CN100391504C - Pharmaceutical composition for treating sexual disorder and its preparation process - Google Patents
Pharmaceutical composition for treating sexual disorder and its preparation process Download PDFInfo
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- CN100391504C CN100391504C CNB2005100567624A CN200510056762A CN100391504C CN 100391504 C CN100391504 C CN 100391504C CN B2005100567624 A CNB2005100567624 A CN B2005100567624A CN 200510056762 A CN200510056762 A CN 200510056762A CN 100391504 C CN100391504 C CN 100391504C
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Abstract
The present invention discloses a medical composition for treating sexual disorders, which is prepared by the following raw material medicine: 10 to 30 parts by weight of epimedium, 2 to 7 parts by weight of ginseng, 5 to 20 parts by weight of pilose antler, 10 to 30 parts by weight of male moth, 10 to 30 parts by weight of wolfberry fruit, 5 to 20 parts by weight of dodder, 1 to 4 parts by weight of common cnidium fruit, 8 to 20 parts by weight of solomonseal rhizome, 10 to 30 parts by weight of philippine violet herb, and 20-80 parts by weight of plantain seed. The present invention can treat sexual disorders, namely that the medical composition improves the erection degree of a penis The medical composition is used for treating sexual disorders, and has the functions of increasing ejaculate volume, prolonging the erection time of a penis, and improving the erection degree of a penis.
Description
Invention field
The present invention relates to a kind of pharmaceutical composition and preparation method thereof, particularly relate to handicapped pharmaceutical composition of a kind of therapeutic and preparation method thereof
Background technology
World Health Organization (WHO) once added up and pointed out, the whole world has 6,000 ten thousand to 8,000 ten thousand couples of Mr. and Mrs to have fertility Issue, just a pair of problems such as infertile, sterile, sexual impotence, seminal emission, premature ejaculation or hyposexuality that exist are arranged the per 10 couples of Mr. and Mrs of China, wherein 5-10% is relevant with insufficiency of kidney-YANG, and this has had a strong impact on the healthy of people.Motherland's medical science to diseases such as sexual impotence due to insufficiency of kidney-YANG understanding early, theoretical explanation is deep.We pass through meticulous prescription on this basis, checking repeatedly, and the invention compositions of making has good the kidney invigorating, QI invigorating and warming YANG effect, is used for the treatment of sexual dysfunction.
Summary of the invention
The object of the invention is to provide a kind of therapeutic handicapped pharmaceutical composition; The object of the invention also is to provide a kind of preparation of drug combination method.
The present invention seeks to be achieved through the following technical solutions.
Pharmaceutical composition crude drug of the present invention consists of:
Herba Epimedii 10-30 weight portion Radix Ginseng 2-7 weight portion Cornu Cervi Pantotrichum 5-20 weight portion
Male Bombycis mori 10-30 weight portion Fructus Lycii 10-30 weight portion Semen Cuscutae 5-20 weight portion
Fructus Cnidii 1-4 weight portion Rhizoma Polygonati 8-20 weight portion Herba Violae 10-30 weight portion
Semen Plantaginis 20-80 weight portion
Pharmaceutical composition crude drug of the present invention is formed optimum ratio:
Herba Epimedii 18 weight portion Radix Ginsengs 5.5 weight portion Cornu Cervi Pantotrichums 10 weight portions
Male Bombycis mori 18 weight portion Fructus Lycii 18 weight portion Semen Cuscutae 11 weight portions
Fructus Cnidii 2 weight portion Rhizoma Polygonatis 14 weight portion Herba Violaes 18 weight portions
Semen Plantaginis 55 weight portions;
Herba Epimedii 15 weight portion Radix Ginsengs 6 weight portion Cornu Cervi Pantotrichums 7 weight portions
Male Bombycis mori 27 weight portion Fructus Lycii 13 weight portion Semen Cuscutae 17 weight portions
Fructus Cnidii 2 weight portion Rhizoma Polygonatis 18 weight portion Herba Violaes 14 weight portions
Semen Plantaginis 30 weight portions;
Herba Epimedii 25 weight portion Radix Ginsengs 3 weight portion Cornu Cervi Pantotrichums 17 weight portions
Male Bombycis mori 15 weight portion Fructus Lycii 25 weight portion Semen Cuscutae 7 weight portions
Fructus Cnidii 3 weight portion Rhizoma Polygonatis 12 weight portion Herba Violaes 25 weight portions
Semen Plantaginis 60 weight portions.
The invention described above pharmaceutical composition can be made clinical acceptable any dosage form, as pill, powder, capsule, granule, drop pill, oral liquid, injection etc.
