CN100391504C - A pharmaceutical composition for treating sexual dysfunction and its preparation method - Google Patents

Abstract

The invention discloses a pharmaceutical composition for treating sexual dysfunction. The composition is prepared from the following crude drugs: 10-30 parts by weight of Epimedium, 2-7 parts by weight of Ginseng, 5-20 parts by weight of velvet antler, 10-30 parts by weight of silkworm moth, 10-30 parts by weight of medlar, 5-20 parts by weight of fruit of dodder, 1-4 parts by weight of Fructus Cnidii, 8-20 parts by weight of Polygonatum, 10-30 parts by weight of Viola chinensis, 20 parts by weight of Fructus Plantaginis -80 parts by weight. Sexual dysfunction refers to improved penile erection. The composition is used for treating sexual dysfunction, and has the effects of increasing ejaculation volume, prolonging penile erection time and improving penile erection degree.

Description

A pharmaceutical composition for treating sexual dysfunction and its preparation method

field of invention

The invention relates to a pharmaceutical composition and a preparation method thereof, in particular to a pharmaceutical composition for treating sexual dysfunction and a preparation method thereof

Background technique

According to the statistics of the World Health Organization, there are 60 million to 80 million couples in the world who have fertility problems. In my country, one out of every 10 couples has problems such as infertility, infertility, impotence, spermatorrhea, premature ejaculation or frigidity, among which 5 -10% is related to kidney yang deficiency, which seriously affects people's health. Traditional Chinese medicine has an early understanding of impotence and other diseases caused by kidney yang deficiency, and the theoretical elaboration is profound. On the basis of this, we carefully formulated the prescription and verified repeatedly, and the invented composition has good effects of invigorating the kidney, replenishing qi and warming yang, and is used for treating sexual dysfunction.

Contents of the invention

The purpose of the present invention is to provide a pharmaceutical composition for treating sexual dysfunction; the purpose of the present invention is also to provide a preparation method of the pharmaceutical composition.

The object of the present invention is achieved through the following technical solutions.

The pharmaceutical composition crude drug of the present invention consists of:

Epimedium 10-30 parts by weight Ginseng 2-7 parts by weight velvet antler 5-20 parts by weight

10-30 parts by weight of male silkworm moth 10-30 parts by weight of medlar 5-20 parts by weight of dodder

1-4 parts by weight of Fructus Cnidii 8-20 parts by weight of Polygonatum 10-30 parts by weight of Viola

Semen psyllium 20-80 parts by weight

The preferred proportioning ratio of the pharmaceutical composition crude drug composition of the present invention is:

Epimedium 18 parts by weight Ginseng 5.5 parts by weight Deer antler 10 parts by weight

18 parts by weight of male silkworm moth 18 parts by weight of wolfberry fruit 11 parts by weight of dodder

2 parts by weight of Fructus Cnidii 14 parts by weight of Polygonatum 18 parts by weight of Viola

Semen psyllium 55 parts by weight;

Epimedium 15 parts by weight Ginseng 6 parts by weight Deer antler 7 parts by weight

27 parts by weight of male silkworm moth 13 parts by weight of wolfberry fruit 17 parts by weight of dodder

2 parts by weight of Fructus Cnidii 18 parts by weight of Polygonatum 14 parts by weight of Viola

30 parts by weight of psyllium;

Epimedium 25 parts by weight Ginseng 3 parts by weight Deer antler 17 parts by weight

15 parts by weight of male silkworm moth 25 parts by weight of wolfberry fruit 7 parts by weight of dodder

3 parts by weight of Fructus Cnidii 12 parts by weight of Polygonatum 25 parts by weight of Viola

Semen psyllium 60 parts by weight.

The above-mentioned pharmaceutical composition of the present invention can be made into any clinically acceptable dosage form, such as pills, powders, capsules, granules, dropping pills, oral liquid preparations, injections and the like.

The preparation method of pharmaceutical composition of the present invention is:

Except wolfberry, the rest of the nine flavors such as epimedium are crushed into the coarsest powder; soaked for 24-72 hours respectively; with 40-50% white wine as solvent, velvet antler is infiltrated separately, wolfberry and ginseng are infiltrated separately, and the rest Mix and infiltrate the seven flavors of male silkworm moth, collect the filtrates separately, and let them stand; filter and combine the three kinds of filtrates; add conventional excipients to make any clinically acceptable dosage form, such as pills, powders, capsules, granules, drops, etc. Pills, oral liquid preparations, etc.

