples, measure by method under [assay] item respectively, and calculate with following formula:
Wherein:
A
i=test sample integrated value A
s=reference substance integrated value
C
s=reference substance solution concentration (mg/ml)
The measurement result of ten batch samples is as shown in the table.
Table 32 sample size measurement result (mg/ grain)
Description of drawings
Fig. 1 peoniflorin is dissolved in the uv-spectrogram in the mobile phase.
Fig. 2 peoniflorin has good linear relationship in the scope of 0.42-1.26 μ g.
Following embodiment all can realize the effect of above-mentioned experimental example.
The specific embodiment
Embodiment 1: the preparation of granule
Ramulus Uncariae Cum Uncis 336kg Rhizoma Chuanxiong 303kg Herba Ephedrae 168kg
Herba Asari 168kg Radix Aconiti Lateralis Preparata (system) 168kg Radix Paeoniae Alba 201kg
Rhizoma Et Radix Notopterygii 168kg Radix Angelicae Pubescentis 102kg Radix Saposhnikoviae 168kg
Radix Rehmanniae 168kg Radix Angelicae Sinensis 168kg Caulis Spatholobi 507kg
Semen Persicae 102kg Flos Carthami 102kg Radix Angelicae Dahuricae 168kg
Get Flos Carthami powder and be broken into fine powder, sieve; Ramulus Uncariae Cum Uncis is ground into coarse powder, with 75% alcohol dipping secondary, and each 24 hours, filter, filtrate recycling ethanol is condensed into thick paste, and drying under reduced pressure below 70 ℃ is ground into thin dried cream powder; 13 flavors such as medicinal residues and all the other Radix Paeoniae Albas decoct with water secondary, each 2 hours, collect distilled volatile oil simultaneously, decocting liquid filters, and it is 1.10 clear paste that filtrate decompression is concentrated into 80 ℃ of relative densities, adds ethanol and makes that to contain the alcohol amount be 60%, leave standstill, divide and get supernatant, decompression recycling ethanol concentrates, drying is ground into thin dried cream powder; Volatile oil with above-mentioned two kinds of thin dried cream powders, Flos Carthami fine powder mix homogeneously, adds conventional auxiliary materials and mixing with the beta-cyclodextrin inclusion compound of 7 times of amounts, granulates, and drying, promptly.
Embodiment 2: the preparation of capsule
Ramulus Uncariae Cum Uncis 310kg Rhizoma Chuanxiong 330kg Herba Ephedrae 125kg
Herba Asari 190kg Radix Aconiti Lateralis Preparata 130kg Radix Paeoniae Alba 240kg
Rhizoma Et Radix Notopterygii 125kg Radix Angelicae Pubescentis 150kg Radix Saposhnikoviae 135kg
Radix Rehmanniae 195kg Radix Angelicae Sinensis 140kg Caulis Spatholobi 545kg
Semen Persicae 65kg Flos Carthami 145kg Radix Angelicae Dahuricae 130kg.
Get Flos Carthami powder and be broken into fine powder, sieve; Ramulus Uncariae Cum Uncis is ground into coarse powder, with 75% alcohol dipping 2 times, and each 24 hours, filter, filtrate recycling ethanol is condensed into thick paste, and drying under reduced pressure below 70 ℃ is ground into thin dried cream powder; 13 flavors such as medicinal residues and all the other Radix Paeoniae Albas decoct with water each 2 hours 2 times, collect distilled volatile oil simultaneously, decocting liquid filters, and it is 1.10 clear paste that filtrate decompression is concentrated into 85 ℃ of relative densities, adds ethanol and makes that to contain the alcohol amount be 60%, leave standstill, divide and get supernatant, decompression recycling ethanol concentrates, drying is ground into thin dried cream powder; Volatile oil with above-mentioned two kinds of thin dried cream powders, Flos Carthami fine powder mix homogeneously, is used 90% alcohol granulation with the beta-cyclodextrin inclusion compound of 7 times of amounts, and drying incapsulates, and makes 1000, promptly.