Preparation of drug combination method of the present invention is:
Except that Fructus Lycii, all the other Herba Epimedii etc. nine flavor is ground into coarse powder; Flooded respectively 24-72 hour; Chinese liquor with 40-50% is made solvent, the independent percolation of Cornu Cervi Pantotrichum, and Fructus Lycii and Radix Ginseng be the device percolation in addition, and seven flavors such as all the other male Bombycis mori mix percolation, collect the liquid of filtering respectively, leave standstill; Filter, merge three kinds of liquid of filtering; Add conventional adjuvant, make clinical acceptable any dosage form, as pill, powder, capsule, granule, drop pill, oral liquid etc.
Method for optimizing is:
Except that Fructus Lycii, all the other Herba Epimedii etc. nine flavor is ground into coarse powder; Flooded respectively 48 hours; Chinese liquor with 45% is made solvent, the independent percolation of Cornu Cervi Pantotrichum, and Fructus Lycii and Radix Ginseng be the device percolation in addition, and seven flavors such as all the other male Bombycis mori mix percolation, with the speed percolation of per minute 1～3ml, collect the liquid of filtering respectively, leave standstill; Filter, merge three kinds of liquid of filtering; Add conventional adjuvant, make clinical acceptable any dosage form, as pill, powder, capsule, granule, drop pill, oral liquid etc.
The quality determining method of drug composition oral liquid preparation of the present invention comprises one or more that following discriminating is central:
Differentiate: a. gets preparation 50ml, puts in the water-bath and steams to about 10ml, adds water 20ml, changes in the separatory funnel, extracts with ether 30ml, divides water intaking liquid standby; Ether solution volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution.Other gets Fructus Lycii control medicinal material 2g, adds water 50ml, decocts 20 minutes, filters, and filtrate is extracted with ether 30ml jolting, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (attached VIB of Chinese Pharmacopoeia version in 2000), drawing each 10 μ l. of above-mentioned two kinds of solution puts respectively in same and contains on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is an adhesive, with benzene-ethyl acetate-formic acid (8: 5: 0.4) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
B. get water liquid ethyl acetate extraction 2 times of differentiating under a item, each 20ml merges ethyl acetate extraction liquid, evaporate to dryness, residue adds methanol 5ml makes dissolving, be added on the polyamide column handled well (internal diameter 1cm,, the high 10cm of post), with ethyl acetate 40ml eluting, collect eluent, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution.Other gets the icariin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000), draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same and contain on the silica GF254 lamellae that sodium carboxymethyl cellulose is an adhesive, with ethyl acetate-butanone-formic acid-water (10: 1: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (254nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
C. get preparation 50ml, put in the water-bath and steam to about 10ml, add water 30ml, mixing gets twice with ether, and each 30ml divides water intaking liquid standby; Merge ether solution, with 5% sodium carbonate liquor washing 2 times, each 30ml, branch is got ether solution, and low temperature volatilizes, and the residue 1ml that adds diethyl ether makes dissolving, as test solution.Other gets Fructus Cnidii control medicinal material 0.2g, the 20ml that adds diethyl ether, and reflux, extract, 10 minutes filters, and filtrate is concentrated into 1ml, in contrast medical material solution.Get the osthole reference substance again, add ethanol and make the solution that every 1ml contains 0.5mg, in contrast product solution.According to thin layer chromatography, (Chinese Pharmacopoeia one one of version in 2000 is paid record VIB) test, draw each 10 μ l of above-mentioned three kinds of solution, put respectively in same and contain on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is an adhesive, with benzene-ethyl acetate (30: 1) is developing solvent, launches, and takes out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
D. get and differentiate c item water liquid down, with water saturated n-butanol extraction 2 times, each 30ml merges n-butanol extracting liquid, washs 3 times with ammonia solution, at every turn 30ml; The water 30ml that the reuse n-butyl alcohol is saturated, washing once divide and get n-butyl alcohol liquid, evaporate to dryness, residue adds and contains 7% vitriolic 45% ethanol liquid 10ml, and reflux 1 hour changes in the evaporating dish, steam to there not being the alcohol flavor, add water to 10ml, use ether extraction 2 times, each 10ml, merge ether solution, evaporate to dryness, the residue 1ml that adds diethyl ether makes dissolving, as need testing solution.Other gets panoxadiol, panaxatriol's reference substance, add diethyl ether and make the mixed solution that contains 1mg among every 1ml, product solution is tested according to thin layer chromatography (appendix VlB of Chinese Pharmacopoeia version in 2000) in contrast, draw each 10 μ l of above-mentioned two kinds of solution, putting respectively in same and contain on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is an adhesive, is developing solvent with cyclohexane extraction-acetone (2: 1), launches, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color, put again under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
The quality determining method of drug composition oral liquid preparation of the present invention also comprises following assay: according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2000 measures).