The preferred method is:

Except medlar, the other nine flavors such as epimedium are crushed into the coarsest powder; soaked separately for 48 hours; use 45% white wine as solvent, velvet antler is infiltrated separately, medlar and ginseng are infiltrated separately, and the other seven flavors such as male silkworm moth are infiltrated. Mix and percolate, percolate at a rate of 1-3ml per minute, collect the filtrates separately, and let them stand; filter and combine the three kinds of filtrates; add conventional excipients to make any clinically acceptable dosage form, such as pills, powders, Capsules, granules, dripping pills, oral liquid preparations, etc.

The quality detection method of the oral liquid preparation of the pharmaceutical composition of the present invention includes one or more of the following identifications:

Identification: a. Take 50ml of the preparation, steam it on a water bath to about 10ml, add 20ml of water, transfer it to a separatory funnel, extract with 30ml of ether, and separate the water for later use; evaporate the ether solution to dryness, add 1ml of ethyl acetate to dissolve the residue, As the test solution. Take another 2 g of wolfberry reference medicinal material, add 50 ml of water, decoct for 20 minutes, filter, shake and extract the filtrate with 30 ml of ether, and prepare the reference medicinal material solution in the same way. According to the test of thin-layer chromatography (Chinese Pharmacopoeia 2000 edition one with VIB), draw 10 μl of each of the above two solutions and place them on the same silica gel G thin-layer plate containing sodium carboxymethylcellulose as a binder, and use benzene- Ethyl acetate-formic acid (8:5:0.4) was used as the developer, developed, taken out, dried in the air, and inspected under ultraviolet light (365nm). In the chromatogram of the test product, at the position corresponding to the chromatogram of the control medicinal material, there are fluorescent spots of the same color.

b. Take the water under the identification item a and extract it twice with ethyl acetate, 20ml each time, combine the ethyl acetate extract, evaporate to dryness, add 5ml of methanol to the residue to dissolve, add to the treated polyamide column (inner diameter 1cm, column height 10cm), elute with 40ml of ethyl acetate, collect the eluent, evaporate to dryness, add 1ml of ethyl acetate to the residue to dissolve, and use it as the test solution. Take another icariin reference substance, add methanol to make a solution containing 1mg per 1ml, as the reference substance solution. According to the test of thin-layer chromatography (Appendix VIB of the Chinese Pharmacopoeia in 2000), draw 10 μl of each of the above two solutions, and spot them on the same silica gel GF254 thin-layer plate containing carboxymethylcellulose sodium as the binder, and add ethyl acetate Ester-butanone-formic acid-water (10:1:1) was used as the developer, developed, taken out, dried in the air, and inspected under ultraviolet light (254nm). In the chromatogram of the test product, at the position corresponding to the chromatogram of the reference product, there are fluorescent spots of the same color.

c. Take 50ml of the preparation, put it on a water bath and steam it to about 10ml, add 30ml of water, mix well, take it twice with diethyl ether, 30ml each time, and separate the water for later use; combine the diethyl ether solution, wash it twice with 5% sodium carbonate solution, Take 30ml of diethyl ether, evaporate to dryness at low temperature, add 1ml of diethyl ether to dissolve the residue, and use it as the test solution. Take 0.2 g of Cnidium as a reference medicinal material, add 20 ml of ether, extract under reflux for 10 minutes, filter, and concentrate the filtrate to 1 ml as the reference medicinal material solution. Then take osthole reference substance, add ethanol to make a solution containing 0.5mg per 1ml, as the reference substance solution. According to thin-layer chromatography, (Chinese Pharmacopoeia 2000 Edition, Part One Supplement VIB) test, draw 10 μl of each of the above three solutions, and spot them on the same silica gel G thin-layer plate containing sodium carboxymethylcellulose as a binder, to Benzene-ethyl acetate (30:1) was used as the developer, developed, taken out, dried in the air, and inspected under ultraviolet light (365nm). In the chromatogram of the test product, fluorescent spots of the same color are displayed at the positions corresponding to the chromatograms of the reference medicinal material and the reference product.

