CN103494925A - Compound cottonrose hibiscus effervescent vaginal dilation suppository as well as preparation method and detection method thereof - Google Patents
Compound cottonrose hibiscus effervescent vaginal dilation suppository as well as preparation method and detection method thereof Download PDFInfo
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Abstract
The invention relates to a compound cottonrose hibiscus effervescent vaginal dilation suppository as well as a preparation method and a detection method thereof. The dilation suppository comprises a Chinese medicine composition, citric acid, sodium bicarbonate, a matrix and a dilation carrier, wherein the Chinese medicine composition is prepared from six raw medicinal materials, such as radix sophorae flavescentis and cottonrose hibiscus leaves; dalbergia wood and dandelion are added in the Chinese medicine composition, so that the curative effect of the compound cottonrose hibiscus effervescent vaginal dilation suppository on the trichomonas vaginitis and the colpitis mycotica can be improved; the polyethylene dodecyl stearate has the capability of improving the absorption of the Chinese medicine composition; a capsule shell is wrapped on the outer layer of the compound cottonrose hibiscus effervescent vaginal dilation suppository, so that the stability and the flexibility of the dilation suppository can be improved and the irritation of the dilation suppository can be reduced; in addition, the compound cottonrose hibiscus effervescent vaginal dilation suppository adopts six unique technologies and has the beneficial effects of preventing outflow of medicine liquor and preventing secondary infection, and is high in stability, durable in curative effect and the like.
Description
Technical field
The invention belongs to the vaginal suppository field, particularly a kind of compound recipe Hibisci Mutabilis effervescent vagina expansible plug and preparation method thereof and detection method.
Background technology
Compound recipe Hibisci Mutabilis type of effervescent suppository is prepared from by Radix Sophorae Flavescentis, Fructus Cnidii, Cortex Phellodendri, Folium Hibisci Mutabilis, Folium Artemisiae Argyi and Alumen and appropriate amount of auxiliary materials; Described compound recipe Hibisci Mutabilis type of effervescent suppository has heat clearing and damp drying, the effect of killing parasites for relieving itching, comprise infusorian property, colpitis mycotica for damp-heat type pudendal pruritus, cardinal symptom is the pudendum flushing, and swelling is very itched bitterly, profuse leukorrhea, yellow skin is as pus or be foam water from washing rice sample or the bean dregs sample, and its gas is stench, red tongue, yellow and greasy fur, soft and rapid pulse.
The curative effect of compound recipe Hibisci Mutabilis type of effervescent suppository has obtained clinical confirmation for many years, but itself still exists some technical problems, and for example traditional compound recipe Hibisci Mutabilis effervescent suppository bioavailability is low; Effervescent in type of effervescent suppository, used often vaginal mucosa produced to zest; Under hot and humid environment, described suppository is easily softening, affects the stability of suppository; And the cotton sliver in above-mentioned disclosed compound recipe Hibisci Mutabilis type of effervescent suppository is without expansion, or it is unordered to expand, and greatly reduces clinical application; The easy pollution clothes of suppository, not easy to clean; Method of quality control is unreliable, causes in actual production process, content, the stability between batch, melts and becomes the time limit and alter a great deal.
Summary of the invention
In order to solve the problems of the technologies described above, give full play to the curative effect of compound recipe Hibisci Mutabilis type of effervescent suppository, improve the stability of compound recipe Hibisci Mutabilis type of effervescent suppository, the invention provides a kind of compound recipe Hibisci Mutabilis effervescent vagina expansible plug and preparation method thereof; The science detection method that can control above-mentioned compound recipe Hibisci Mutabilis effervescent vagina expansible plug product quality further is provided.
The concrete technical scheme of the present invention is as follows:
The invention provides a kind of compound recipe Hibisci Mutabilis effervescent vagina expansible plug, described expansible plug comprises the Chinese medicine composition that weight portion is 6-35 part, the citric acid that weight portion is 10-30 part, the sodium bicarbonate that weight portion is 8-25 part, the expandable expansion carrier that the substrate that weight portion is 75-220 part and weight portion are 60-400 part, described Chinese medicine composition, citric acid and sodium bicarbonate and substrate formed pastille substrate are coated in the expansion carrier surface, the swell value of described expansion carrier after saturated water suction is greater than 1.1, described Chinese medicine composition mainly is prepared from through processing by the crude drug of following weight portion:
Radix Sophorae Flavescentis 25-100 Fructus Cnidii 25-100 Cortex Phellodendri 10-50
Folium Hibisci Mutabilis 15-75 Folium Artemisiae Argyi 10-50 Alumen 5-15
Described substrate comprises one or more in Acrawax, natural acid ester, lipoidis substrate, water-soluble base, glyceride, hydrogenated oil and fat or distillate oil;
Described Acrawax comprises one or more in mixed fatty glycerides, propylene glycol stearate, fixed oil, semi-synthetic fatty acid glyceride, semi-synthetic cocos nucifera oil ester, Witepsol, semi-synthetic Petiolus Trachycarpi grease or semi-synthetic Fructus Litseae ester;
Described natural acid ester comprises one or more in oleum sapii, Oleum Linderae, Fructus Foeniculi fat, Ke Kemu fat or cocoa butter;
Described lipoidis substrate comprises lanoline or lanonol;
Described water-soluble base comprises one or more in PEG400, polyethylene glycol 1500, Macrogol 4000, polyethylene glycol 6000, glycerin gelatine, polysorbate60, polysorbate65, polyoxyethylene condensation substance Idropostal, polyoxyethylene monostearate or poloxamer;
Described hydrogenated oil and fat comprises one or more in hydrogenated vegetable oil, hydrogenated groundnut, castor oil hydrogenated or cotmar;
Described glyceride comprises Adeps Solidus, Massa Estarinum A, Massa Estarinum AS, Massa Estarinum B, Massa Estarinum C, Massa Estarinum D, Massa Estarinum E, Massa Estarinum I, Massa Estarinum T, Massa Mf13, Suppository Base W, Suppository Base AB, Suppository Base A, Suppository Base B, Suppository Base BC, Suppository Base BD, Suppository Base BBC, Suppository Base E, Suppository Base BCF, Suppository Base C, Suppository Base D, Suppository Base299, Wecobee W, Wecobee K, Wecobee S, Wecobee M, Wecobee ES, Massuppol, Massuppol15, Suppocire OSI, Suppocire OSIx Suppocire A, Suppocire B, Suppocire C, Suppocire D, Suppocire DM, Suppocire H, Suppocire L, Tegester Triglyceride Bases-9, Tegester Triglyceride Bases-MA, one or more in Tegester Triglyceride Bases-57,
Described distillate oil comprises one or more in fractional distillation Petiolus Trachycarpi oil, fractionated coconut oil or fractional distillation Oleum Ricini.
The substrate of English name of the present invention include in " industrial pharmacy theory and practice " book (J.L. card Buddhist nun is uncommon for L. La Heman, H.A. profit Berman. industrial pharmacy theory and practice, Chemical Industry Press, second edition: 215-217).
The present invention has adopted original creation " intravaginal sticking type medicine-feeding technology ", and this technology by adding the expansion carrier to realize in suppository.Ordinary suppository is due to the relation of gravity, no matter user is standing, under sitting posture or the formula position of lying, always have vagina can not or the less medicated layer that touches, after described expansion carrier expands, medicated layer can be 360 ° and contact with vaginal walls, fully administration, 6 times of administration enlarged areas, medicine directly attaches to lesions position, makes the position that originally can't contact medicine also can obtain effectively attaching treatment; And due to the buffer action that stype plays in the middle of vagina, make no longer to contact with each other between wound surface, thereby avoid superinfection, it is shown effect no longer repeatedly.In addition, " anti-side leakage key " design concept has been applied in the introducing of expansion carrier, because the expansion of expansion carrier tail end (non-medicated layer) can be close to vaginal wall, and then prevent the outflow of medicine and substrate, reduce the pollution of medicated clothing and keep the valid density of medicine.And, by " inner core coefficient of expansion control technology ", the swell value of carrier after saturated water suction that can make to expand is greater than 1.1.