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Acetonitrile: water (33: 67) is mobile phase; The detection wavelength is 270nm; Number of theoretical plate presses that the icariin peak calculates should be not 2000.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the icariin reference substance, adds the solution that 45% ethanol is made every 1ml icariin 25ug, promptly.
The preparation of need testing solution: precision is measured preparation 25ml, puts in the 100ml measuring bottle, adds 45% ethanol dilution to scale, shakes up, and filters, and gets subsequent filtrate, promptly.
Algoscopy: accurate respectively reference substance solution and need testing solution and each 10ul of need testing solution of drawing, inject chromatograph of liquid, measure, the every 1ml of preparation contains Herba Epimedii with icariin (C
33H
40O
15) meter, must not be less than 0.05mg.
The medicine that the present composition is made has the merit of the tonifying YANG of tonifying Qi of the kidney.Wherein medicated wine proves through central laboratory of Chengdu Traditional Chinese Medical College pharmacodynamics test, and preparation has extremely strong kidney invigorating and YANG supporting effect.Acute and chronic toxicity test proves, its safety non-toxic has carried out 60 routine clinical observations, determined curative effect on this basis.
Following experimental example and embodiment are used for explanation but are not limited to the present invention.
The clinical observation development test
Random packet is adopted in this test, is divided into treatment group and matched group, and ratio is 1: 1.
30 examples are organized in treatment, give oral medicated wine of the present invention, and every day, oral 50ml took five every day 1 time, altogether 250ml.Treatment group patient must not use the medicine of other treatment sexual impotence except that oral medicated wine of the present invention.
Matched group 30 examples, the longevity powder that giving oral Shanxi pharmaceutical factory of traditional Chinese medicine provides is spilt, and every day, oral 50ml took five days every day 1 time, altogether 250ml.The matched group patient also must not use the medicine of other treatment sexual impotence except that oral GUILINGJI JIU.The course of treatment: treatment group and matched group are five days the course of treatment, after the drug withdrawal, and observe the curative effect in 1 month.
Observed result is as follows
1. medicated wine of the present invention is to the influence (as shown in table 1) of clinical efficacy:
Table 1 medicated wine of the present invention is to the comparison of clinical efficacy influence
Observation group's produce effects 9 examples (accounting for 30%) after taking medicine as can be seen from Table 1, effective 16 examples (accounting for 53.3%), invalid 5 examples (accounting for 16.7%), total effective 25 examples, total effective rate is 83.3%; Matched group produce effects 4 examples (accounting for 13.3%), invalid 11 examples of effective 15 examples (50%) (accounting for 36.7%), total effective 19 examples, total effective rate is 63.3%.Observation group's matched group (P＜0.05) that is better than evident in efficacy is described.
2, medicated wine of the present invention is to the influence (as shown in table 2) of decline of the fire from the gate of life patient libido
Table 2 medicated wine of the present invention is to the comparison of decline of the fire from the gate of life patient libido influence
As can be seen from Table 2, the preceding two groups of decline of the fire from the gate of life patient libido situations of treatment compare there was no significant difference (P＞0.05).Treatment back observation group significantly is better than matched group (P＜0.05) to the improvement of decline of the fire from the gate of life patient libido.Single with regard to observation group, to the effect of having clear improvement of decline of the fire from the gate of life patient libido, there were significant differences (P＞0.05) for the treatment cross-reference at the forward and backward medicated wine of the present invention of treatment.
3, medicated wine of the present invention is to the influence (as shown in table 3) of decline of the fire from the gate of life patient erection degree
The influence of table 3 pair decline of the fire from the gate of life patient erection degree
As can be seen from Table 3, treat preceding two groups of decline of the fire from the gate of life patient erection degree and learn processing no significant difference (P＞0.05) by statistics, after treatment, observation group significantly is better than matched group (P＜0.05) to the improvement of decline of the fire from the gate of life patient erection degree.Relatively, can see decline of the fire from the gate of life patient erection being significantly improved after taking medicated wine of the present invention that contrast has utmost point significant difference (P＜0.01) before and after the treatment before and after the treatment of observation group.
4, medicated wine of the present invention is to the decline of the fire from the gate of life patient influence of erection time (as shown in table 4).
The influence of table 4 pair decline of the fire from the gate of life patient erection time
As can be seen from Table 4, before the treatment and two groups of decline of the fire from the gate of life patient erection times of treatment back more all do not have a significant difference (P＞0.05), but single with regard to before observation group's treatment and after the treatment more as can be seen, can make decline of the fire from the gate of life patient erection time significant prolongation after medicated wine of the present invention is oral, utmost point significant difference (P＜0.01) relatively be arranged with the treatment front and back.
5, medicated wine of the present invention is to the influence (as shown in table 5) of decline of the fire from the gate of life patient ejaculate volume.