Embodiment 3: the preparation of pill
Ramulus Uncariae Cum Uncis 355kg Rhizoma Chuanxiong 260kg Herba Ephedrae 200kg
Herba Asari 120kg Radix Aconiti Lateralis Preparata 185kg Radix Paeoniae Alba 150kg
Rhizoma Et Radix Notopterygii 200kg Radix Angelicae Pubescentis 60kg Radix Saposhnikoviae 195kg
Radix Rehmanniae 125kg Radix Angelicae Sinensis 180kg Caulis Spatholobi 450kg
Semen Persicae 150kg Flos Carthami 65kg Radix Angelicae Dahuricae 175kg.
With the present invention's ten five tastes medical materials, be ground into fine powder, sieve, mixing is used water pill, and drying is used the active carbon coating, polishing, drying, promptly.
Embodiment 4: the preparation of tablet
Ramulus Uncariae Cum Uncis 336kg Rhizoma Chuanxiong 303kg Herba Ephedrae 168kg
Herba Asari 168kg Radix Aconiti Lateralis Preparata (system) 168kg Radix Paeoniae Alba 201kg
Rhizoma Et Radix Notopterygii 168kg Radix Angelicae Pubescentis 102kg Radix Saposhnikoviae 168kg
Radix Rehmanniae 168kg Radix Angelicae Sinensis 168kg Caulis Spatholobi 507kg
Semen Persicae 102kg Flos Carthami 102kg Radix Angelicae Dahuricae 168kg
Get Flos Carthami powder and be broken into fine powder, sieve; Ramulus Uncariae Cum Uncis is ground into coarse powder, with 75% alcohol dipping secondary, and each 24 hours, filter, filtrate recycling ethanol is condensed into thick paste, and drying under reduced pressure below 70 ℃ is ground into fine powder; 13 flavors such as medicinal residues and all the other Radix Paeoniae Albas decoct with water secondary, each 2 hours, collect distilled volatile oil simultaneously, decocting liquid filters, and it is 1.10 clear paste that filtrate decompression is concentrated into 80 ℃ of relative densities, adds ethanol and makes that to contain the alcohol amount be 60%, leave standstill, divide and get supernatant, decompression recycling ethanol concentrates, drying is ground into fine powder; Volatile oil with above-mentioned thin dried cream powder, Flos Carthami fine powder mix homogeneously, adds conventional auxiliary materials and mixing with the beta-cyclodextrin inclusion compound of 7 times of amounts, makes granule, tabletting, promptly.
Embodiment 5: the preparation of oral liquid
Ramulus Uncariae Cum Uncis 310kg Rhizoma Chuanxiong 330kg Herba Ephedrae 125kg
Herba Asari 190kg Radix Aconiti Lateralis Preparata 130kg Radix Paeoniae Alba 240kg
Rhizoma Et Radix Notopterygii 125kg Radix Angelicae Pubescentis 150kg Radix Saposhnikoviae 135kg
Radix Rehmanniae 195kg Radix Angelicae Sinensis 140kg Caulis Spatholobi 545kg
Semen Persicae 65kg Flos Carthami 145kg Radix Angelicae Dahuricae 130kg.
The hook taking rattan is ground into coarse powder, with 75% alcohol dipping secondary, each 24 hours, filters filtrate recycling ethanol; 14 flavors such as medicinal residues and all the other Radix Paeoniae Albas decoct with water secondary, each 2 hours, collect distilled volatile oil simultaneously, decocting liquid filters, and it is 1.10 clear paste that filtrate decompression is concentrated into 85 ℃ of relative densities, adds ethanol and makes that to contain the alcohol amount be 60%, leaves standstill, divide and get supernatant, decompression recycling ethanol is risen extracting solution with hook and is merged, the volatile oil of collecting is dissolved in the medicinal liquid, adds appropriate amount of auxiliary materials, add water and adjust volume, stir evenly, supernatant is got in cold preservation 48 hours, embedding, sterilization, promptly.