Further, the mixture that described substrate is Acrawax and distillate oil, the ratio of weight and number of described Acrawax and distillate oil is 9-15:1.
Compound recipe Hibisci Mutabilis type of effervescent suppository of the present invention can promote contacting of Chinese medicine composition and agents area, improves the curative effect of expansible plug.
Further, prepare Lignum Dalbergiae Odoriferae that the raw materials used medicine of described Chinese medicine composition also comprises that weight portion is 25-100 part and the Herba Taraxaci of 10-50 part.
The present invention is by the further screening to the Chinese medicine crude drug, discovery adds a certain proportion of Lignum Dalbergiae Odoriferae and Herba Taraxaci in the Chinese medicine composition of described compound recipe Hibisci Mutabilis effervescent vagina expansible plug, can significantly improve the curative effect of compound recipe Hibisci Mutabilis effervescent vagina expansible plug to trichomonal vaginitis and colpitis mycotica.
Preferably, described Acrawax is the semi-synthetic cocos nucifera oil ester that weight portion is 100 parts, described distillate oil is the fractional distillation Oleum Ricini that weight portion is 8 parts, the weight portion of described Chinese medicine composition is 15 parts, the weight portion of described citric acid is 15 parts, the weight portion of described sodium bicarbonate is 12 parts, and the weight portion of described expansion carrier is 200 parts, and the parts by weight that prepare the raw materials used medicine of described Chinese medicine composition are:
Radix Sophorae Flavescentis 60 Fructus Cnidii 50 Cortex Phellodendris 20
Folium Hibisci Mutabilis 30 Folium Artemisiae Argyi 20 Alumens 10.
Further preferably, the pastille substrate of compound recipe Hibisci Mutabilis effervescent vagina expansible plug of the present invention also comprises stearic acid polyethylene ten diester that weight portion is 2-5.5 part.Described stearic acid polyethylene ten diester can promote the absorption of Chinese medicine composition, improve the bioavailability of compound recipe Hibisci Mutabilis effervescent vagina expansible plug.
Further preferred, the skin parcel capsule shells of compound recipe Hibisci Mutabilis effervescent vagina expansible plug of the present invention, described capsule shells comprises the capsule material that weight portion is 5-15 part, the ethyl oleate of 2-6 part and the water of 5-15 part, the mixture that described capsule material is trehalose and sodium carboxymethyl cellulose, the ratio of weight and number of described trehalose and sodium carboxymethyl cellulose is 1:10-15.After compound recipe Hibisci Mutabilis effervescent vagina expansible plug parcel capsule shells of the present invention, can improve the stability of expansible plug under hot and humid environment; The capsule shells softness of being made by trehalose and sodium carboxymethyl cellulose, and can avoid the zest of the acid-base pair vagina in type of effervescent suppository, improve patient's compliance.
The swell value of expansion carrier of the present invention after saturated water suction is greater than 1.5, and described swell value is swell value radially; Described expansion carrier includes but not limited to cotton sliver, also can comprise the sterilizable material that other can expand, as non-woven fabrics, elastic fiber etc.
Pastille substrate of the present invention is the front end 1/5-4/5 place that Semi surrounding type is coated in described expansion carrier, according to " human engineering suppository " shape, be designed to the shapes such as duckbill, Herba sagittariae pygmaeae shape, spherical, avette, bullet shaped, torpedo, oblateness, cylindrical, taper shape or clavate.
The rear end of the expansion carrier of compound recipe Hibisci Mutabilis effervescent vagina expansible plug of the present invention is connected with bracing wire, stype after expansion, by the rear end bracing wire of tractive expansion carrier, the dead bark that be adsorbed on the virus be killed on the expansion carrier, toxin, comes off is also pulled out external in the lump, change dressings at every turn and just equal to do once thoroughly clean to vagina, fundamentally prevention of inflammation recurs again, and this expansible plug belongs to " integrated dosage form is cleaned in treatment ".
Meet in order to reach compound recipe Hibisci Mutabilis effervescent vagina expansible plug of the present invention the effect that water can expand rapidly, after described expansion carrier water suction, the maximum water absorption of every is not less than 1.5 milliliters; Suitable water absorption, can guarantee suitable swell value, and too low or too high water absorption all can cause bad impact; When water absorption is too low, can not guarantee that compound recipe Hibisci Mutabilis effervescent vagina expansible plug of the present invention meets the characteristics that water expand and make to expand insufficient; When water absorption is too high, the expansion carrier is understood too much absorption ingredient and is limited its diffusion; Therefore, water absorption is too low or too high, is not the desired expansion carrier of the present invention.
The present invention provides the preparation method of compound recipe Hibisci Mutabilis effervescent vagina expansible plug on the other hand, and described method comprises the steps:
1) preparation of pastille substrate:
A. substrate is placed in to the water-bath heating and melting, makes fused mass;
B. the preparation of Chinese medicine composition:
I. take Radix Sophorae Flavescentis, Cortex Phellodendri and the Folium Artemisiae Argyi of recipe quantity, pulverize, decoct with water three times, water consumption is Radix Sophorae Flavescentis, Cortex Phellodendri and Folium Artemisiae Argyi gross weight 10 times for the first time, decoct 3 hours, the second water consumption is Radix Sophorae Flavescentis, Cortex Phellodendri and Folium Artemisiae Argyi gross weight 5 times, decocts 2 hours, water consumption is Radix Sophorae Flavescentis, Cortex Phellodendri and Folium Artemisiae Argyi gross weight 3 times for the third time, decoct 1 hour, collecting decoction, filter, filtrate is concentrated into thick paste, is spray dried to fine powder;
II. take Fructus Cnidii and the Folium Hibisci Mutabilis of recipe quantity, pulverize, add twice of 75% alcohol reflux, adding for the first time amount of alcohol is 10 times of amounts of Fructus Cnidii and Folium Hibisci Mutabilis gross weight, reflux 3 hours, adding for the second time amount of alcohol is 5 times of amounts of Fructus Cnidii and Folium Hibisci Mutabilis gross weight, refluxes 2 hours, adding for the third time amount of alcohol is 3 times of amounts of Fructus Cnidii and Folium Hibisci Mutabilis gross weight, reflux 1 hour, merging filtrate, filter, filtrate is concentrated into thick paste, is spray dried to fine powder;
III. take the Alumen of recipe quantity, grind to form fine powder;
IV. the fine powder mix homogeneously by step I, II and III makes Chinese medicine composition;
C. Chinese medicine composition is mixed homogeneously with citric acid, sodium bicarbonate and stearic acid polyethylene ten diester, make mixture;
D. under stirring, the mixture of step c is added in the fused mass of step a, mix homogeneously, make pastille substrate;
2) preparation of expansible plug: pastille substrate is poured in the bolt mould, inserted the expansion carrier, cooling and shaping, make expansible plug;
3) preparation of capsule shells: heat water to 75 ℃, under stirring, add ethyl oleate, continue to stir, add the capsule material, stir, vacuum outgas, standby;
4) by step 2) described expansible plug and the described capsule shells of step 3) mix, and adopts pressing, makes the expansible plug of outer parcel capsule shells.
Further, the preparation method of Chinese medicine composition of the present invention also comprises the step of Lignum Dalbergiae Odoriferae and Herba Taraxaci being made to fine powder, described step is as follows: the Lignum Dalbergiae Odoriferae and the Herba Taraxaci that take recipe quantity, pulverize, decoct with water three times, water consumption is Lignum Dalbergiae Odoriferae and Herba Taraxaci gross weight 12 times for the first time, decoct 4 hours, the second water consumption is Lignum Dalbergiae Odoriferae and Herba Taraxaci gross weight 8 times, decocts 2 hours, water consumption is Lignum Dalbergiae Odoriferae and Herba Taraxaci gross weight 5 times for the third time, decoct 1.5 hours, collecting decoction, filter, filtrate is concentrated into thick paste, is spray dried to fine powder.
The preparation method of compound recipe Hibisci Mutabilis effervescent vagina expansible plug of the present invention has adopted " the integrally formed technology of the disposable fill of stype ".
