CN103520295B - Health woman spirit vaginal expansion plug and preparation method thereof and detection method - Google Patents
Health woman spirit vaginal expansion plug and preparation method thereof and detection method Download PDFInfo
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Abstract
The present invention relates to a kind of health woman spirit vaginal expansion plug and preparation method thereof and detection method, described expansible plug comprises Chinese medicine composition, substrate and expandable carrier, described Chinese medicine composition and substrate form pastille substrate and are coated in expandable carrier surface, and described Chinese medicine composition is prepared from primarily of Radix Et Rhizoma Rhei, catechu, Radix Arnebiae (Radix Lithospermi) and Borneolum Syntheticum processing; Rhizoma Cyperi and Ramulus Cinnamomi is also added in described Chinese medicine composition; Described pastille substrate also comprises maltose alcohol and Emulsifier LM-102, and it can improve the bioavailability of rehabilitation spirit vaginal expansion plug synergistically; Described acrylic resin and carrageenan improve the action time of expansible plug to vagina, extend curative effect; And described health woman spirit vaginal expansion plug have employed seven unique technology, and have and prevent medicinal liquid from outflowing, stability is high, and curative effect is lasting, prevents the beneficial effects such as superinfection.
Description
Technical field
The invention belongs to vaginal suppository field, particularly a kind of health woman spirit vaginal expansion plug and preparation method thereof and detection method.
Background technology
Health woman spirit bolt, is a kind of classical Chinese patent medicine, records in " the Sanitation Ministry medicine standard Traditional Chinese medicine historical preparation " the 8th, make 365 by Radix Et Rhizoma Rhei 246g, catechu 10g, Radix Arnebiae (Radix Lithospermi) 100g, Borneolum Syntheticum 7g and semi-synthetic fatty acid ester; Health woman spirit bolt, has effect that heat-clearing and toxic substances removing, removing dampness and killing parasites, convergence are antipruritic, clinically for the colpitis caused by the various cause of disease.
The curative effect of health woman spirit bolt obtains clinical confirmation for many years, but after making itself and semi-synthetic fatty acid ester make suppository containing Oleum sesami composition in traditional health woman spirit bolt, must preserve below 30 DEG C, and not easy-formation, thus transport, preserve inconvenience; And described health woman spirit bolt is short in the intravaginal holdup time, and mucosa-adherent is poor, and bioavailability is low, slow curative effect; In order to solve the problem that traditional health woman spirit bolt easily softens, CN101455729 has entered paraffin and Cera Flava two kinds of adjuvants in traditional health woman spirit bolt, although not easily soften after the suppository made, still there is the poor adhesion of mucosa, the technical problem that bioavailability is low; And the cotton sliver in above-mentioned disclosed health woman spirit bolt 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, batch between content, stability, melt become the time limit 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 health woman spirit bolt, improving the bioavailability of suppository, the invention provides a kind of health woman spirit vaginal expansion plug and preparation method thereof; The science detection method that can control above-mentioned health woman spirit vaginal expansion plug product quality is provided further.