d. Take the water liquid under identification c, extract it twice with n-butanol saturated with water, 30ml each time, combine the n-butanol extract, wash with ammonia test solution 3 times, 30ml each time; then use n-butanol saturated n-butanol Wash once with 30ml of water, separate the n-butanol solution, evaporate to dryness, add 10ml of 45% ethanol solution containing 7% sulfuric acid to the residue, heat and reflux for 1 hour, transfer to an evaporating dish, steam until there is no alcohol smell, add water to 10ml, Extract with diethyl ether twice, 10ml each time, combine the diethyl ether solution, evaporate to dryness, add 1ml diethyl ether to dissolve the residue, and use it as the test solution. Take Panaxadiol and Panaxatriol reference substances in addition, add ether to make a mixed solution containing 1mg in each 1ml, as the reference substance solution, test according to thin-layer chromatography (Appendix VlB of the Chinese Pharmacopoeia in 2000), absorb the above-mentioned 10 μl each of the two solutions was spotted on the same silica gel G thin-layer plate containing carboxymethylcellulose sodium as the adhesive, and cyclohexane-acetone (2:1) was used as the developer, developed, taken out, and dried in the air. Spray with 10% sulfuric acid ethanol solution, and heat at 105°C until the spots are clearly colored. In the chromatogram of the test product, at the position corresponding to the chromatogram of the reference product, spots of the same color are displayed, and then inspected under an ultraviolet lamp (365nm). In the chromatogram of the test product, at the position corresponding to the chromatogram of the reference product, there are fluorescent spots of the same color;

The quality detection method of the oral liquid preparation of the pharmaceutical composition of the present invention also includes the following content determination: according to the high performance liquid chromatography (the Chinese Pharmacopoeia 2000 edition an appendix VID determination).

Chromatographic conditions and system suitability test: use octadecylsilane bonded silica gel as filler; acetonitrile: water (33:67) as mobile phase; detection wavelength is 270nm; 2000.

Preparation of reference substance solution: Accurately weigh an appropriate amount of icariin reference substance, add 45% ethanol to make a solution of 25ug of icariin per 1ml, and obtain the solution.

Preparation of the test solution: precisely measure 25ml of the preparation, put it in a 100ml measuring bottle, add 45% ethanol to dilute to the mark, shake well, filter, and get the filtrate to get final product.

Determination method: Accurately draw 10ul each of the reference solution, the test solution and the test solution respectively, inject it into the liquid chromatograph, and determine that each 1ml of the preparation contains epimedium and icariin (C ₃₃ H ₄₀ O ₁₅ ) shall not be less than 0.05mg.

The medicine prepared from the composition of the invention has the functions of invigorating kidney, replenishing qi and strengthening yang. Among them, the wine preparation has been proved by the pharmacodynamics test of the Central Laboratory of Chengdu College of Traditional Chinese Medicine that the preparation has a very strong effect of tonifying the kidney and strengthening yang. Acute and chronic toxicity tests have proved that it is safe and non-toxic. On this basis, 60 cases of clinical observation have been carried out, and the curative effect is definite.

The following experimental examples and examples are used to illustrate but not limit the present invention.

clinical observational research trial

This experiment adopts random grouping, is divided into treatment group and control group, the ratio is 1:1.

30 cases in the treatment group were given oral liquor of the present invention, 50ml orally every day, once a day, and took five days, 250ml altogether. The patients in the treatment group must not use other medicines for treating impotence except oral liquor of the present invention.

The 30 cases in the control group were given Guilingjisa provided by Shanxi Traditional Chinese Medicine Factory orally, 50ml per day, once a day, for five days, a total of 250ml. In addition to taking Guilingjijiu orally, the patients in the control group were not allowed to use other drugs for treating impotence. Course of treatment: The course of treatment for both the treatment group and the control group was five days, and the curative effect was observed within one month after drug withdrawal.

The observations are as follows

1. the influence (as shown in table 1) of wine preparation of the present invention on clinical curative effect:

Table 1 wine preparation of the present invention is to the comparison of clinical curative effect influence

As can be seen from Table 1, after taking medicine, 9 cases of observation group are markedly effective (accounting for 30%), effective for 16 cases (accounting for 53.3%), invalid for 5 cases (accounting for 16.7%), total effective 25 cases, and the total effective rate is 83.3%; In the control group, 4 cases were markedly effective (accounting for 13.3%), 15 cases (50%) were effective, and 11 cases (accounting for 36.7%) were ineffective, and 19 cases were totally effective, and the total effective rate was 63.3%. It shows that the curative effect of the observation group is significantly better than that of the control group (P<0.05).