The present invention also provides the detection method of described compound recipe Hibisci Mutabilis effervescent vagina expansible plug on the other hand, and described detection method comprises swell value assay method, weight differential detection method, assay etc.
Wherein said swell value assay method comprises:
A. along radially the choosing a bit or some points of described compound recipe Hibisci Mutabilis effervescent vagina expansible plug end face, measure the initial length H of described expansion carrier;
B. after the saturated water suction of described compound recipe Hibisci Mutabilis effervescent vagina expansible plug, be determined at the rear length h of selected location place's expansion carrier expansion in a step;
While c. calculating described swell value, according to the I formula, calculate;
（I）
Wherein, p means that axial swell value, h mean to expand rear length, H means initial length;
Or described swell value assay method is as follows:
A. along described compound recipe Hibisci Mutabilis effervescent vagina expansible plug axially choose a place or some positions, measure the initial diameter R of described expansion carrier;
B. after the saturated water suction of described compound recipe Hibisci Mutabilis effervescent vagina expansible plug, be determined at the rear diameter r of selected location place's expansion carrier expansion in a step;
While c. calculating described swell value, press the II formula and calculate;
（II）
Wherein, P means that swell value, r radially mean to expand rear diameter, R means initial diameter;
Described weight differential assay method comprises:
A. get described compound recipe Hibisci Mutabilis effervescent vagina expansible plug, take weight M;
B. get the expansion carrier in the described compound recipe Hibisci Mutabilis effervescent vagina expansible plug that scrapes pastille substrate, drying, take weight m, according to the weight X of pastille substrate as described in calculating as the III formula:
X=M-m
（Ⅲ）。
Further, in the detection method of described compound recipe Hibisci Mutabilis effervescent vagina expansible plug, after being melted the detection of change time limit, then carry out following at least one detection method:
1) the swell value assay method is as follows:
A. first along radially the choosing a bit or some points of described compound recipe Hibisci Mutabilis effervescent vagina expansible plug end face, after measuring the initial length H of described expansion carrier, then the different angles of rolling measure several times, and Hi averages;
B., after described compound recipe Hibisci Mutabilis effervescent vagina expansible plug is melted the detection of change time limit, be determined at the rear length h of selected location place's expansion carrier expansion in a step; The different angles of rolling are again measured several times, ask the rear average length hi that expands;
While c. calculating described swell value, according to the I formula, calculate;
（I）
Wherein, pi means that axial swell value, hi mean to expand rear average length, Hi means average initial length;
Or described swell value assay method is as follows:
A. first an angle along described compound recipe Hibisci Mutabilis effervescent vagina expansible plug axially choose a place or some positions, after measuring the initial diameter R of described expansion carrier, then the different angles of rolling measure several times, Ri averages;
B., after described compound recipe Hibisci Mutabilis effervescent vagina expansible plug is melted the detection of change time limit, be determined at the rear diameter r of selected location place's expansion carrier expansion in a step; The different angles of rolling are again measured several times, ask the rear average diameter ri that expands;
While c. calculating described swell value, press the II formula and calculate;
（II）
Wherein, Pi means that swell value, ri radially mean to expand rear average diameter, Ri means average initial diameter.
The wherein said change time limit assay method (two appendix of existing Chinese Pharmacopoeia) that melts comprising: get 3 of described compound recipe Hibisci Mutabilis effervescent vagina expansible plugs, after room temperature is placed 1 hour, be placed on respectively on lower floor's plectane of 3 metal rack, in the sleeve pipe of packing into separately, and fixing with hook.Except as otherwise herein provided, said apparatus is dipped vertically into respectively in the container that fills 37.0 ± 0.5 ℃ of water that are no less than 4L, its upper end position should fill a rot at 90mm place, underwater in container, overturns this device every 10 minutes once in solution.Above numerical range should not be construed as limitation of the present invention, and the technical scheme in above-mentioned numerical range is not in protection scope of the present invention yet.
2) weight differential assay method:
A. get described compound recipe Hibisci Mutabilis effervescent vagina expansible plug, take weight M;
B. scrape pastille substrate, the expansion carrier is placed in to 20-90 ℃ of organic solvent, take out, in 50-150 ℃ of dry 1-10h, take weight m, according to the weight X of pastille substrate as described in calculating as the III formula
X=M-m（Ⅲ）
Wherein, described organic solvent is selected from one or more in ethanol, methanol or isopropyl alcohol.
Further, in the detection method of described compound recipe Hibisci Mutabilis effervescent vagina expansible plug, described expansion carrier is cotton sliver, and described detection method comprises following at least one detection method:
1) swell value assay method:
Get 3 of described compound recipe Hibisci Mutabilis effervescent vagina expansible plugs, with slide gauge, survey its afterbody cotton sliver diameter, roll approximately 90 ° and survey once again, survey twice for every, obtain 2 meansigma methods Ri of every mensuration; After above-mentioned 3 bolts are used for melting the mensuration end of change time limit, take out immediately the residue cotton sliver, treat disconnected of water, all gently be placed on glass plate, measure two ends and middle three positions of each cotton sliver with slide gauge, roll approximately after 90 ° and measure three positions again, each cotton sliver obtains six data altogether, obtains 6 meansigma methods r of mensuration
i, calculate the swell value P of every
i, the swell value of three bolts all should be greater than 1.5.
2) weight differential assay method:
Get 10 of described compound recipe Hibisci Mutabilis effervescent vagina expansible plugs, the accurately weighed weight of difference, gently scrape pastille substrate (must not lose cotton sliver), cotton sliver is placed in to the 200-400ml ethanol of 50-80 ℃, preferably, cotton sliver is placed in to the 300ml ethanol of 60-70 ℃, and 80khz frequency ultrasonic cleaning 5 minutes, the remaining stromatolysis in cotton sliver surface is removed, taking out cotton sliver firmly extracts, with filter paper, inhale 3 times again, in 105 ℃ of dryings 2 hours, take out, room temperature was placed after 1 hour, the accurately weighed cotton sliver weight of difference, obtain every pastille substrate weight and average pastille substrate weight, every pastille substrate weight and average pastille substrate weight ratio are, what exceed average pastille substrate weight ± 10% must not be more than 2, and 1 times of 1 overrun must not be arranged.
The assay method of the swell value of compound recipe Hibisci Mutabilis effervescent vagina expansible plug provided by the present invention adopts repeatedly measuring method of multi-angle, has improved the accuracy of measuring, and has increased the operability of measuring, and method is easier to judgement; When carrying out the standard detection compound recipe Hibisci Mutabilis of the present invention effervescent vagina expansible plug of state-promulgated pharmacopoeia appendix weight differential, substrate need be scraped off, scraping degree difference due to operator's grasp, cause every scraping degree difference larger, so the present invention adopts the substrate on dissolution with solvents expansible plug surface, through verification experimental verification, when adopting hot ethanol to clean the substrate on expansible plug surface, result is better, and repeatability is higher, and described weight differential assay method is more convenient stable.
Described content assaying method is according to Chinese Pharmacopoeia appendix VI D high effective liquid chromatography for measuring.
Compound recipe Hibisci Mutabilis effervescent vagina expansible plug provided by the present invention has the high beneficial effect that waits of bioavailability, and this compound recipe Hibisci Mutabilis effervescent vagina expansible plug has adopted six leading technologies of original creation, expansion carrier in described compound recipe Hibisci Mutabilis effervescent vagina expansible plug add " the disposable fill of stype is integrally formed " technology of having applied original creation, " control of the inner core coefficient of expansion " technology, " human engineering bolt type " technology, " treatment is clean integrated " dosage form, " administration of intravaginal sticking type " technology, " anti-side leakage key design " six technology, this expansion carrier can make the pastille substrate of compound recipe Hibisci Mutabilis effervescent vagina expansible plug fully contact with vaginal walls, and prevent the medicinal liquid outflow, also there is the effect that the cleaning vagina prevents superinfection, the Lignum Dalbergiae Odoriferae added in described Chinese medicine composition and Herba Taraxaci can improve the curative effect of compound recipe Hibisci Mutabilis effervescent vagina expansible plug to trichomonal vaginitis and colpitis mycotica, described stearic acid polyethylene ten diester have the effect that improves the Chinese medicine composition absorption, in the skin parcel capsule shells of compound recipe Hibisci Mutabilis effervescent vagina expansible plug, can improve stability, the flexibility of expansible plug, reduce zest, improve patient's compliance.