Embodiment 6: the discrimination method in the quality testing
Getting the compositions of embodiment 2 differentiates:
Discrimination method comprises one or more in the following discriminating:
A. the compositions of getting it filled is put microscopically and observed: pollen grain is ball-type or class is round, three germinal aperatures of tool, and outer wall has dentation;
B. compositions content 5.6g gets it filled, put in the cable type extractor according, moistening with ammonia, 50ml adds diethyl ether, reflux 4 hours, ether solution volatilizes, and residue adds 10% sulfuric acid solution 20ml makes dissolving, more than the reuse ammonia adjust pH to 10, extract with chloroform 20ml, divide and get chloroform solution, steam to about 2ml, as need testing solution; Other is hook taking rattan control medicinal material 4g, add 80% alcohol dipping 24 hours, filter the filtrate evaporate to dryness, residue adds ammonia 2ml dissolving, extract with ether 20ml, divide and get ether solution, volatilize, residue adds 10% sulfuric acid solution 20ml dissolving, press the need testing solution preparation method,, shine medical material solution in pairs with legal system from " more than the reuse ammonia adjust pH to 10 ".An appendix VIB is according to the thin layer chromatography test for Chinese Pharmacopoeia version in 2000, draws each 5 μ l of above-mentioned two kinds of solution, puts respectively on same silica gel g thin-layer plate, with 50: 30: 0.1 chloroform-acetone-ammonia was developing solvent, launched, and took out, dry, spray is with rare bismuth potassium iodide test solution; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
C. the compositions content 5g that gets it filled, it is moistening to add ammonia, adds chloroform 20ml again, and supersound process 20 minutes filters, and filtrate evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Other gets Herba Ephedrae control medicinal material 2g, shines medical material solution in pairs with legal system; Get the ephedrine hydrochloride reference substance again, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution; An appendix VIB is according to the thin layer chromatography test for Chinese Pharmacopoeia version in 2000, drawing each 5 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with 20: 5: 0.1 chloroform-methanol-ammonia, launch, take out, dry, spray is with ninhydrin solution, it is clear to dry by the fire to the speckle colour developing at 105 ℃, in the test sample chromatograph, respectively with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle of same color;
D. the compositions content 5g that gets it filled adds methanol 60ml, and supersound process 10 minutes filters, residue washs with methanol 10ml, and merging filtrate and washing liquid are used 60-90 ℃ of Petroleum ether extraction 2 times, each 50ml, merge petroleum ether liquid, be concentrated into about 2ml, as need testing solution; Other gets Herba Asari control medicinal material 2g, adds methanol 60ml, puts in the water-bath reflux 30 minutes, puts coldly, filters, and filtrate is with 60-90 ℃ of Petroleum ether extraction 2 times, and each 50ml merges petroleum ether liquid, is concentrated into about 2ml, makes control medicinal material solution.According to the 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 60-90 ℃ of 17: 1 petroleum ether-ethyl acetate is developing solvent, launches, and takes out, dry, spray is with 2% vanillin sulfuric acid solution, and it is clear to be heated to speckle colour developing at 100 ℃; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
E. the compositions content 1g that gets it filled adds methanol 30ml, supersound process 15 minutes, filter, filtrate evaporate to dryness, residue add water 50ml dissolving, with chloroform extraction 3 times, each 30ml discards chloroform solution, water layer is with water saturated n-butanol extraction 4 times, each 30ml merges n-butyl alcohol liquid, with the saturated water 50ml washing of n-butyl alcohol, divide and get n-butyl alcohol liquid, evaporate to dryness, residue add water 20ml makes dissolving, filters, the filtrate evaporate to dryness, residue adds ethyl acetate 30ml makes dissolving, filters the filtrate evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution.Other gets Radix Paeoniae Alba control medicinal material 1.5g, adds water 50ml and decocts 1 hour, filters, the saturated n-butanol extraction of filtrate water 3 times, each 30ml merges n-butanol extracting liquid, with the saturated water 50ml washing of n-butyl alcohol, divide and get n-butyl alcohol liquid, evaporate to dryness, residue adds water 20ml makes dissolving, filters the filtrate evaporate to dryness, residue adds ethyl acetate 30ml makes dissolving, filters the filtrate evaporate to dryness, residue adds methanol 1ml makes dissolving, makes control medicinal material solution; Get the peoniflorin reference substance again, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution; According to the thin layer chromatography test, draw each 2 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with 7: 1 ethyl acetate-methanol, launch, take out, to dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to dry by the fire to the speckle colour developing at 105 ℃; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle of same color;
F. the compositions content 5g that gets it filled adds water 20ml, adds 60-90 ℃ of petroleum ether 20ml again, and supersound process 25 minutes is divided and got petroleum ether layer, and evaporate to dryness, residue add chloroform 1ml makes dissolving, as need testing solution; Other gets Radix Angelicae Pubescentis control medicinal material 1g, shines medical material solution in pairs with legal system; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with 60-90 ℃ of 6: 3 petroleum ether-ethyl acetate, launch, take 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;
[inspection] aconitine limit precision takes by weighing this product content 3.0g, puts in the tool plug conical flask 70ml that adds diethyl ether, jolting 10 minutes, add ammonia solution 10ml again, jolting 30 minutes was placed 2 hours, divided and got ether solution, volatilize, residue adds dehydrated alcohol 2ml makes dissolving, as need testing solution.Other gets the aconitine reference substance, adds dehydrated alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution.Test according to thin layer chromatography (2000 editions appendix VIG of Chinese Pharmacopoeia), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate-dehydrated alcohol-ammonia (15: 5: 1: 0.1) be developing solvent, launch, take out, dry, spray is with bismuth potassium iodide test solution.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, the speckle of appearance should or speckle not occur less than the speckle of reference substance.
Embodiment 7: the content assaying method in the quality testing
Get the compositions of embodiment 3 and carry out assay:
According to high performance liquid chromatography:
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; 20: 80 acetonitrile-waters are mobile phase; The detection wavelength is 230nm; Number of theoretical plate calculates by the peoniflorin peak should be not less than 8000;
The preparation of reference substance solution: it is an amount of to get the peoniflorin reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 0.1mg, shakes up, promptly;
The preparation of need testing solution: the content under the compositions content uniformity of the getting it filled item, mixing is got 2g, the accurate title, decide, and adds water 100ml, claims to decide weight, supersound process 15 minutes is put coldly, claims to decide weight again, water is supplied the weight that subtracts mistake, filters, and measures subsequent filtrate 25ml, add chloroform and extract 2 times, each 20ml discards chloroform solution, water layer is with water saturated n-butanol extraction 4 times, and each 30ml merges n-butanol extracting liquid, sodium chloride solution 10ml washing with saturated divides and gets n-butyl alcohol liquid, adds anhydrous sodium sulfate 8g, jolting filters the filtrate evaporate to dryness, the residue dissolve with methanol, and be transferred in the 10ml measuring bottle, add methanol and be diluted to scale, shake up, promptly;
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
Every of pharmaceutical composition contains the Radix Paeoniae Alba with peoniflorin (C
23H
28O
11) meter, must not be less than 1.1mg.