The comparison of table 5 pair ejaculate volume effect
As can be seen from Table 5, the ejaculate volume that the decline of the fire from the gate of life patient of observation group takes after the medicated wine treatment of the present invention increases than having significantly before treating, and relatively there were significant differences (P＜0.05) in front and back.Observe and matched group patient's treatment before and after the ejaculate volume variation relatively do not have a significant difference (P＞0.05), increasing of ejaculate volume all arranged.
6, female benefit bank liquid is to the influence (as shown in table 6) of decline of the fire from the gate of life patient T and PRL.
The comparison of the influence of table 6 couple T and PRL
Table 6 prompting, experimental group treatment back serum testosterone is significantly higher than treatment preceding (P＜0.05), and more also there were significant differences with matched group.And serum prolactin also shows reduction in various degree for two groups, but treatment front and back and the result between two groups are relatively, no difference of science of statistics.
7, medicated wine of the present invention is to the influence (as shown in table 7) of decline of the fire from the gate of life patient cardinal symptom.
The influence of table 7 pair main tcm symptom
As can be seen from Table 7, observation group and matched group decline of the fire from the gate of life patient traditional Chinese medical science disease average integral relatively do not have significant difference (P＞0.05) before the treatment; The reduction marked difference of the treatment back decline of the fire from the gate of life patient of observation group traditional Chinese medical science disease average integral is in matched group, relatively there were significant differences (P＜0.05) between two groups, the decline of the fire from the gate of life patient of observation group traditional Chinese medical science disease integration after medicated wine treatment of the present invention significantly reduces before the treatment, and there were significant differences (P＜0.05) in the front and back contrast.
Conclusion: medicated wine treatment decline of the fire from the gate of life impotent patient total effective rate of the present invention is 83.3%, and relatively there were significant differences (P＜0.05) with matched group.Medicated wine of the present invention is to the effect of being significantly improved of decline of the fire from the gate of life patient libido, and there were significant differences (P＜0.05) in contrast before and after the treatment, and relatively there were significant differences (P＜0.05) with matched group.Medicated wine of the present invention can significantly improve decline of the fire from the gate of life patient erection degree, and contrast has utmost point significant difference (P＜0.01) before and after its treatment, and relatively there were significant differences (P＜0.05) with matched group.But medicated wine significant prolongation decline of the fire from the gate of life patient's erection time of the present invention, contrast has utmost point significant difference (P＜0.01) before and after its treatment, but does not relatively have significant difference (P＞0.05) with matched group.Medicated wine of the present invention can significantly increase decline of the fire from the gate of life patient ejaculate volume, and contrast has significant difference (P＜0.05) before and after its treatment, but compares there was no significant difference (P＞0.05) with matched group.Medicated wine of the present invention can significantly increase decline of the fire from the gate of life patient's serum testosterone value (T), relatively reaching and the photograph group more all had a significant difference (P＜0.05) before and after its treatment; Medicated wine of the present invention does not have significance to the influence of decline of the fire from the gate of life patient's serum prolactin value (PRL), does not more all have significant difference (P＞0.05) before and after its treatment and with matched group.The traditional Chinese medical science disease effects of being significantly improved such as medicated wine of the present invention is cold and cool to penis due to the decline of the fire from the gate of life, the acid of waist knee joint is cold, limbs fear of cold, spiritlessness and weakness, clear urine in large amounts and pale tongue, deep-thready pulse are slow, before and after its treatment and with matched group significant difference (P＜0.05) more all arranged.
Embodiment 1:The capsule preparation
Herba Epimedii 18g Radix Ginseng 5.5g Cornu Cervi Pantotrichum 10g male Bombycis mori 18g
Fructus Lycii 18g Semen Cuscutae 11g Fructus Cnidii 2g Rhizoma Polygonati 14g
Herba Violae 18g Semen Plantaginis 55g; Add conventional adjuvant and make capsule.
Embodiment 2:The drop pill preparation
Herba Epimedii 15g Radix Ginseng 6g Cornu Cervi Pantotrichum 7g male Bombycis mori 27g
Fructus Lycii 13g Semen Cuscutae 17g Fructus Cnidii 2g Rhizoma Polygonati 18g
Herba Violae 14g Semen Plantaginis 30g; Add adjuvant and make drop pill.
Embodiment 3:Preparation of granules
Herba Epimedii 25g Radix Ginseng 3g Cornu Cervi Pantotrichum 17g male Bombycis mori 15g
Fructus Lycii 25g Semen Cuscutae 7g Fructus Cnidii 3g Rhizoma Polygonati 12g
Herba Violae 25g Semen Plantaginis 60g; Add adjuvant and make granule.