The accompanying drawing explanation
Fig. 1 and Fig. 2 swell value assay method schematic diagram.
The specific embodiment
Embodiment 1
Preparation method:
1) preparation of pastille substrate:
A. semi-synthetic cocos nucifera oil ester and fractional distillation Oleum Ricini are placed in to the water-bath heating and melting, make fused mass;
B. the preparation of Chinese medicine composition:
I. take Radix Sophorae Flavescentis, Cortex Phellodendri and the Folium Artemisiae Argyi of recipe quantity, pulverize, decoct with water three times, water consumption is Radix Sophorae Flavescentis, Cortex Phellodendri and Folium Artemisiae Argyi gross weight 10 times for the first time, decoct 3 hours, the second water consumption is Radix Sophorae Flavescentis, Cortex Phellodendri and Folium Artemisiae Argyi gross weight 5 times, decocts 2 hours, water consumption is Radix Sophorae Flavescentis, Cortex Phellodendri and Folium Artemisiae Argyi gross weight 3 times for the third time, decoct 1 hour, collecting decoction, filter, filtrate is concentrated into thick paste, is spray dried to fine powder;
II. take Fructus Cnidii and the Folium Hibisci Mutabilis of recipe quantity, pulverize, add twice of 75% alcohol reflux, adding for the first time amount of alcohol is 10 times of amounts of Fructus Cnidii and Folium Hibisci Mutabilis gross weight, reflux 3 hours, adding for the second time amount of alcohol is 5 times of amounts of Fructus Cnidii and Folium Hibisci Mutabilis gross weight, refluxes 2 hours, adding for the third time amount of alcohol is 3 times of amounts of Fructus Cnidii and Folium Hibisci Mutabilis gross weight, reflux 1 hour, merging filtrate, filter, filtrate is concentrated into thick paste, is spray dried to fine powder;
III. take the Alumen of recipe quantity, grind to form fine powder;
IV. the fine powder mix homogeneously by step I, II and III makes the Chinese medicine composition that weight is about 15g;
C. by Chinese medicine composition and citric acid and sodium bicarbonate mix homogeneously, make mixture;
D. under stirring, the mixture of step c is added in the fused mass of step a, mix homogeneously, make pastille substrate;
2) preparation of expansible plug: pastille substrate is poured in the bolt mould, inserted cotton sliver, cooling and shaping, make 100 pieces of duckbill suppositorys, every piece of heavily about 3.5g.
Embodiment 2
Preparation method:
1) preparation of pastille substrate:
A. semi-synthetic fatty acid glyceride and fractional distillation Petiolus Trachycarpi oil are placed in to the water-bath heating and melting, make fused mass;
B. the preparation of Chinese medicine composition:
I. take Radix Sophorae Flavescentis, Cortex Phellodendri and the Folium Artemisiae Argyi of recipe quantity, pulverize, decoct with water three times, water consumption is Radix Sophorae Flavescentis, Cortex Phellodendri and Folium Artemisiae Argyi gross weight 10 times for the first time, decoct 3 hours, the second water consumption is Radix Sophorae Flavescentis, Cortex Phellodendri and Folium Artemisiae Argyi gross weight 5 times, decocts 2 hours, water consumption is Radix Sophorae Flavescentis, Cortex Phellodendri and Folium Artemisiae Argyi gross weight 3 times for the third time, decoct 1 hour, collecting decoction, filter, filtrate is concentrated into thick paste, is spray dried to fine powder;
II. take Fructus Cnidii and the Folium Hibisci Mutabilis of recipe quantity, pulverize, add twice of 75% alcohol reflux, adding for the first time amount of alcohol is 10 times of amounts of Fructus Cnidii and Folium Hibisci Mutabilis gross weight, reflux 3 hours, adding for the second time amount of alcohol is 5 times of amounts of Fructus Cnidii and Folium Hibisci Mutabilis gross weight, refluxes 2 hours, adding for the third time amount of alcohol is 3 times of amounts of Fructus Cnidii and Folium Hibisci Mutabilis gross weight, reflux 1 hour, merging filtrate, filter, filtrate is concentrated into thick paste, is spray dried to fine powder;
III. take the Alumen of recipe quantity, grind to form fine powder;
IV. take Lignum Dalbergiae Odoriferae and the Herba Taraxaci of recipe quantity, pulverize, decoct with water three times, water consumption is Lignum Dalbergiae Odoriferae and Herba Taraxaci gross weight 12 times for the first time, decoct 4 hours, the second water consumption is Lignum Dalbergiae Odoriferae and Herba Taraxaci gross weight 8 times, decocts 2 hours, water consumption is Lignum Dalbergiae Odoriferae and Herba Taraxaci gross weight 5 times for the third time, decoct 1.5 hours, collecting decoction, filter, filtrate is concentrated into thick paste, is spray dried to fine powder;
V. the fine powder mix homogeneously by step I, II, III and IV makes the Chinese medicine composition that weight is about 6g;
C. by Chinese medicine composition and citric acid and sodium bicarbonate mix homogeneously, make mixture;
D. under stirring, the mixture of step c is added in the fused mass of step a, mix homogeneously, make pastille substrate;
2) preparation of expansible plug: pastille substrate is poured in the bolt mould, inserted cotton sliver, cooling and shaping, make 100 pieces of spherical suppositorys, every piece of heavily about 5.0g.
Embodiment 3
Preparation method: prepare 100 pieces of avette suppositorys by the described method of embodiment 2, every piece of heavily about 1.8g.
Embodiment 4
Preparation method:
1) preparation of pastille substrate:
A. mixed fatty glycerides and fractionated coconut oil are placed in to the water-bath heating and melting, mix homogeneously, make fused mass;
B. the preparation of Chinese medicine composition: the method by embodiment 1 described Chinese medicine composition makes the Chinese medicine composition that weight is about 25g;
C. Chinese medicine composition is mixed homogeneously with citric acid, sodium bicarbonate and stearic acid polyethylene ten diester, make mixture;
D. under stirring, the mixture of step c is added in the fused mass of step a, mix homogeneously, make pastille substrate;
2) preparation of expansible plug: pastille substrate is poured in the bolt mould, inserted cotton sliver, cooling and shaping, make 100 pieces of clavate suppositorys, every piece of heavily about 3.7g.
Embodiment 5
Preparation method:
1) preparation of pastille substrate:
A. fixed oil, propylene glycol stearate and fractional distillation Petiolus Trachycarpi oil are placed in to the water-bath heating and melting, mix homogeneously, make fused mass;
B. the preparation of Chinese medicine composition: the method by embodiment 2 described Chinese medicine compositions makes the Chinese medicine composition that weight is about 35g;
C. Chinese medicine composition is mixed homogeneously with citric acid, sodium bicarbonate and stearic acid polyethylene ten diester, make mixture;
D. under stirring, the mixture of step c is added in the fused mass of step a, mix homogeneously, make pastille substrate;
2) preparation of expansible plug: pastille substrate is poured in the bolt mould, inserted cotton sliver, cooling and shaping, make 100 pieces of torpedo suppositorys, every piece of heavily about 4.1g.
Embodiment 6
Preparation method: prepare 100 pieces of cylindrical suppositorys by the described method of embodiment 4, every piece of heavily about 2.5g.