The concrete technical scheme of the present invention is as follows:
The invention provides a kind of health woman spirit vaginal expansion plug, described expansible plug comprises the Chinese medicine composition that weight portion is 6-35 part, the expandable expandable carrier of weight portion to be the substrate of 70-220 part and weight portion be 60-400 part, described Chinese medicine composition and substrate formed pastille substrate are coated in expandable carrier surface, the swell value of described expandable carrier after saturated water suction is greater than 1.1, and described Chinese medicine composition is prepared from through processing primarily of the crude drug of following weight portion:
Radix Et Rhizoma Rhei 30-150 catechu 1-10 Radix Arnebiae (Radix Lithospermi) 15-100
Borneolum Syntheticum 0.5-4
Described substrate comprise in Acrawax, natural acid ester, lipoidis substrate, water-soluble base, gel-type vehicle, hydrogenated oil and fat, glyceride, distillate oil or colloidal compound one or more;
Described Acrawax comprise 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 one or more;
Described natural acid ester comprise in oleum sapii, Oleum Linderae, Fructus Foeniculi fat, Ke Kemu fat or cocoa butter one or more;
Described lipoidis substrate comprises lanoline or lanonol;
Described water-soluble base comprise in PEG400, polyethylene glycol 1500, Macrogol 4000, polyethylene glycol 6000, glycerin gelatine, polysorbate60, polysorbate65, polyethylene oxide condensate Idropostal, polyoxyethylene monostearate or poloxamer one or more;
Described gel-type vehicle comprise in sodium carboxymethyl cellulose, methylcellulose, hypromellose, chitosan, carbomer, alginic acid or sodium alginate one or more;
Described hydrogenated oil and fat comprise in hydrogenated vegetable oil, hydrogenated groundnut, castor oil hydrogenated or cotmar one or more;
Described glyceride comprises AdepsSolidus, MassaEstarinumA, MassaEstarinumAS, MassaEstarinumB, MassaEstarinumC, MassaEstarinumD, MassaEstarinumE, MassaEstarinumI, MassaEstarinumT, MassaMf13, SuppositoryBaseW, SuppositoryBaseAB, SuppositoryBaseA, SuppositoryBaseB, SuppositoryBaseBC, SuppositoryBaseBD, SuppositoryBaseBBC, SuppositoryBaseE, SuppositoryBaseBCF, SuppositoryBaseC, SuppositoryBaseD, SuppositoryBase299, WecobeeW, WecobeeK, WecobeeS, WecobeeM, WecobeeES, Massuppol, Massuppol15, SuppocireOSI, SuppocireOSIxSuppocireA, SuppocireB, SuppocireC, SuppocireD, SuppocireDM, SuppocireH, SuppocireL, TegesterTriglycerideBases-9, TegesterTriglycerideBases-MA, TegesterTriglycerideBases-57, tripalmitin, glycerol tristearate, one or more in glycerol three rosin ester or trilaurin,
Described distillate oil comprises fractionating palm oil or fractionated coconut oil;
Described colloidal compound comprise in arabic gum, gelatin or pectin one or more.
The substrate of English name of the present invention is included in " industrial pharmacy theory and practice " book (L. La Heman, H.A. profit Berman, J.L. card Buddhist nun is uncommon. industrial pharmacy theory and practice, Chemical Industry Press, the second edition: 215-217).
Present invention employs " the intravaginal sticking type medicine-feeding technology " of original creation, this technology by adding expandable carrier to realize in suppository.Ordinary suppository is due to the relation of gravity, no matter user is standing, under sitting posture or formula position of lying, always there is vagina or lessly can not to touch medicated layer, after described expandable carrier expands, medicated layer can contact with vaginal walls in 360 °, abundant administration, administration enlarged areas 6 times, medicine directly attaches to lesions position, makes the position that originally cannot contact medicine also effectively can be attached 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, thus avoid superinfection, make its no longer recurrent exerbation.In addition, the introducing of expandable carrier applies " lateral leakage protection key " design concept, because the expansion of expandable 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 expandable carrier after saturated water suction can be made to be greater than 1.1.
Further, substrate of the present invention is the mixture of natural acid ester and glyceride, and the ratio of weight and number of described natural acid ester and glyceride is 3-7:1.The mixed-matrix of natural acid ester of the present invention and glyceride overcomes the technical problem that traditional suppository easily softens; Improve the rate of release of Chinese medicine composition simultaneously, Chinese medicine composition is discharged fast.
In the technical scheme of further improvement, prepare the Ramulus Cinnamomi that the raw materials used medicine of described Chinese medicine composition also comprises Rhizoma Cyperi that parts by weight are 30-150 part and 15-100 part.
The present invention is by the further screening to Chinese medicine crude drug, find to add a certain proportion of Rhizoma Cyperi and Ramulus Cinnamomi in the Chinese medicine composition of described health woman spirit vaginal expansion plug, can significantly improve health woman spirit vaginal expansion plug to colpitic curative effect, described health woman spirit vaginal expansion plug also has good therapeutic effect to cervical erosion simultaneously.