2, the influence (as shown in table 2) of wine preparation of the present invention on the patient's sexual desire of Mingmen fire failure

Table 2 Comparison of the influence of liquor of the present invention on the sexual desire of patients with Mingmen fire failure

It can be seen from Table 2 that there was no significant difference in sexual desire between the two groups before treatment (P>0.05). After treatment, the improvement of libido in the observation group was significantly better than that in the control group (P<0.05). As far as the observation group is concerned, the liquor of the present invention can significantly improve the libido of patients with Mingmen fire failure before and after treatment, and there is a significant difference between before and after treatment (P>0.05).

3, the influence (as shown in table 3) of wine preparation of the present invention on the patient's penile erection degree of Mingmen fire failure

Table 3 Effects on the degree of penile erection in patients with Mingmen Huoshui

It can be seen from Table 3 that there was no statistically significant difference in the degree of penile erection between the two groups of patients with Mingmen Huoshui before treatment (P>0.05). Significantly better than the control group (P<0.05). Compared before and after the treatment of the observation group, it can be seen that after taking the liquor of the present invention, the penile erection of patients with Mingmen fire failure has been significantly improved, and there is a very significant difference (P<0.01) compared before and after the treatment.

4, the influence (as shown in table 4) of wine preparation of the present invention on the patient's penile erection time of Mingmen fire failure.

Table 4 Effects on penile erection time of patients with Mingmen Huoshui

It can be seen from Table 4 that there was no significant difference in the penile erection time between the two groups of Mingmen Huoshui patients before and after treatment (P>0.05), but it can be seen from the comparison of the observation group before and after treatment that After oral administration, the liquor of the present invention can significantly prolong the erection time of the penis of patients with Qimen Huoshui, and there is a very significant difference (P<0.01) compared with before and after treatment.

5, the influence (as shown in table 5) of wine preparation of the present invention on the patient's ejaculation volume of Mingmen fire failure.

Table 5 Comparison of effects on ejaculate volume

As can be seen from Table 5, the amount of ejaculate significantly increased after taking the wine preparation of the present invention in the observation group of Mingmen fire failure patients compared with before treatment, and there was a significant difference before and after (P<0.05). There was no significant difference in the change of ejaculate volume before and after treatment between the observation group and the control group (P>0.05), and both had increased ejaculate volume.

6. The effect of Kunbukan Liquid on T and PRL in patients with Mingmen Huoshui (as shown in Table 6).

Table 6 Comparison of effects on T and PRL

Table 6 shows that the serum testosterone in the experimental group after treatment was significantly higher than that before treatment (P<0.05), and there was also a significant difference compared with the control group. The two groups of serum prolactin also showed different degrees of reduction, but there was no statistical difference in the results before and after treatment and between the two groups.

7, the influence (as shown in table 7) of wine preparation of the present invention on the main symptoms of patients with Mingmen fire failure.

Table 7 Impact on main TCM symptoms

It can be seen from Table 7 that there was no significant difference in the average score of TCM symptoms between the observation group and the control group before treatment (P>0.05); after treatment, the average score of TCM symptoms in the observation group was significantly different Compared with the control group, there was a significant difference between the two groups (P<0.05), and the TCM symptom scores of the patients in the observation group were significantly reduced after being treated with the liquor of the present invention, and there was a significant difference before and after the comparison (P<0.05). .

Conclusion: The total effective rate of the wine preparation of the present invention in treating impotence patients with Mingmen fire failure is 83.3%, which is significantly different from that of the control group (P<0.05). The liquor of the present invention can significantly improve the sexual desire of patients with Mingmen fire failure, and there is a significant difference (P<0.05) before and after treatment, and a significant difference (P<0.05) compared with the control group. The liquor of the present invention can significantly improve the degree of penile erection of patients with Mingmen fire failure, and there is a very significant difference (P<0.01) before and after treatment, and a significant difference (P<0.05) compared with the control group. The liquor of the present invention can significantly prolong the penile erection time of patients with Mingmen fire failure, and there is a very significant difference (P<0.01) before and after treatment, but no significant difference (P>0.05) compared with the control group. The wine preparation of the present invention can significantly increase the ejaculation volume of patients with vital energy failure, and there is a significant difference before and after treatment (P<0.05), but there is no significant difference compared with the control group (P>0.05). Liquor of the present invention can significantly increase the serum testosterone value (T) of the patient with the failure of vital energy, and there is a significant difference (P＜0.05) between the comparison before and after its treatment and the comparison with the contrast group (P＜0.05); There was no significant effect on the serum prolactin level (PRL) of patients with fire failure, and there was no significant difference before and after treatment and compared with the control group (P>0.05). The liquor of the present invention can significantly improve symptoms of traditional Chinese medicine such as coldness of the penis, soreness and coldness of the waist and knees, chills in the limbs, fatigue, clear and long urine, pale tongue, deep and slow pulse and other symptoms caused by the failure of Mingmen fire. There were significant differences before and after and compared with the control group (P<0.05).