Embodiment 8: quality determining method
Get the compositions of embodiment 1 and carry out quality testing
Discrimination method comprises one or more in the following discriminating:
A. the compositions of getting it filled is put microscopically and observed: pollen grain is ball-type or class is round, three germinal aperatures of tool, and outer wall has dentation;
B. compositions content 5.6g gets it filled, put in the cable type extractor according, moistening with ammonia, 50ml adds diethyl ether, reflux 4 hours, ether solution volatilizes, and residue adds 10% sulfuric acid solution 20ml makes dissolving, more than the reuse ammonia adjust pH to 10, extract with chloroform 20ml, divide and get chloroform solution, steam to about 2ml, as need testing solution; Other is hook taking rattan control medicinal material 4g, add 80% alcohol dipping 24 hours, filter the filtrate evaporate to dryness, residue adds ammonia 2ml dissolving, extract with ether 20ml, divide and get ether solution, volatilize, residue adds 10% sulfuric acid solution 20ml dissolving, press the need testing solution preparation method,, shine medical material solution in pairs with legal system from " more than the reuse ammonia adjust pH to 10 ".An appendix VIB is according to the thin layer chromatography test for Chinese Pharmacopoeia version in 2000, draws each 5 μ l of above-mentioned two kinds of solution, puts respectively on same silica gel g thin-layer plate, with 50: 30: 0.1 chloroform-acetone-ammonia was developing solvent, launched, and took out, dry, spray is with rare bismuth potassium iodide test solution; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
C. the compositions content 5g that gets it filled, it is moistening to add ammonia, adds chloroform 20ml again, and supersound process 20 minutes filters, and filtrate evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Other gets Herba Ephedrae control medicinal material 2g, shines medical material solution in pairs with legal system; Get the ephedrine hydrochloride reference substance again, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution; An appendix VIB is according to the thin layer chromatography test for Chinese Pharmacopoeia version in 2000, drawing each 5 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with 20: 5: 0.1 chloroform-methanol-ammonia, launch, take out, dry, spray is with ninhydrin solution, it is clear to dry by the fire to the speckle colour developing at 105 ℃, in the test sample chromatograph, respectively with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle of same color;
D. the compositions content 5g that gets it filled adds methanol 60ml, and supersound process 10 minutes filters, residue washs with methanol 10ml, and merging filtrate and washing liquid are used 60-90 ℃ of Petroleum ether extraction 2 times, each 50ml, merge petroleum ether liquid, be concentrated into about 2ml, as need testing solution; Other gets Herba Asari control medicinal material 2g, adds methanol 60ml, puts in the water-bath reflux 30 minutes, puts coldly, filters, and filtrate is with 60-90 ℃ of Petroleum ether extraction 2 times, and each 50ml merges petroleum ether liquid, is concentrated into about 2ml, makes control medicinal material solution.According to the 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 60-90 ℃ of 17: 1 petroleum ether-ethyl acetate is developing solvent, launches, and takes out, dry, spray is with 2% vanillin sulfuric acid solution, and it is clear to be heated to speckle colour developing at 100 ℃; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
E. the compositions content 1g that gets it filled adds methanol 30ml, supersound process 15 minutes, filter, filtrate evaporate to dryness, residue add water 50ml dissolving, with chloroform extraction 3 times, each 30ml discards chloroform solution, water layer is with water saturated n-butanol extraction 4 times, each 30ml merges n-butyl alcohol liquid, with the saturated water 50ml washing of n-butyl alcohol, divide and get n-butyl alcohol liquid, evaporate to dryness, residue add water 20ml makes dissolving, filters, the filtrate evaporate to dryness, residue adds ethyl acetate 30ml makes dissolving, filters the filtrate evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution; Other gets Radix Paeoniae Alba control medicinal material 1.5g, adds water 50ml and decocts 1 hour, filters, the saturated n-butanol extraction of filtrate water 3 times, each 30ml merges n-butanol extracting liquid, with the saturated water 50ml washing of n-butyl alcohol, divide and get n-butyl alcohol liquid, evaporate to dryness, residue adds water 20ml makes dissolving, filters the filtrate evaporate to dryness, residue adds ethyl acetate 30ml makes dissolving, filters the filtrate evaporate to dryness, residue adds methanol 1ml makes dissolving, makes control medicinal material solution; Get the peoniflorin reference substance again, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution.According to the thin layer chromatography test, draw each 2 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with 7: 1 ethyl acetate-methanol, launch, take out, to dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to dry by the fire to the speckle colour developing at 105 ℃; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle of same color;