Further, in health woman of the present invention spirit vaginal expansion plug, described natural acid ester to be weight portion the be Fructus Foeniculi fat of 75 parts, described glyceride to be weight portion the be tripalmitin of 15 parts; The weight portion of described Chinese medicine composition is 10 parts, and the weight portion of described expandable carrier is 200 parts, and the parts by weight preparing the raw materials used medicine of described Chinese medicine composition are:
Radix Et Rhizoma Rhei 67.4 catechu 2.74 Radix Arnebiae (Radix Lithospermi) 27.4
Borneolum Syntheticum 1.92.
Preferably, the pastille substrate of health woman spirit vaginal expansion plug of the present invention also comprises the maltose alcohol that weight portion is 3-7.5 part.Described maltose alcohol can increase the cohesion of substrate and Chinese medicine composition, is beneficial to the molding of suppository, makes it make not easily to soften in transport and use procedure, has good hardness; Described maltose alcohol can prevent the precipitation of Chinese medicine composition simultaneously, thus improves the stability of suppository.
Further preferably, pastille substrate of the present invention also comprises the Emulsifier LM-102 that weight portion is 0.7-2.3 part.Described Emulsifier LM-102 and maltose alcohol can promote the absorption of Chinese medicine composition synergistically, improve the bioavailability of health woman spirit vaginal expansion plug.
Further preferred, the pastille substrate of health woman spirit vaginal expansion plug of the present invention also comprises the carrageenan of acrylic resin that weight portion is 1-4 part and 0.5-2 part.Described acrylic resin and carrageenan can extend the action time of Chinese medicine composition to vagina, extend the curative effect of health woman spirit vaginal expansion plug, also can improve the adhesiveness of mucosa simultaneously, improve bioavailability.
The swell value of expandable carrier of the present invention after saturated water suction is greater than 1.5, and described swell value is radial swell value; Described expandable carrier includes but not limited to cotton sliver, also can comprise other sterilizable materials that can expand, as non-woven fabrics, elastic fiber etc.
Pastille substrate of the present invention is the 1/5-4/5 place, front end that Semi surrounding type is coated in described expandable carrier, according to " human engineering suppository " shape, be designed to the shape such as duckbill, Herba sagittariae pygmaeae shape, spherical, avette, bullet shaped, torpedo, oblateness, cylindrical, conical or clavate.
The rear end of the expandable carrier of health woman spirit vaginal expansion plug of the present invention is connected with bracing wire, stype after expansion, by the rear end bracing wire of tractive expandable carrier, be adsorbed on the virus be killed on expandable carrier, toxin, the dead bark that comes off also pull out external in the lump, change dressings at every turn and just equal to do to vagina once thoroughly to clean, fundamentally prevention of inflammation recurs again, and namely this expansible plug belongs to " the integrated dosage form for the treatment of cleaning ".
In order to reach health woman of the present invention spirit vaginal expansion plug meet water can the effect of undergoes rapid expansion, after described expandable carrier water suction, the maximum water absorption of every is not less than 1.5 milliliters; Suitable water absorption, can ensure the swell value be suitable for, too low or too high water absorption, all can cause bad impact; When water absorption is too low, can not ensure that health woman of the present invention spirit vaginal expansion plug is met feature that namely water expand and makes expansion insufficient; When water absorption is too high, the absorption ingredient that expandable carrier can be too much and limit its diffusion; Therefore, water absorption is too low or too high, is not the expandable carrier desired by the present invention.