Embodiment 7
Preparation method:
1) preparation of pastille substrate:
A. semi-synthetic cocos nucifera oil ester and fractional distillation Oleum Ricini are placed in to the water-bath heating and melting, mix homogeneously, make fused mass;
B. the preparation of Chinese medicine composition: the method by embodiment 1 described Chinese medicine composition makes the Chinese medicine composition that weight is about 15g;
C. Chinese medicine composition is mixed homogeneously with citric acid, sodium bicarbonate and stearic acid polyethylene ten diester, make mixture;
D. under stirring, the mixture of step c is added in the fused mass of step a, mix homogeneously, make pastille substrate;
2) preparation of expansible plug: pastille substrate is poured in the bolt mould, inserted cotton sliver, cooling and shaping, make 100 pieces of conical suppositorys, every piece of heavily about 3.5g;
3) preparation of capsule shells: heat water to 75 ℃, under stirring, add ethyl oleate, continue to stir, add trehalose and sodium carboxymethyl cellulose, stir, vacuum outgas, standby;
4) by step 2) described expansible plug and the described capsule shells of step 3) mix, and adopts pressing, makes the expansible plug of outer parcel capsule shells.
Embodiment 8
Preparation method:
1) preparation of pastille substrate:
A. semi-synthetic Fructus Litseae ester and fractional distillation Petiolus Trachycarpi oil are placed in to the water-bath heating and melting, mix homogeneously, make fused mass;
B. the preparation of Chinese medicine composition: the method by embodiment 2 described Chinese medicine compositions makes the Chinese medicine composition that weight is about 10g;
C. Chinese medicine composition is mixed homogeneously with citric acid, sodium bicarbonate and stearic acid polyethylene ten diester, make mixture;
D. under stirring, the mixture of step c is added in the fused mass of step a, mix homogeneously, make pastille substrate;
2) preparation of expansible plug: pastille substrate is poured in the bolt mould, inserted cotton sliver, cooling and shaping, make 100 pieces of bullet shaped suppositorys, every piece of heavily about 4.3g;
3) preparation of capsule shells: heat water to 75 ℃, under stirring, add ethyl oleate, continue to stir, add trehalose and sodium carboxymethyl cellulose, stir, vacuum outgas, standby;
4) by step 2) described expansible plug and the described capsule shells of step 3) mix, and adopts pressing, makes the expansible plug of outer parcel capsule shells.
Embodiment 9
Preparation method: make 100 pieces of conical suppositorys by the described method of embodiment 8, every piece of heavily about 4.6g.
Test example 1 stability test
1. accelerated test
Get the described compound recipe Hibisci Mutabilis of embodiment 7-9 effervescent vagina expansible plug and common compound recipe Hibisci Mutabilis type of effervescent suppository, all under 30 ℃ ± 2 ℃ of constant temperature, under the constant humidity condition that relative humidity is 65% ± 5%, place 6 months, at duration of test, sample respectively once 1 month, 2 months, 3 months, 6 the end of month, press the regulation in Chinese Pharmacopoeia, detect the shape of expansible plug, containing the labelled amount (%) of matrine, melt and become the time limit, the accelerated test of the described compound recipe Hibisci Mutabilis of embodiment 7-9 effervescent vagina expansible plug and common compound recipe Hibisci Mutabilis type of effervescent suppository the results are shown in Table 1.
The compound recipe Hibisci Mutabilis effervescent vagina expansible plug of table 1 embodiment 7-9 and the accelerated test result of compound recipe Hibisci Mutabilis effervescent suppository
The described compound recipe Hibisci Mutabilis of embodiment of the present invention 7-9 effervescent vagina expansible plug as can be seen from the table, under the environment of constant temperature high humidity, after placing 6 months, the color of described expansible plug, the labelled amount that contains matrine, melt and become the time limit and all occur significantly to change; And common compound recipe Hibisci Mutabilis effervescent suppository was placed after 6 months under high humidity, the suppository color changes, and speckle appears in the suppository surface, suppository generation fracture phenomena; And in described compound recipe Hibisci Mutabilis effervescent suppository, the content of matrine obviously descends, melt and become the time limit significant prolongation; Show that compound recipe Hibisci Mutabilis effervescent vagina expansible plug of the present invention compares stability with compound recipe Hibisci Mutabilis effervescent suppository and significantly improve.
2. long term test
Get the described compound recipe Hibisci Mutabilis of embodiment 7-9 effervescent vagina expansible plug and compound recipe Hibisci Mutabilis type of effervescent suppository, at 25 ℃ ± 2 ℃ of temperature, under the condition that relative humidity is 60% ± 10%, place 36 months, sampling in every 3 months once, respectively at 0 month, 3 months, 6 months, 9 months, sampling in 12 months, detect the shape of expansible plug, labelled amount (%) containing matrine, melt and become the time limit, after 12 months, still need to continue to investigate index of correlation, respectively at 18 months, 24 months, sampling in 36 months is detected, and testing result and comparison in 0 month, the long-term test results of the described compound recipe Hibisci Mutabilis of embodiment 7-9 effervescent vagina expansible plug and compound recipe Hibisci Mutabilis type of effervescent suppository is in Table 2.
The compound recipe Hibisci Mutabilis effervescent vagina expansible plug of table 2 embodiment 7-9 and the long-term test results of common compound recipe Hibisci Mutabilis effervescent suppository
The described compound recipe Hibisci Mutabilis of embodiment 7-9 effervescent vagina expansible plug as can be seen from the table, under the environment of constant temperature high humidity, after placing 36 months, the color of described expansible plug, the labelled amount that contains matrine, melt and become the time limit and all occur significantly to change; And common compound recipe Hibisci Mutabilis type of effervescent suppository was placed after 9 months, the suppository color changes, and after placing 18 months, speckle appears in the suppository surface, and part suppository breaks; And in compound recipe Hibisci Mutabilis effervescent suppository, the content of matrine significantly descends, melt and become the time limit significant prolongation; Show that compound recipe Hibisci Mutabilis effervescent vagina expansible plug of the present invention compares stability with compound recipe Hibisci Mutabilis effervescent suppository and significantly improve.
Test example 2 swell value determination tests
Method one
Get 3 of described compound recipe Hibisci Mutabilis effervescent vagina expansible plugs, with slide gauge, survey its afterbody cotton sliver diameter, roll approximately 90 ° and survey once again, survey twice for every, obtain 2 meansigma methods Ri of every mensuration; After above-mentioned 3 bolts are used for melting the mensuration end of change time limit, take out immediately the residue cotton sliver, treat disconnected of water, all gently be placed on glass plate, measure two ends and middle three positions of each cotton sliver with slide gauge, roll approximately after 90 ° and measure three positions again, each cotton sliver obtains six data altogether, obtains 6 meansigma methods r of mensuration
i, calculate the swell value P of every
i, the swell value of three bolts all is greater than 1.5.