F. the compositions content 5g that gets it filled adds water 20ml, adds petroleum ether (60-90 ℃) 20ml again, and supersound process 25 minutes is divided and got petroleum ether layer, and evaporate to dryness, residue add chloroform 1ml makes dissolving, as need testing solution; Other gets Radix Angelicae Pubescentis control medicinal material 1g, shines medical material solution in pairs with legal system; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with 60-90 ℃ of 6: 3 petroleum ether-ethyl acetate, launch, take 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;
Aconitine limit is checked: precision takes by weighing this product content 3.0g, puts in the tool plug conical flask 70ml that adds diethyl ether, jolting 10 minutes, add ammonia solution 10ml again, jolting 30 minutes was placed 2 hours, divided and got ether solution, volatilize, residue adds dehydrated alcohol 2ml makes dissolving, as need testing solution.Other gets the aconitine reference substance, adds dehydrated alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution.Test according to thin layer chromatography (2000 editions appendix VIG of Chinese Pharmacopoeia), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate-dehydrated alcohol-ammonia (15: 5: 1: 0.1) be developing solvent, launch, take out, dry, spray is with bismuth potassium iodide test solution.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, the speckle of appearance should or speckle not occur less than the speckle of reference substance;
According to high performance liquid chromatography:
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; 20: 80 acetonitrile-waters are mobile phase; The detection wavelength is 230nm; Number of theoretical plate calculates by the peoniflorin peak should be not less than 8000;
The preparation of reference substance solution: it is an amount of to get the peoniflorin reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 0.1mg, shakes up, promptly;
The preparation of need testing solution: the content under the compositions content uniformity of the getting it filled item, mixing is got 2g, the accurate title, decide, and adds water 100ml, claims to decide weight, supersound process 15 minutes is put coldly, claims to decide weight again, water is supplied the weight that subtracts mistake, filters, and measures subsequent filtrate 25ml, add chloroform and extract 2 times, each 20ml discards chloroform solution, water layer is with water saturated n-butanol extraction 4 times, and each 30ml merges n-butanol extracting liquid, sodium chloride solution 10ml washing with saturated divides and gets n-butyl alcohol liquid, adds anhydrous sodium sulfate 8g, jolting filters the filtrate evaporate to dryness, the residue dissolve with methanol, and be transferred in the 10ml measuring bottle, add methanol and be diluted to scale, shake up, promptly;
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
Every of pharmaceutical composition contains the Radix Paeoniae Alba with peoniflorin (C
23H
28O
11) meter, must not be less than 1.1mg.
Claims (6)
1. the quality determining method of a pharmaceutical composition is characterized in that this method comprises following discrimination method:
D. the compositions content 5g that gets it filled adds methanol 60ml, and supersound process 10 minutes filters, and residue is with methanol 10ml washing, merging filtrate and washing liquid, and with 60-90 ℃ of Petroleum ether extraction 2 times, each 50ml merges petroleum ether liquid, is concentrated into 2ml, as need testing solution; Other gets Herba Asari control medicinal material 2g, adds methanol 60ml, puts in the water-bath reflux 30 minutes, puts coldly, filters, and filtrate is with 60-90 ℃ of Petroleum ether extraction 2 times, and each 50ml merges petroleum ether liquid, is concentrated into 2ml, makes control medicinal material solution; According to the 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 60-90 ℃ of petroleum ether-ethyl acetate is developing solvent at 17: 1, launches, and takes out, dry, spray is with 2% vanillin sulfuric acid solution, and it is clear to be heated to speckle colour developing at 100 ℃; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