Embodiment 4:The preparation of medicated wine
Herba Epimedii 18g Radix Ginseng 5.5g Cornu Cervi Pantotrichum 10g male Bombycis mori 18g
Fructus Lycii 18g Semen Cuscutae 11g Fructus Cnidii 2g Rhizoma Polygonati 14g
Herba Violae 18g Semen Plantaginis 55g
More than ten flavors, except that Fructus Lycii, all the other Herba Epimedii etc. nine flavor is ground into coarse powder.According to the percolation under fluid extract and the extractum item (appendix IO of Chinese Pharmacopoeia version in 2000), make solvent with 45% Chinese liquor, the independent percolation of Cornu Cervi Pantotrichum, Fructus Lycii and Radix Ginseng be the device percolation in addition, all the other male Bombycis mori etc. seven flavor mixes percolation, flood 48 hours respectively after, with the speed percolation of per minute 1～3ml, collect the liquid of filtering successively respectively, 120ml, 188ml, 692ml, leave standstill. filter, merge three kinds of liquid of filtering, with sucrose 40g, stir evenly, leave standstill-week, filter, add Chinese liquor (45v/v) and transfer to 1000ml, packing, promptly.
Embodiment 5:Quality determining method
Carry out quality testing as the embodiment 4 preparation present compositions:
Differentiate: a. gets preparation 50ml, puts in the water-bath and steams to about 10ml, adds water 20ml, changes in the separatory funnel, extracts with ether 30ml, divides water intaking liquid standby; Ether solution volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution.Other gets Fructus Lycii control medicinal material 2g, adds water 50ml, decocts 20 minutes, filters, and filtrate is extracted with ether 30ml jolting, shines medical material solution in pairs with legal system.According to thin layer chromatography (attached VIB of Chinese Pharmacopoeia version in 2000) test, draw each 10 μ l of above-mentioned two kinds of solution.Putting respectively in same and contain on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is an adhesive, is developing solvent with benzene-ethyl acetate-formic acid (8: 5: 0.4), launches, and takes out, and dries, and puts under the ultra-violet lamp (365nm) and inspects.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
B. get water liquid ethyl acetate extraction 2 times of differentiating under a item, each 20ml merges ethyl acetate extraction liquid, evaporate to dryness, residue adds methanol 5ml makes dissolving, be added on the polyamide column handled well (internal diameter 1cm,, the high 10cm of post), with ethyl acetate 40ml eluting, collect eluent, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution.Other gets the icariin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000), draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same and contain on the silica GF254 lamellae that sodium carboxymethyl cellulose is an adhesive, with ethyl acetate-butanone-formic acid-water (10: 1: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (254nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
C. get preparation 50ml, put in the water-bath and steam to about 10ml, add water 30ml, mixing gets twice with ether, and each 30ml divides water intaking liquid standby; Merge ether solution, with 5% sodium carbonate liquor washing 2 times, each 30ml, branch is got ether solution, and low temperature volatilizes, and the residue 1ml that adds diethyl ether makes dissolving, as test solution.Other gets Fructus Cnidii control medicinal material 0.2g, the 20ml that adds diethyl ether, and reflux, extract, 10 minutes filters, and filtrate is concentrated into 1ml, in contrast medical material solution.Get the osthole reference substance again, add ethanol and make the solution that every 1ml contains 0.5mg, in contrast product solution.According to thin layer chromatography, (Chinese Pharmacopoeia one one of version in 2000 is paid record VIB) test, draw each 10 μ l of above-mentioned three kinds of solution, put respectively in same and contain on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is an adhesive, with benzene-ethyl acetate (30: 1) is developing solvent, launches, and takes out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
D. get and differentiate c item water liquid down, with water saturated n-butanol extraction 2 times, each 30ml merges n-butanol extracting liquid, washs 3 times with ammonia solution, at every turn 30ml; The water 30ml that the reuse n-butyl alcohol is saturated, washing once divide and get n-butyl alcohol liquid, evaporate to dryness, residue adds and contains 7% vitriolic 45% ethanol liquid 10ml, and reflux 1 hour changes in the evaporating dish, steam to there not being the alcohol flavor, add water to 10ml, use ether extraction 2 times, each 10ml, merge ether solution, evaporate to dryness, the residue 1ml that adds diethyl ether makes dissolving, as need testing solution.Other gets panoxadiol, panaxatriol's reference substance, add diethyl ether and make the mixed solution that contains 1mg among every 1ml, product solution is tested according to thin layer chromatography (appendix VlB of Chinese Pharmacopoeia version in 2000) in contrast, draw each 10 μ l of above-mentioned two kinds of solution, putting respectively in same and contain on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is an adhesive, is developing solvent with cyclohexane extraction-acetone (2: 1), launches, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color, put again under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
Assay: according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2000 measures).