The swell value of measuring the described compound recipe Hibisci Mutabilis of embodiment 1-9 effervescent vagina expansible plug according to above-mentioned swell value assay method is as shown in table 3;
The swell value of the described compound recipe Hibisci Mutabilis of table 3 embodiment 1-9 effervescent vagina expansible plug
| Embodiment | Average diameter (mm) before expanding | Average diameter (mm) after expanding | Swell value (doubly) | Result |
| Embodiment 1 | 12.02 | 21.36 | 1.78 | Qualified |
| Embodiment 2 | 11.98 | 20.85 | 1.74 | Qualified |
| Embodiment 3 | 12.11 | 22.03 | 1.82 | Qualified |
| Embodiment 4 | 12.09 | 21.74 | 1.80 | Qualified |
| Embodiment 5 | 11.87 | 20.65 | 1.74 | Qualified |
| Embodiment 6 | 12.17 | 22.34 | 1.84 | Qualified |
| Embodiment 7 | 12.22 | 22.71 | 1.86 | Qualified |
| Embodiment 8 | 12.26 | 21.93 | 1.79 | Qualified |
| Embodiment 9 | 11.92 | 20.88 | 1.75 | Qualified |
Method two
As depicted in figs. 1 and 2, the detection method of vagina expansible plug:
1) swell value assay method:
A. first along described vagina expansible plug end face, radially choose C1, C2, tri-points of C3, measure initial length H1, H2, the H3 of described expansion carrier with slide gauge after, the 90 ° of measurements of rolling again, after radially the choosing C1, C4, tri-points of C5 and measure initial length H4, H5, the H6 of described expansion carrier with slide gauge of described vagina expansible plug end face, ask the meansigma methods Hi of H1, H2, H3, H4, H5 and H6;
B., after described vagina expansible plug is melted the detection of change time limit, with slide gauge, be determined at selected C1, C2 in a step, C3 tri-expansions of position expansion carriers rear length h1, h2, h3; Roll again 90 °, with slide gauge, be determined at selected C1, C4 in a step, C5 tri-expansions of position expansion carriers rear length h4, h5, h6, ask the average length of h1, h2, h3, h4, h5 and h6, be the rear average length hi that expands;
While c. calculating described swell value, according to the I formula, calculate;
（I）
Wherein, pi means that axial swell value, hi mean to expand rear average length, Hi means average initial length;
Or, the swell value assay method:
D. first an angle, along described vagina expansible plug, axially choose A1, A2 and tri-points of A3, measure initial diameter R1, the R2 and R3 of described expansion carrier with slide gauge after, roll again 90 °, axially choose B1, B2 and tri-points of B3 along described vagina expansible plug, measure initial diameter R4, the R5 and R6 of described expansion carrier with slide gauge after, ask the meansigma methods Ri of R1, R2, R3, R4, R5 and six initial diameters of R6;
E. described vagina expansible plug is melted and is become after the time limit detects, and after being determined in the d step selected A1, A2 and A3 position expansion carrier and expanding, diameter is respectively r1, r2 and r3; Roll again 90 ° measure in d step selected B1, B2 and B3 position expansion carrier and expand after diameter be respectively r4, r5 and r6, ask the meansigma methods of r1, r2, r3, r4, r5 and r6, average diameter ri afterwards must expand;
While f. calculating described swell value, press the II formula and calculate;
（II）
Wherein, Pi means that swell value, ri radially mean to expand rear average diameter, Ri means average initial diameter.
Test example 3 weight differential determination tests
Get 10 of described compound recipe Hibisci Mutabilis effervescent vagina expansible plugs, the accurately weighed weight of difference, gently scrape pastille substrate (must not lose cotton sliver), cotton sliver is placed in to the 300ml ethanol of 60-70 ℃, and 80khz frequency ultrasonic cleaning 5 minutes, the remaining stromatolysis in cotton sliver surface is removed, taking out cotton sliver firmly extracts, with filter paper, inhale 3 times again, in 105 ℃ of dryings 2 hours, take out, room temperature was placed after 1 hour, the accurately weighed cotton sliver weight of difference, obtain every pastille substrate weight and average pastille substrate weight, every pastille substrate weight and average pastille substrate weight ratio are, what exceed average pastille substrate weight ± 10% must not be more than 2, and 1 times of 1 overrun must not be arranged.
Repeat aforesaid operations, detect the described compound recipe Hibisci Mutabilis of embodiment 1-9 effervescent vagina expansible plug, the equal conformance with standard of its weight differential.
Test example 4 clinical trials
1. test case: accept patient's totally 92 examples for medical treatment, all through gynecologial examination, make a definite diagnosis trichomonal vaginitis patient 45 examples, colpitis mycotica patient's 47 examples, the age is all between 21-60 year, get rid of gestation and age of sucking the patient;
2. diagnostic criteria:
Symptom: pruritus vulvae, causalgia, or with frequent micturition, urgent micturition, dysurea;
Gynecologial examination: trichomonal vaginitis secretions is yellow cystose; Colpitis mycotica secretions is bean dregs sample or curdy, includes white plates;
Lab testing: visible infusorian under trichomonal vaginitis vaginal secretions microscope; The colpitis mycotica vaginal secretions is visible spore and pseudohypha under high power microscope;
3. grouping and administration: by 45 routine trichomonal vaginitis patients, be divided at random treatment group 28 example and matched group 17 examples; By 47 routine colpitis mycotica patients, be divided at random treatment group 32 example and matched group 15 examples; Above treatment group all gives the described compound recipe Hibisci Mutabilis of embodiment 8 effervescent vagina expansible plug, and matched group gives compound recipe Hibisci Mutabilis type of effervescent suppository, and two groups of administrations are once a day, within 7 days, are a course for the treatment of;
4. observation item
4.1 therapeutic is observed
(1) symptom;
(2) gynecologial examination: comprise pudendum, vagina, cervix uteri and vaginal secretions inspection;
(3) lab testing: to the vaginal secretions inspection, comprise under mirror, smear;
(4) antibacterial culturing;
4.2 safety is observed
(1) general health check-up project;
(2) blood, urine, just routine test;
(3) heart, liver, kidney function test;
4.3 untoward reaction is observed
Any abnormal symptom occurred during medication, sign, lab testing, all answer serious analysis, carefully differentiates;
5. efficacy assessment standard:
Recovery from illness: transference cure, gynecologial examination and lab testing are normal;
Produce effects: symptom obviously alleviates, and gynecologial examination and lab testing are clearly better;
Effectively: symptom alleviates to some extent, and gynecologial examination and lab testing take a turn for the better to some extent;
Invalid: after treatment, treatment is front unchanged;
6. therapeutic outcome: after the equal administration of patient 4 courses for the treatment of, therapeutic effect is in Table 4 and table 5;
Table 4 liang group compares the therapeutic effect of trichomonal vaginitis
Table 5 liang group compares the therapeutic effect of colpitis mycotica
7. conclusion
Compound recipe Hibisci Mutabilis effervescent vagina expansible plug is 96.4% to the effective percentage of trichomonal vaginitis, to the effective percentage of colpitis mycotica, is 96.9%, compares with matched group and significant difference is all arranged (P<0.01); In its curative effect process of checking, do not find any toxic and side effects, safe and reliable, evident in efficacy.
Test example 6 vaginal mucosa irritation tests
Get 10 of rabbit, be divided at random 2 groups, 5 every group, be divided into tested group and matched group; Described tested group gives the described compound recipe Hibisci Mutabilis of embodiment 7 effervescent vagina expansible plug, every day 1 time, and successive administration 7 days, matched group gives compound recipe compound recipe type of effervescent suppository, every day 1 time, successive administration 7 days; The general signs of administration every day fore-and-aft observing rabbit, comprise appetite, hair color, have or not abnormal secretion thing etc.; During administration, each group is showed no obvious abnormalities phenomenon; Last administration 24h takes out vagina tissue, for compound recipe Hibisci Mutabilis effervescent vagina expansible plug group, and the perusal smooth mucosal, without hyperemia, edema, hemorrhage, ulcer and the phenomenon such as rotten to the corn, pathological examination mucosa structural integrity, without ulcer, inflammation and rotten to the corn formation; For compound recipe Hibisci Mutabilis type of effervescent suppository group, the perusal mucosa is more coarse, and hyperemia, edema, phenomenon are arranged, pathological examination mucosa structural integrity, but ulcer and rotten to the corn formation are arranged; Show the sign not obviously impact of compound recipe Hibisci Mutabilis effervescent vagina expansible plug of the present invention on animal, to the mucosa nonirritant.
Claims (12)
1. a compound recipe Hibisci Mutabilis effervescent vagina expansible plug, it is characterized in that, described expansible plug comprises the Chinese medicine composition that weight portion is 6-35 part, the citric acid that weight portion is 10-30 part, the sodium bicarbonate that weight portion is 8-25 part, the expandable expansion carrier that the substrate that weight portion is 75-220 part and weight portion are 60-400 part, described Chinese medicine composition, citric acid and sodium bicarbonate and substrate formed pastille substrate are coated in the expansion carrier surface, the swell value of described expansion carrier after saturated water suction is greater than 1.1, described Chinese medicine composition mainly is prepared from through processing by the crude drug of following weight portion:
Radix Sophorae Flavescentis 25-100 Fructus Cnidii 25-100 Cortex Phellodendri 10-50
Folium Hibisci Mutabilis 15-75 Folium Artemisiae Argyi 10-50 Alumen 5-15
Described substrate comprises one or more in Acrawax, natural acid ester, lipoidis substrate, water-soluble base or distillate oil;
Described Acrawax comprises one or more in mixed fatty glycerides, propylene glycol stearate, fixed oil, semi-synthetic fatty acid glyceride, semi-synthetic cocos nucifera oil ester, semi-synthetic Petiolus Trachycarpi grease or semi-synthetic Fructus Litseae ester;
Described natural acid ester comprises one or more in oleum sapii, Oleum Linderae, Fructus Foeniculi fat, Ke Kemu fat or cocoa butter;
Described lipoidis substrate comprises lanoline or lanonol;
Described water-soluble base comprises one or more in polyethylene glycol 1500, Macrogol 4000, polyethylene glycol 6000, glycerin gelatine, polysorbate60, polysorbate65, polyoxyethylene monostearate or poloxamer;
Described distillate oil comprises one or more in fractional distillation Petiolus Trachycarpi oil, fractionated coconut oil or fractional distillation Oleum Ricini.