Embodiment 1: capsule preparation

Epimedium 18g Ginseng 5.5g Deer antler 10g Male silkworm moth 18g

Lycium barbarum 18g Cuscuta 11g Cnidium 2g Polygonatum 14g

Viola 18g, psyllium 55g; add conventional auxiliary materials to make capsules.

Embodiment 2: drop pill preparation

Epimedium 15g Ginseng 6g velvet antler 7g Male silkworm moth 27g

Lycium barbarum 13g Cuscuta 17g Cnidium 2g Polygonatum 18g

Viola 14g, psyllium 30g; add auxiliary materials to make drop pills.

Example 3: Granule Preparation

Epimedium 25g Ginseng 3g velvet antler 17g Male silkworm moth 15g

Lycium barbarum 25g Cuscuta 7g Cnidium 3g Polygonatum 12g

Viola 25g, psyllium 60g; add auxiliary materials to make granules.

Embodiment 4: the preparation of liquor

Epimedium 18g Ginseng 5.5g Deer antler 10g Male silkworm moth 18g

Lycium barbarum 18g Cuscuta 11g Cnidium 2g Polygonatum 14g

Viola 18g Psyllium 55g

The above ten flavors, except medlar, other nine flavors such as epimedium are crushed into the coarsest powder. According to the percolation method (Appendix IO of Chinese Pharmacopoeia 2000 edition) under the liquid extract and extract item, use 45% white wine as a solvent, velvet antler is percolated separately, medlar and ginseng are percolated separately, and the remaining male silkworm moths, etc. Mix and percolate the seven flavors. After soaking for 48 hours, percolate at a rate of 1-3ml per minute, collect the filtrates in turn, 120ml, 188ml, 692ml, let stand, filter, combine the three kinds of filtrates, add 40g of sucrose , stir well, let it stand for one week, filter, add white wine (45v/v) to adjust to 1000ml, pack it separately, and get it.

Embodiment 5: Quality detection method

Prepare composition of the present invention and carry out quality detection as embodiment 4:

Identification: a. Take 50ml of the preparation, steam it on a water bath to about 10ml, add 20ml of water, transfer it to a separatory funnel, extract with 30ml of ether, and separate the water for later use; evaporate the ether solution to dryness, add 1ml of ethyl acetate to dissolve the residue, As the test solution. Take another 2 g of wolfberry reference medicinal material, add 50 ml of water, decoct for 20 minutes, filter, shake and extract the filtrate with 30 ml of ether, and prepare the reference medicinal material solution in the same way. According to the thin-layer chromatography (Chinese Pharmacopoeia 2000 edition one with VIB) test, draw 10 μl of each of the above two solutions. Spot on the same silica gel G thin-layer plate containing sodium carboxymethyl cellulose as the binder, develop with benzene-ethyl acetate-formic acid (8:5:0.4) as the developer, take it out, dry it in the air, and put it under ultraviolet light. View under light (365nm). In the chromatogram of the test product, at the position corresponding to the chromatogram of the control medicinal material, there are fluorescent spots of the same color.

b. Take the water under the identification item a and extract it twice with ethyl acetate, 20ml each time, combine the ethyl acetate extract, evaporate to dryness, add 5ml of methanol to the residue to dissolve, add to the treated polyamide column (inner diameter 1cm, column height 10cm), elute with 40ml of ethyl acetate, collect the eluent, evaporate to dryness, add 1ml of ethyl acetate to the residue to dissolve, and use it as the test solution. Take another icariin reference substance, add methanol to make a solution containing 1mg per 1ml, as the reference substance solution. According to the test of thin-layer chromatography (Appendix VIB of the Chinese Pharmacopoeia in 2000), draw 10 μl of each of the above two solutions, and spot them on the same silica gel GF254 thin-layer plate containing carboxymethylcellulose sodium as the binder, and add ethyl acetate Ester-butanone-formic acid-water (10:1:1) was used as the developer, developed, taken out, dried in the air, and inspected under ultraviolet light (254nm). In the chromatogram of the test product, at the position corresponding to the chromatogram of the reference product, there are fluorescent spots of the same color.