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Acetonitrile: water (33: 67) is mobile phase; The detection wavelength is 270nm; Number of theoretical plate presses that the icariin peak calculates should be not 2000.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the icariin reference substance, adds the solution that 45% ethanol is made every 1ml icariin 25ug, promptly.
The preparation of need testing solution: precision is measured preparation 25ml, puts in the 100ml measuring bottle, adds 45% ethanol dilution to scale, shakes up, and filters, and gets subsequent filtrate, promptly.
Algoscopy: accurate respectively reference substance solution and need testing solution and each 10ul of need testing solution of drawing, inject chromatograph of liquid, measure, the every 1ml of preparation contains Herba Epimedii with icariin (C
33H
40O
15) meter, must not be less than 0.05mg.
Embodiment 6:Quality determining method
Carry out quality testing as the embodiment 4 preparation present compositions:
Differentiate: a gets preparation 50ml, puts in the water-bath and steams to about 10ml, adds water 20ml, changes in the separatory funnel, extracts with ether 30ml, divides water intaking liquid standby; Ether solution volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution.Other gets Fructus Lycii control medicinal material 2g, adds water 50ml, decocts 20 minutes, filters, and filtrate is extracted with ether 30ml jolting, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (attached VIB of Chinese Pharmacopoeia version in 2000), drawing each 10 μ l. of above-mentioned two kinds of solution puts respectively in same and contains on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is an adhesive, with benzene-ethyl acetate-formic acid (8: 5: 0.4) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
B. get water liquid ethyl acetate extraction 2 times of differentiating under a item, each 20ml merges ethyl acetate extraction liquid, evaporate to dryness, residue adds methanol 5ml makes dissolving, be added on the polyamide column handled well (internal diameter 1cm,, the high 10cm of post), with ethyl acetate 40ml eluting, collect eluent, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution.Other gets the icariin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000), draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same and contain on the silica GF254 lamellae that sodium carboxymethyl cellulose is an adhesive, with ethyl acetate-butanone-formic acid-water (10: 1: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (254nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
C. get preparation 50ml, put in the water-bath and steam to about 10ml, add water 30ml, mixing gets twice with ether, and each 30ml divides water intaking liquid standby; Merge ether solution, with 5% sodium carbonate liquor washing 2 times, each 30ml, branch is got ether solution, and low temperature volatilizes, and the residue 1ml that adds diethyl ether makes dissolving, as test solution.Other gets Fructus Cnidii control medicinal material 0.2g, the 20ml that adds diethyl ether, and reflux, extract, 10 minutes filters, and filtrate is concentrated into 1ml, in contrast medical material solution.Get the osthole reference substance again, add ethanol and make the solution that every 1ml contains 0.5mg, in contrast product solution.According to thin layer chromatography, (Chinese Pharmacopoeia one one of version in 2000 is paid record VIB) test, draw each 10 μ l of above-mentioned three kinds of solution, put respectively in same and contain on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is an adhesive, with benzene-ethyl acetate (30: 1) is developing solvent, launches, and takes out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
Assay: according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2000 measures).
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Acetonitrile: water (33: 67) is mobile phase; The detection wavelength is 270nm; Number of theoretical plate presses that the icariin peak calculates should be not 2000.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the icariin reference substance, adds the solution that 45% ethanol is made every 1ml icariin 25ug, promptly.
The preparation of need testing solution: precision is measured preparation 25ml, puts in the 100ml measuring bottle, adds 45% ethanol dilution to scale, shakes up, and filters, and gets subsequent filtrate, promptly.
Algoscopy: accurate respectively reference substance solution and need testing solution and each 10ul of need testing solution of drawing, inject chromatograph of liquid, measure, the every 1ml of preparation contains Herba Epimedii with icariin (C
33H
40O
15) meter, must not be less than 0.05mg.
Claims (12)
1. handicapped pharmaceutical composition of therapeutic is characterized in that said composition made by following crude drug:
Herba Epimedii 10-30 weight portion Radix Ginseng 2-7 weight portion Cornu Cervi Pantotrichum 5-20 weight portion
Male Bombycis mori 10-30 weight portion Fructus Lycii 10-30 weight portion Semen Cuscutae 5-20 weight portion
Fructus Cnidii 1-4 weight portion Rhizoma Polygonati 8-20 weight portion Herba Violae 10-30 weight portion
Semen Plantaginis 20-80 weight portion.
2. pharmaceutical composition as claimed in claim 1 is characterized in that this pharmaceutical composition made by following crude drug:
Herba Epimedii 18 weight portion Radix Ginsengs 5.5 weight portion Cornu Cervi Pantotrichums 10 weight portions
Male Bombycis mori 18 weight portion Fructus Lycii 18 weight portion Semen Cuscutae 11 weight portions
Fructus Cnidii 2 weight portion Rhizoma Polygonatis 14 weight portion Herba Violaes 18 weight portions
Semen Plantaginis 55 weight portions.