E. the compositions content 1g that gets it filled adds methanol 30ml, supersound process 15 minutes, filter, filtrate evaporate to dryness, residue add water 50ml dissolving, with chloroform extraction 3 times, each 30ml discards chloroform solution, water layer is with water saturated n-butanol extraction 4 times, and each 30ml merges n-butyl alcohol liquid, with the saturated water 50ml washing of n-butyl alcohol, divide and get n-butyl alcohol liquid, evaporate to dryness, residue adds water 20ml makes dissolving, filters the filtrate evaporate to dryness, residue adds ethyl acetate 30ml makes dissolving, filters the filtrate evaporate to dryness, residue adds methanol 1ml makes dissolving, and as need testing solution, other gets Radix Paeoniae Alba control medicinal material 1.5g, add water 50ml and decocted 1 hour, filter, the saturated n-butanol extraction of filtrate water 3 times, each 30ml merges n-butanol extracting liquid, with the saturated water 50ml washing of n-butyl alcohol, divide and get n-butyl alcohol liquid, evaporate to dryness, residue add water 20ml makes dissolving, filter, filtrate evaporate to dryness, residue add ethyl acetate 30ml makes dissolving, filter, filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, makes control medicinal material solution; Get the peoniflorin reference substance again, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution; According to the thin layer chromatography test, draw each 2 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with 7: 1 ethyl acetate-methanol, launch, take out, to dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to dry by the fire to the speckle colour developing at 105 ℃; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle of same color;
F. the compositions content 5g that gets it filled adds water 20ml, adds 60-90 ℃ of petroleum ether 20ml again, and supersound process 25 minutes is divided and got petroleum ether layer, and evaporate to dryness, residue add chloroform 1ml makes dissolving, as need testing solution; Other gets Radix Angelicae Pubescentis control medicinal material 1g, shines medical material solution in pairs with legal system; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be at 6: 3 developing solvent with 60-90 ℃ of petroleum ether-ethyl acetate, launch, take 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;
The crude drug of wherein said pharmaceutical composition consists of:
Ramulus Uncariae Cum Uncis 300-360 weight portion Rhizoma Chuanxiong 260-330 weight portion Herba Ephedrae 120-200 weight portion
Herba Asari 120-200 weight portion Radix Aconiti Lateralis Preparata 120-200 weight portion Radix Paeoniae Alba 150-250 weight portion
Rhizoma Et Radix Notopterygii 120-200 weight portion Radix Angelicae Pubescentis 60-150 weight portion Radix Saposhnikoviae 120-200 weight portion
Radix Rehmanniae 120-200 weight portion Radix Angelicae Sinensis 120-200 weight portion Caulis Spatholobi 450-550 weight portion
Semen Persicae 60-150 weight portion Flos Carthami 60-150 weight portion Radix Angelicae Dahuricae 120-200 weight portion.
2. quality determining method as claimed in claim 1 is characterized in that the pharmaceutical composition in this quality determining method is capsule, pill, tablet, granule, oral liquid or injection.
3. quality determining method as claimed in claim 1 is characterized in that this method comprises following assay:
According to high performance liquid chromatography:
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; 20: 80 acetonitrile-waters are mobile phase; The detection wavelength is 230nm; Number of theoretical plate calculates by the peoniflorin peak should be not less than 8000;
The preparation of reference substance solution: it is an amount of to get the peoniflorin reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 0.1mg, shakes up, promptly;
The preparation of need testing solution: the content under the compositions content uniformity of the getting it filled item, mixing is got 2g, the accurate title, decide, and adds water 100ml, claims to decide weight, supersound process 15 minutes is put coldly, claims to decide weight again, water is supplied the weight that subtracts mistake, filters, and measures subsequent filtrate 25ml, add chloroform and extract 2 times, each 20ml discards chloroform solution, water layer is with water saturated n-butanol extraction 4 times, and each 30ml merges n-butanol extracting liquid, sodium chloride solution 10ml washing with saturated divides and gets n-butyl alcohol liquid, adds anhydrous sodium sulfate 8g, jolting filters the filtrate evaporate to dryness, the residue dissolve with methanol, and be transferred in the 10ml measuring bottle, add methanol and be diluted to scale, shake up, promptly;
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
Every of pharmaceutical composition contains the Radix Paeoniae Alba with peoniflorin C
23H
28O
11Meter must not be less than 1.1mg.
4. quality determining method as claimed in claim 1 is characterized in that the crude drug of the pharmaceutical composition described in this method consists of:
Ramulus Uncariae Cum Uncis 336 weight portion Rhizoma Chuanxiongs 303 weight portion Herba Ephedraes 168 weight portions
The Herba Asari 168 weight portion Radix Aconiti Lateralis Preparata 168 weight portion Radix Paeoniae Albas 201 weight portions
Rhizoma Et Radix Notopterygii 168 weight portion Radix Angelicae Pubescentiss 102 weight portion Radix Saposhnikoviaes 168 weight portions
Radix Rehmanniae 168 weight portion Radix Angelicae Sinensis 168 weight portion Caulis Spatholobis 507 weight portions
The Semen Persicae 102 weight portion Flos Carthamis 102 weight portion Radixs Angelicae Dahuricae 168 weight portions.