c. Take 50ml of the preparation, put it on a water bath and steam it to about 10ml, add 30ml of water, mix well, take it twice with diethyl ether, 30ml each time, and separate the water for later use; combine the diethyl ether solution, wash it twice with 5% sodium carbonate solution, Take 30ml of diethyl ether, evaporate to dryness at low temperature, add 1ml of diethyl ether to dissolve the residue, and use it as the test solution. Take 0.2 g of Cnidium as a reference medicinal material, add 20 ml of ether, extract under reflux for 10 minutes, filter, and concentrate the filtrate to 1 ml as the reference medicinal material solution. Then take osthole reference substance, add ethanol to make a solution containing 0.5mg per 1ml, as the reference substance solution. According to thin-layer chromatography, (Chinese Pharmacopoeia 2000 Edition, Part One Supplement VIB) test, draw 10 μl of each of the above three solutions, and spot them on the same silica gel G thin-layer plate containing sodium carboxymethylcellulose as a binder, to Benzene-ethyl acetate (30:1) was used as the developer, developed, taken out, dried in the air, and inspected under ultraviolet light (365nm). In the chromatogram of the test product, fluorescent spots of the same color are displayed at the positions corresponding to the chromatograms of the reference medicinal material and the reference product.

d. Take the water liquid under identification c, extract it twice with n-butanol saturated with water, 30ml each time, combine the n-butanol extract, wash with ammonia test solution 3 times, 30ml each time; then use n-butanol saturated n-butanol Wash once with 30ml of water, separate the n-butanol solution, evaporate to dryness, add 10ml of 45% ethanol solution containing 7% sulfuric acid to the residue, heat and reflux for 1 hour, transfer to an evaporating dish, steam until there is no alcohol smell, add water to 10ml, Extract with diethyl ether twice, 10ml each time, combine the diethyl ether solution, evaporate to dryness, add 1ml diethyl ether to dissolve the residue, and use it as the test solution. Take Panaxadiol and Panaxatriol reference substances in addition, add ether to make a mixed solution containing 1mg in each 1ml, as the reference substance solution, test according to thin-layer chromatography (Appendix VlB of the Chinese Pharmacopoeia in 2000), absorb the above-mentioned 10 μl each of the two solutions was spotted on the same silica gel G thin-layer plate containing carboxymethylcellulose sodium as the adhesive, and cyclohexane-acetone (2:1) was used as the developer, developed, taken out, and dried in the air. Spray with 10% sulfuric acid ethanol solution, and heat at 105°C until the spots are clearly colored. In the chromatogram of the test product, at the position corresponding to the chromatogram of the reference product, spots of the same color are displayed, and then inspected under an ultraviolet lamp (365nm). In the chromatogram of the test product, at the position corresponding to the chromatogram of the reference product, there are fluorescent spots of the same color;

Determination of content: according to high-performance liquid chromatography (Chinese Pharmacopoeia 2000 edition an appendix VID determination).

Chromatographic conditions and system suitability test: use octadecylsilane bonded silica gel as filler; acetonitrile: water (33:67) as mobile phase; detection wavelength is 270nm; 2000.

Preparation of reference substance solution: Accurately weigh an appropriate amount of icariin reference substance, add 45% ethanol to make a solution of 25ug of icariin per 1ml, and obtain the solution.

Preparation of the test solution: precisely measure 25ml of the preparation, put it in a 100ml measuring bottle, add 45% ethanol to dilute to the mark, shake well, filter, and get the filtrate to get final product.

Determination method: Accurately draw 10ul each of the reference solution, the test solution and the test solution respectively, inject it into the liquid chromatograph, and determine that each 1ml of the preparation contains Epimedium and Icariin (C ₃₃ H ₄₀ O ₁₅ ) shall not be less than 0.05mg.