2. compound recipe Hibisci Mutabilis effervescent vagina expansible plug as claimed in claim 1, is characterized in that, the mixture that described substrate is Acrawax and distillate oil, and the ratio of weight and number of described Acrawax and distillate oil is 9-15:1.
3. compound recipe Hibisci Mutabilis effervescent vagina expansible plug as claimed in claim 1, is characterized in that, prepares Lignum Dalbergiae Odoriferae that the raw materials used medicine of described Chinese medicine composition also comprises that weight portion is 25-100 part and the Herba Taraxaci of 10-50 part.
4. compound recipe Hibisci Mutabilis effervescent vagina expansible plug as claimed in claim 2, it is characterized in that, described Acrawax is the semi-synthetic cocos nucifera oil ester that weight portion is 100 parts, described distillate oil is the fractional distillation Oleum Ricini that weight portion is 8 parts, the weight portion of described Chinese medicine composition is 15 parts, and the weight portion of described citric acid is 15 parts, and the weight portion of described sodium bicarbonate is 12 parts, the weight portion of described expansion carrier is 200 parts, and the parts by weight that prepare the raw materials used medicine of described Chinese medicine composition are:
Radix Sophorae Flavescentis 60 Fructus Cnidii 50 Cortex Phellodendris 20
Folium Hibisci Mutabilis 30 Folium Artemisiae Argyi 20 Alumens 10.
5. compound recipe Hibisci Mutabilis effervescent vagina expansible plug as claimed in claim 1, is characterized in that, described pastille substrate also comprises stearic acid polyethylene ten diester that weight portion is 2-5.5 part.
6. compound recipe Hibisci Mutabilis effervescent vagina expansible plug as claimed in claim 4, it is characterized in that, the skin parcel capsule shells of described expansible plug, described capsule shells comprises the capsule material that weight portion is 5-15 part, the ethyl oleate of 2-6 part and the water of 5-15 part, the mixture that described capsule material is trehalose and sodium carboxymethyl cellulose, the ratio of weight and number of described trehalose and sodium carboxymethyl cellulose is 1:10-15.
7. described compound recipe Hibisci Mutabilis effervescent vagina expansible plug as arbitrary as claim 1-6, is characterized in that, the swell value of described expansion carrier after saturated water suction is greater than 1.5, and described swell value is swell value radially; Described expansion carrier is cotton sliver; Described pastille substrate is the front end 1/5-4/5 place that Semi surrounding type is coated in described expansion carrier, and the rear end of described expansion carrier is connected with bracing wire; After described expansion carrier water suction, the maximum water absorption of every is not less than 1.5 milliliters.
8. the preparation method of compound recipe Hibisci Mutabilis effervescent vagina expansible plug as claimed in claim 6, is characterized in that, described method comprises the steps:
1) preparation of pastille substrate:
A. substrate is placed in to the water-bath heating and melting, makes fused mass;
B. the preparation of Chinese medicine composition:
I. take Radix Sophorae Flavescentis, Cortex Phellodendri and the Folium Artemisiae Argyi of recipe quantity, pulverize, decoct with water three times, water consumption is Radix Sophorae Flavescentis, Cortex Phellodendri and Folium Artemisiae Argyi gross weight 10 times for the first time, decoct 3 hours, the second water consumption is Radix Sophorae Flavescentis, Cortex Phellodendri and Folium Artemisiae Argyi gross weight 5 times, decocts 2 hours, water consumption is Radix Sophorae Flavescentis, Cortex Phellodendri and Folium Artemisiae Argyi gross weight 3 times for the third time, decoct 1 hour, collecting decoction, filter, filtrate is concentrated into thick paste, is spray dried to fine powder;
II. take Fructus Cnidii and the Folium Hibisci Mutabilis of recipe quantity, pulverize, add twice of 75% alcohol reflux, adding for the first time amount of alcohol is 10 times of amounts of Fructus Cnidii and Folium Hibisci Mutabilis gross weight, reflux 3 hours, adding for the second time amount of alcohol is 5 times of amounts of Fructus Cnidii and Folium Hibisci Mutabilis gross weight, refluxes 2 hours, adding for the third time amount of alcohol is 3 times of amounts of Fructus Cnidii and Folium Hibisci Mutabilis gross weight, reflux 1 hour, merging filtrate, filter, filtrate is concentrated into thick paste, is spray dried to fine powder;
III. take the Alumen of recipe quantity, grind to form fine powder;
IV. the fine powder mix homogeneously by step I, II and III makes Chinese medicine composition;
C. Chinese medicine composition is mixed homogeneously with citric acid, sodium bicarbonate and stearic acid polyethylene ten diester, make mixture;
D. under stirring, the mixture of step c is added in the fused mass of step a, mix homogeneously, make pastille substrate;
2) preparation of expansible plug: pastille substrate is poured in the bolt mould, inserted the expansion carrier, cooling and shaping, make expansible plug;
3) preparation of capsule shells: heat water to 75 ℃, under stirring, add ethyl oleate, continue to stir, add the capsule material, stir, vacuum outgas, standby;
4) by step 2) described expansible plug and the described capsule shells of step 3) mix, and adopts pressing, makes the expansible plug of outer parcel capsule shells.
9. the preparation method of compound recipe Hibisci Mutabilis effervescent vagina expansible plug as claimed in claim 8, it is characterized in that, the preparation method of described Chinese medicine composition also comprises the step of Lignum Dalbergiae Odoriferae and Herba Taraxaci being made to fine powder, described step is as follows: the Lignum Dalbergiae Odoriferae and the Herba Taraxaci that take recipe quantity, pulverize, decoct with water three times, water consumption is Lignum Dalbergiae Odoriferae and Herba Taraxaci gross weight 12 times for the first time, decoct 4 hours, the second water consumption is Lignum Dalbergiae Odoriferae and Herba Taraxaci gross weight 8 times, decoct 2 hours, water consumption is Lignum Dalbergiae Odoriferae and Herba Taraxaci gross weight 5 times for the third time, decoct 1.5 hours, collecting decoction, filter, filtrate is concentrated into thick paste, be spray dried to fine powder.