3. pharmaceutical composition as claimed in claim 1 is characterized in that this pharmaceutical composition made by following crude drug:
Herba Epimedii 15 weight portion Radix Ginsengs 6 weight portion Cornu Cervi Pantotrichums 7 weight portions
Male Bombycis mori 27 weight portion Fructus Lycii 13 weight portion Semen Cuscutae 17 weight portions
Fructus Cnidii 2 weight portion Rhizoma Polygonatis 18 weight portion Herba Violaes 14 weight portions
Semen Plantaginis 30 weight portions.
4. pharmaceutical composition as claimed in claim 1 is characterized in that this pharmaceutical composition made by following crude drug:
Herba Epimedii 25 weight portion Radix Ginsengs 3 weight portion Cornu Cervi Pantotrichums 17 weight portions
Male Bombycis mori 15 weight portion Fructus Lycii 25 weight portion Semen Cuscutae 7 weight portions
Fructus Cnidii 3 weight portion Rhizoma Polygonatis 12 weight portion Herba Violaes 25 weight portions
Semen Plantaginis 60 weight portions.
5. as claim 1,2,3 or 4 described preparation of drug combination methods, it is characterized in that this method is:
Except that Fructus Lycii, Herba Epimedii, Radix Ginseng, Cornu Cervi Pantotrichum, male Bombycis mori, Semen Cuscutae, Fructus Cnidii, Rhizoma Polygonati, Herba Violae, Semen Plantaginis nine flavors are ground into coarse powder; Flooded respectively 24-72 hour; Chinese liquor with 40-50% is made solvent, the independent percolation of Cornu Cervi Pantotrichum, and Fructus Lycii and Radix Ginseng be the device percolation in addition, and male Bombycis mori, Herba Epimedii, Semen Cuscutae, Fructus Cnidii, Rhizoma Polygonati, Herba Violae, Semen Plantaginis seven flavors mix percolation, collect the liquid of filtering respectively, leave standstill; Filter, merge three kinds of liquid of filtering; Add conventional adjuvant, make clinical acceptable any dosage form, as pill, powder, capsule, granule, drop pill, oral liquid.
6. preparation of drug combination method as claimed in claim 5 is characterized in that this method is:
Except that Fructus Lycii, Herba Epimedii, Radix Ginseng, Cornu Cervi Pantotrichum, male Bombycis mori, Semen Cuscutae, Fructus Cnidii, Rhizoma Polygonati, Herba Violae, Semen Plantaginis nine flavors are ground into coarse powder; Flooded respectively 48 hours; Chinese liquor with 45% is made solvent, the independent percolation of Cornu Cervi Pantotrichum, and Fructus Lycii and Radix Ginseng be the device percolation in addition, male Bombycis mori, Herba Epimedii, Semen Cuscutae, Fructus Cnidii, Rhizoma Polygonati, Herba Violae, Semen Plantaginis seven flavors mix percolation, with the speed percolation of per minute 1～3ml, collect the liquid of filtering respectively, leave standstill; Filter, merge three kinds of liquid of filtering; Add conventional adjuvant, make clinical acceptable forms, as pill, powder, capsule, granule, drop pill, oral liquid.