Embodiment 6: Quality detection method

Prepare composition of the present invention and carry out quality detection as embodiment 4:

Identification: a. Take 50ml of the preparation, steam it on a water bath to about 10ml, add 20ml of water, transfer it to a separatory funnel, extract with 30ml of ether, and separate the water for later use; evaporate the ether to dryness, add 1ml of ethyl acetate to dissolve the residue, and use it as The test solution. Take another 2 g of wolfberry reference medicinal material, add 50 ml of water, decoct for 20 minutes, filter, shake and extract the filtrate with 30 ml of ether, and prepare the reference medicinal material solution in the same way. According to the test of thin-layer chromatography (Chinese Pharmacopoeia 2000 edition one with VIB), draw 10 μl of each of the above two solutions and place them on the same silica gel G thin-layer plate containing sodium carboxymethylcellulose as a binder, and use benzene- Ethyl acetate-formic acid (8:5:0.4) was used as the developer, developed, taken out, dried in the air, and inspected under ultraviolet light (365nm). In the chromatogram of the test product, at the position corresponding to the chromatogram of the control medicinal material, there are fluorescent spots of the same color.

b. Take the water under the identification item a and extract it twice with ethyl acetate, 20ml each time, combine the ethyl acetate extract, evaporate to dryness, add 5ml of methanol to the residue to dissolve, add to the treated polyamide column (inner diameter 1cm, column height 10cm), elute with 40ml of ethyl acetate, collect the eluent, evaporate to dryness, add 1ml of ethyl acetate to the residue to dissolve, and use it as the test solution. Take another icariin reference substance, add methanol to make a solution containing 1mg per 1ml, as the reference substance solution. According to the test of thin-layer chromatography (Appendix VIB of the Chinese Pharmacopoeia in 2000), draw 10 μl of each of the above two solutions, and spot them on the same silica gel GF254 thin-layer plate containing carboxymethylcellulose sodium as the binder, and add ethyl acetate Ester-butanone-formic acid-water (10:1:1) was used as the developer, developed, taken out, dried in the air, and inspected under ultraviolet light (254nm). In the chromatogram of the test product, at the position corresponding to the chromatogram of the reference product, there are fluorescent spots of the same color.

c. Take 50ml of the preparation, put it on a water bath and steam it to about 10ml, add 30ml of water, mix well, take it twice with diethyl ether, 30ml each time, and separate the water for later use; combine the diethyl ether solution, wash it twice with 5% sodium carbonate solution, Take 30ml of diethyl ether, evaporate to dryness at low temperature, add 1ml of diethyl ether to dissolve the residue, and use it as the test solution. Take 0.2 g of Cnidium as a reference medicinal material, add 20 ml of ether, extract under reflux for 10 minutes, filter, and concentrate the filtrate to 1 ml as the reference medicinal material solution. Then take osthole reference substance, add ethanol to make a solution containing 0.5mg per 1ml, as the reference substance solution. According to thin-layer chromatography, (Chinese Pharmacopoeia 2000 Edition, Part One Supplement VIB) test, draw 10 μl of each of the above three solutions, and spot them on the same silica gel G thin-layer plate containing sodium carboxymethylcellulose as a binder, to Benzene-ethyl acetate (30:1) was used as the developer, developed, taken out, dried in the air, and inspected under ultraviolet light (365nm). In the chromatogram of the test product, fluorescent spots of the same color are displayed at the positions corresponding to the chromatograms of the reference medicinal material and the reference product.

Determination of content: according to high-performance liquid chromatography (Chinese Pharmacopoeia 2000 edition an appendix VID determination).

Chromatographic conditions and system suitability test: use octadecylsilane bonded silica gel as filler; acetonitrile: water (33:67) as mobile phase; detection wavelength is 270nm; 2000.

Preparation of reference substance solution: Accurately weigh an appropriate amount of icariin reference substance, add 45% ethanol to make a solution of 25ug of icariin per 1ml, and obtain the solution.

Preparation of the test solution: precisely measure 25ml of the preparation, put it in a 100ml measuring bottle, add 45% ethanol to dilute to the mark, shake well, filter, and get the filtrate to get final product.

Determination method: Accurately draw 10ul each of the reference solution, the test solution and the test solution respectively, inject it into the liquid chromatograph, and determine that each 1ml of the preparation contains epimedium and icariin (C ₃₃ H ₄₀ O ₁₅ ) shall 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.