10. as the detection method of claim 1-6 or the arbitrary described compound recipe Hibisci Mutabilis effervescent vagina expansible plug of 8-9, it is characterized in that, described detection method comprises following at least one method:
1) the swell value assay method is as follows:
A. along radially the choosing a bit or some points of described compound recipe Hibisci Mutabilis effervescent vagina expansible plug end face, measure the initial length H of described expansion carrier;
B. after the saturated water suction of described compound recipe Hibisci Mutabilis effervescent vagina expansible plug, be determined at the rear length h of selected location place's expansion carrier expansion in a step;
While c. calculating described swell value, according to the I formula, calculate;
（I）
Wherein, p means that axial swell value, h mean to expand rear length, H means initial length;
Or the swell value assay method is as follows:
A. along described compound recipe Hibisci Mutabilis effervescent vagina expansible plug axially choose a place or some positions, measure the initial diameter R of described expansion carrier;
B. after the saturated water suction of described compound recipe Hibisci Mutabilis effervescent vagina expansible plug, be determined at the rear diameter r of selected location place's expansion carrier expansion in a step;
While c. calculating described swell value, press the II formula and calculate;
（II）
Wherein, P means that swell value, r radially mean to expand rear diameter, R means initial diameter;
2) weight differential assay method:
A. get described compound recipe Hibisci Mutabilis effervescent vagina expansible plug, take weight M;
B. get the expansion carrier in the described compound recipe Hibisci Mutabilis effervescent vagina expansible plug that scrapes pastille substrate, drying, take weight m, according to the weight X of pastille substrate as described in calculating as the III formula:
X=M-m
（Ⅲ）。
11. the detection method of compound recipe Hibisci Mutabilis effervescent vagina expansible plug as claimed in claim 10, is characterized in that, after being melted the detection of change time limit, then carries out following at least one detection method:
1) the swell value assay method is as follows:
A. first along radially the choosing a bit or some points of described compound recipe Hibisci Mutabilis effervescent vagina expansible plug end face, after measuring the initial length H of described expansion carrier, then the different angles of rolling measure several times, and Hi averages;
B., after described compound recipe Hibisci Mutabilis effervescent vagina expansible plug is melted the detection of change time limit, be determined at the rear length h of selected location place's expansion carrier expansion in a step; The different angles of rolling are again measured several times, ask the rear average length hi that expands;
While c. calculating described swell value, according to the I formula, calculate;
（I）
Wherein, pi means that axial swell value, hi mean to expand rear average length, Hi means average initial length;
Or the swell value assay method is as follows:
A. first an angle along described compound recipe Hibisci Mutabilis effervescent vagina expansible plug axially choose a place or some positions, after measuring the initial diameter R of described expansion carrier, then the different angles of rolling measure several times, Ri averages;
B., after described compound recipe Hibisci Mutabilis effervescent vagina expansible plug is melted the detection of change time limit, be determined at the rear diameter r of selected location place's expansion carrier expansion in a step; The different angles of rolling are again measured several times, ask the rear average diameter ri that expands;
While c. calculating described swell value, press the II formula and calculate;
（II）
Wherein, Pi means that swell value, ri radially mean to expand rear average diameter, Ri means average initial diameter;
2) weight differential assay method:
A. get described compound recipe Hibisci Mutabilis effervescent vagina expansible plug, take weight M;
B. scrape pastille substrate, the expansion carrier is placed in to 20-90 ℃ of organic solvent, take out, in 50-150 ℃ of dry 1-10h, take weight m, according to the weight X of pastille substrate as described in calculating as the III formula
X=M-m（Ⅲ）
Wherein, described organic solvent is selected from one or more in ethanol, methanol or isopropyl alcohol.
12. the detection method of compound recipe Hibisci Mutabilis effervescent vagina expansible plug as claimed in claim 11 is characterized in that described expansion carrier is cotton sliver, described detection comprises following at least one method:
1) swell value assay method:
Get 3 of described compound recipe Hibisci Mutabilis effervescent vagina expansible plugs, with slide gauge, survey its afterbody cotton sliver diameter, roll approximately 90 ° and survey once again, survey twice for every, obtain 2 meansigma methods Ri of every mensuration; After above-mentioned 3 bolts are used for melting the mensuration end of change time limit, take out immediately the residue cotton sliver, treat disconnected of water, all gently be placed on glass plate, measure two ends and middle three positions of each cotton sliver with slide gauge, roll approximately after 90 ° and measure three positions again, each cotton sliver obtains six data altogether, obtains 6 meansigma methods r of mensuration
i, calculate the swell value P of every
i, the swell value of three bolts all should be greater than 1.5;
2) weight differential assay method:
Get 10 of described compound recipe Hibisci Mutabilis effervescent vagina expansible plugs, the accurately weighed weight of difference, gently scrape pastille substrate (must not lose cotton sliver), cotton sliver is placed in to the 200-400ml ethanol of 50-80 ℃, preferably, cotton sliver is placed in to the 300ml ethanol of 60-70 ℃, and 80khz frequency ultrasonic cleaning 5 minutes, the remaining stromatolysis in cotton sliver surface is removed, taking out cotton sliver firmly extracts, with filter paper, inhale 3 times again, in 105 ℃ of dryings 2 hours, take out, room temperature was placed after 1 hour, the accurately weighed cotton sliver weight of difference, obtain every pastille substrate weight and average pastille substrate weight, every pastille substrate weight and average pastille substrate weight ratio are, what exceed average pastille substrate weight ± 10% must not be more than 2, and 1 times of 1 overrun must not be arranged.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310472861.5A CN103494925B (en) | 2013-10-11 | 2013-10-11 | Compound cottonrose hibiscus effervescent vaginal dilation suppository as well as preparation method and detection method thereof |
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|---|---|---|---|
| CN201310472861.5A CN103494925B (en) | 2013-10-11 | 2013-10-11 | Compound cottonrose hibiscus effervescent vaginal dilation suppository as well as preparation method and detection method thereof |
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| Publication Number | Publication Date |
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| CN103494925A true CN103494925A (en) | 2014-01-08 |
| CN103494925B CN103494925B (en) | 2015-04-08 |
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| CN201310472861.5A Active CN103494925B (en) | 2013-10-11 | 2013-10-11 | Compound cottonrose hibiscus effervescent vaginal dilation suppository as well as preparation method and detection method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110638744A (en) * | 2019-11-11 | 2020-01-03 | 哈尔滨欧替药业有限公司 | Vaginal effervescent suppository and preparation method and application thereof |
| CN114452315A (en) * | 2022-03-16 | 2022-05-10 | 郑州大学第一附属医院 | Vaginal effervescent suppository and preparation method thereof |
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| KR20010111964A (en) * | 2000-06-14 | 2001-12-20 | 김정웅 | Antibacterial composition of herb medicines, preparing method thereof and texture containing the same |
| CN102048876A (en) * | 2009-11-05 | 2011-05-11 | 天津开发区太人生物科技有限公司 | Bagged external washing ointment for assisting treatment of gynecologic inflammation and itchiness and preparation method thereof |
| TW201332586A (en) * | 2012-02-03 | 2013-08-16 | Qi-Xian Zheng | Female external use cleaning and health care ball |
| CN103285133A (en) * | 2013-06-21 | 2013-09-11 | 哈尔滨欧替药业有限公司 | Xiaomi vagina expansion suppository, preparation method and detection method thereof |
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| CN1131546A (en) * | 1995-03-21 | 1996-09-25 | 林秀明 | Vaginal antiphlogistic powder and its preparation method |
| KR20010111964A (en) * | 2000-06-14 | 2001-12-20 | 김정웅 | Antibacterial composition of herb medicines, preparing method thereof and texture containing the same |
| CN102048876A (en) * | 2009-11-05 | 2011-05-11 | 天津开发区太人生物科技有限公司 | Bagged external washing ointment for assisting treatment of gynecologic inflammation and itchiness and preparation method thereof |
| TW201332586A (en) * | 2012-02-03 | 2013-08-16 | Qi-Xian Zheng | Female external use cleaning and health care ball |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110638744A (en) * | 2019-11-11 | 2020-01-03 | 哈尔滨欧替药业有限公司 | Vaginal effervescent suppository and preparation method and application thereof |
| CN114452315A (en) * | 2022-03-16 | 2022-05-10 | 郑州大学第一附属医院 | Vaginal effervescent suppository and preparation method thereof |
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| CN103494925B (en) | 2015-04-08 |
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Effective date of registration: 20211126 Address after: 150040 office building 7, Bohai Third Road, haping road concentration area, Harbin Economic Development Zone, Harbin, Heilongjiang Province Patentee after: Harbin Tianmei Pharmaceutical Co.,Ltd. Address before: 150069, No. three, No. 7, Bohai, Harbin, Heilongjiang, China Patentee before: HARBIN OT PHARMACEUTICALS Co.,Ltd. Patentee before: Qiu Mingshi |
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Denomination of invention: Compound Furong Effervescent Vaginal Expansion Suppository and Its Preparation and Detection Method Effective date of registration: 20230908 Granted publication date: 20150408 Pledgee: China Merchants Bank Co.,Ltd. Harbin Branch Pledgor: Harbin Tianmei Pharmaceutical Co.,Ltd. Registration number: Y2023230000075 |