7. as the quality determining method of the oral liquid of claim 1,2,3 or 4 described pharmaceutical compositions, it is characterized in that this method comprises one or more in the following discriminating:
Differentiate: a. gets preparation 50ml, puts and steams in the water-bath to 10ml, adds water 20ml, changes in the separatory funnel, extracts with ether 30ml, divides water intaking liquid standby; Ether solution volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Fructus Lycii control medicinal material 2g, adds water 50ml, decocts 20 minutes, filters, and filtrate is extracted with ether 30ml jolting, shines medical material solution in pairs with legal system; According to thin layer chromatography test, draw each 10 μ l. of above-mentioned two kinds of solution and put respectively in same and contain on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is an adhesive, be developing solvent with 8: 5: 0.4 benzene-ethyl acetate-formic acid, 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;
B. get water liquid ethyl acetate extraction 2 times of differentiating under a item, each 20ml, merge ethyl acetate extraction liquid, evaporate to dryness, residue add methanol 5ml makes dissolving, be added on the polyamide column that oneself handles well, with ethyl acetate 40ml eluting, collect eluent, evaporate to dryness, residue adds ethyl acetate 1ml makes dissolving, as need testing solution; Other gets the icariin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same and contain on the silica GF254 lamellae that sodium carboxymethyl cellulose is an adhesive, with 10: 1: 1 ethyl acetate-butanone-formic acid-water was developing solvent, launched, and took out, dry, put under the 254nm 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;
C. get preparation 50ml, put and steam in the water-bath to 10ml, add water 30ml, mixing gets twice with ether, and each 30ml divides water intaking liquid standby; Merge ether solution, with 5% sodium carbonate liquor washing 2 times, each 30ml, branch is got ether solution, and low temperature volatilizes, and the residue 1ml that adds diethyl ether makes dissolving, as test solution; Other gets Fructus Cnidii control medicinal material 0.2g, the 20ml that adds diethyl ether, and reflux, extract, 10 minutes filters, and filtrate is concentrated into 1ml, in contrast medical material solution; Get the osthole reference substance again, add ethanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; According to thin layer chromatography test, draw each 10 μ l of above-mentioned three kinds of solution, put respectively in same and contain on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is an adhesive, be developing solvent with 30: 1 benzene-ethyl acetates, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
D. get and differentiate c item water liquid down, with water saturated n-butanol extraction 2 times, each 30ml merges n-butanol extracting liquid, washs 3 times with ammonia solution, at every turn 30ml; The water 30ml that the reuse n-butyl alcohol is saturated, washing once divide and get n-butyl alcohol liquid, evaporate to dryness, residue adds and contains 7% vitriolic 45% ethanol liquid 10ml, and reflux 1 hour changes in the evaporating dish, steam to there not being the alcohol flavor, add water to 10ml, use ether extraction 2 times, each 10ml, merge ether solution, evaporate to dryness, the residue 1ml that adds diethyl ether makes dissolving, as need testing solution; Other gets panoxadiol, panaxatriol's reference substance, add diethyl ether and make the mixed solution that contains 1mg among every 1ml, product solution is tested according to thin layer chromatography in contrast, draw each 10 μ l of above-mentioned two kinds of solution, putting respectively in same and contain on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is an adhesive, is developing solvent with 2: 1 cyclohexane extraction-acetone, launches, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color, put again 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.
8. the quality determining method of the oral liquid of pharmaceutical composition as claimed in claim 7 is characterized in that this method also comprises following assay:
According to high performance liquid chromatography, 33: 67 acetonitrile: water is mobile phase; The detection wavelength is 270nm; Number of theoretical plate calculates by the icariin peak should be not less than 2000; It is an amount of that the preparation of reference substance solution, precision take by weighing the icariin reference substance, adds the solution that 45% ethanol is made every 1ml icariin 25ug, promptly; Preparation 25ml is measured in the preparation of need testing solution, precision, puts in the 100ml measuring bottle, adds 45% ethanol dilution to scale, shakes up, and filters, and gets subsequent filtrate, promptly; Accurate respectively reference substance solution and need testing solution and each 10ul of need testing solution of drawing injects chromatograph of liquid, measures, and the every 1ml of preparation contains Herba Epimedii in icariin, must not be less than 0.05mg.
9. as claim 1,2, the application of 3 or 4 described pharmaceutical compositions in the handicapped medicine of preparation therapeutic.
10. application as claimed in claim 9, it is characterized in that the therapeutic dysfunction is meant improves the erection degree.
11. application as claimed in claim 9 is characterized in that the therapeutic dysfunction is meant the increase ejaculate volume.
12. application as claimed in claim 9 is characterized in that the therapeutic dysfunction is meant the prolongation erection time.
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| CN101439116B (en) * | 2007-11-23 | 2011-05-04 | 河北以岭医药研究院有限公司 | Use of Chinese medicinal composition in preparing medicament for treating diabetes mellitus induced erectile dysfunction |
| CN108872426A (en) * | 2018-06-27 | 2018-11-23 | 上海应用技术大学 | The content assaying method of icariin in a kind of health preserving wine |
| CN109142563B (en) * | 2018-07-25 | 2021-03-02 | 山西广誉远国药有限公司 | Method for constructing tortoise age collection UPLC fingerprint and application thereof |
| CN110187046B (en) * | 2019-06-12 | 2021-08-17 | 贵州联盛药业有限公司 | Thin-layer identification and determination method for barbary wolfberry fruit, naringin and icariin in Shengjing tablets |
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| CN1298718A (en) * | 2000-08-18 | 2001-06-13 | 焦更海 | Chinese medicine for treating man's sexual disfunction and its preparing process |
| CN1313111A (en) * | 2000-03-15 | 2001-09-19 | 蒲荣 | Health-care medical wine for invigorating function of kidney and strengthening bone |
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| CN1313111A (en) * | 2000-03-15 | 2001-09-19 | 蒲荣 | Health-care medical wine for invigorating function of kidney and strengthening bone |
| CN1298718A (en) * | 2000-08-18 | 2001-06-13 | 焦更海 | Chinese medicine for treating man's sexual disfunction and its preparing process |
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