5. quality determining method as claimed in claim 1 is characterized in that the crude drug of the pharmaceutical composition described in this method consists of:
Ramulus Uncariae Cum Uncis 310 weight portion Rhizoma Chuanxiongs 330 weight portion Herba Ephedraes 125 weight portions
The Herba Asari 190 weight portion Radix Aconiti Lateralis Preparata 130 weight portion Radix Paeoniae Albas 240 weight portions
Rhizoma Et Radix Notopterygii 125 weight portion Radix Angelicae Pubescentiss 150 weight portion Radix Saposhnikoviaes 135 weight portions
Radix Rehmanniae 195 weight portion Radix Angelicae Sinensis 140 weight portion Caulis Spatholobis 545 weight portions
The Semen Persicae 65 weight portion Flos Carthamis 145 weight portion Radixs Angelicae Dahuricae 130 weight portions.
6. quality determining method as claimed in claim 1 is characterized in that the crude drug of the pharmaceutical composition described in this method consists of:
Ramulus Uncariae Cum Uncis 355 weight portion Rhizoma Chuanxiongs 260 weight portion Herba Ephedraes 200 weight portions
The Herba Asari 120 weight portion Radix Aconiti Lateralis Preparata 185 weight portion Radix Paeoniae Albas 150 weight portions
Rhizoma Et Radix Notopterygii 200 weight portion Radix Angelicae Pubescentiss 60 weight portion Radix Saposhnikoviaes 195 weight portions
Radix Rehmanniae 125 weight portion Radix Angelicae Sinensis 180 weight portion Caulis Spatholobis 450 weight portions
The Semen Persicae 150 weight portion Flos Carthamis 65 weight portion Radixs Angelicae Dahuricae 175 weight portions.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2006100869686A CN1895438B (en) | 2006-06-21 | 2006-06-21 | Chinese-medicinal composition for treating cephalagia and its preparation |
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| CN2006100869686A CN1895438B (en) | 2006-06-21 | 2006-06-21 | Chinese-medicinal composition for treating cephalagia and its preparation |
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| CN1895438B true CN1895438B (en) | 2010-12-08 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101647911B (en) * | 2009-09-08 | 2012-06-06 | 北京同仁堂科技发展股份有限公司 | Traditional Chinese medicine composite and preparation for treating headache and preparation method thereof |
| CN102091296B (en) * | 2011-01-24 | 2012-07-25 | 郭智义 | Medicament for treating breast hyperplasia |
| CN102698009A (en) * | 2012-05-16 | 2012-10-03 | 江苏苏南药业实业有限公司 | Medicine composition for treating migraine and preparation method thereof |
| CN103536698B (en) * | 2013-11-04 | 2015-08-12 | 华润三九医药股份有限公司 | The application of a kind of Chinese medicine composition in the medicine of preparation treatment vascular dementia |
| CN104606634A (en) * | 2015-01-22 | 2015-05-13 | 高歌 | Traditional Chinese medicine composition for treating hemicrania, and preparation method of traditional Chinese medicine composition |
| CN110794079A (en) * | 2019-11-20 | 2020-02-14 | 刘圣梅 | Identification method of ephedra and aconitine preparation |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1748747A (en) * | 2005-10-20 | 2006-03-22 | 北京润德康医药技术有限公司 | Chinese medicine compound medicinal preparation for pain killing of channels an dits preparing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1748747A (en) * | 2005-10-20 | 2006-03-22 | 北京润德康医药技术有限公司 | Chinese medicine compound medicinal preparation for pain killing of channels an dits preparing method |
Non-Patent Citations (1)
| Title |
|---|
| 国家药典委员会编.麻黄.中华人民共和国药典2000年版一部.化学工业出版社,2000,262. * |
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