The present invention provides the preparation method of health woman spirit vaginal expansion plug on the other hand, and described method comprises the steps:
1) preparation of pastille substrate:
A. substrate is placed in water-bath heating and melting, mix homogeneously, obtained fused mass;
B. the preparation of Chinese medicine composition:
I. take the Radix Et Rhizoma Rhei of recipe quantity, pulverize, add 75% alcohol reflux twice, first time adds 10 times that amount of alcohol is Radix Et Rhizoma Rhei weight, backflow 3h, second time adds 5 times that amount of alcohol is Radix Et Rhizoma Rhei weight, and backflow 1.5h, merges backflow, filter, filtrate is condensed into thick paste, and thick paste is spray dried to fine powder;
II. take the Radix Arnebiae (Radix Lithospermi) of recipe quantity, pulverize, decoct with water twice, amount of water is 10 times of Radix Arnebiae (Radix Lithospermi) weight for the first time, decocts 2h, and second time amount of water is 4 times of Radix Arnebiae (Radix Lithospermi) weight, decoct 1.5h, merge decoction liquor, filter, it be 60 DEG C of relative densities is the clear paste of 1.02 that filtrate is concentrated into temperature, add the ethanol of 80%, make alcohol content reach 70%, leave standstill, filter out precipitation, precipitation is spray dried to fine powder;
III. catechu is ground into fine powder;
IV. borneol and grinding is become fine powder;
V. by step I, II, the fine powder mix homogeneously of III and IV, obtained Chinese medicine composition;
C., under grinding, slowly Chinese medicine composition is mixed homogeneously with maltose alcohol, Emulsifier LM-102, continue to grind to form pastel;
D. carrageenan is placed in water-bath heating and melting, adds acrylic resin under stirring, mix homogeneously, continue to stir, add the pastel of step c, mix homogeneously, obtained mixture;
E. under stirring, the mixture of steps d is added in the fused mass of step a, mix homogeneously, obtained pastille substrate;
2) preparation of expansible plug: pastille substrate poured in bolt mould, insert expandable carrier, cooling and shaping, makes suppository.
Further, described in the preparation method of health woman spirit vaginal expansion plug of the present invention, the preparation method of Chinese medicine composition also comprises step Rhizoma Cyperi and Ramulus Cinnamomi being made fine powder, described step is as follows: the Rhizoma Cyperi and the Ramulus Cinnamomi that take recipe quantity, pulverize, add the alcohol reflux twice of 85%, first time adds 15 times that amount of alcohol is Rhizoma Cyperi and Ramulus Cinnamomi gross weight, backflow 1.5h, second time adds 10 times that amount of alcohol is Radix Et Rhizoma Rhei weight, backflow 1h, merges backflow, filters, filtrate is condensed into thick paste, and thick paste is spray dried to fine powder.
The preparation method of health woman spirit vaginal expansion plug of the present invention have employed " the integrally formed technology of the disposable fill of stype ".
The present invention additionally provides the detection method of described health woman spirit vaginal expansion 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. the radial direction along described health woman spirit vaginal expansion plug end face is chosen a bit or some points, measures the initial length H of described expandable carrier;
B., after the saturated water suction of described health woman spirit vaginal expansion plug, expandable carrier expansion rear length h in selected location place in a step is determined at;
When c. calculating described swell value, calculate according to I formula;
Wherein, p represent axial swell value, h represent expand after length, H represent initial length;
Or described swell value assay method is as follows:
A. the axis along described health woman spirit vaginal expansion plug chooses a place or some positions, measures the initial diameter R of described expandable carrier;
B., after the saturated water suction of described health woman spirit vaginal expansion plug, selected location place expandable carrier expanded diameter r in a step is determined at;
When c. calculating described swell value, calculate by II formula;
Wherein, P represents the swell value of radial direction, r represents expanded diameter, R represents initial diameter;
Described weight differential assay method comprises:
A. get described health woman spirit vaginal expansion plug, take weight M;
B. the expandable carrier scraped in the described health woman spirit vaginal expansion plug of pastille substrate is got, dry, take weight m, the weight X according to pastille substrate as described in formula III calculating:
X=M-m
（Ⅲ）。
Further, in the detection method of described health woman spirit vaginal expansion plug, after carrying out melting the detection of change time limit, following at least one detection method is carried out:
1) swell value assay method is as follows:
A. first choose a bit or some points along the radial direction of described health woman spirit vaginal expansion plug end face, after measuring the initial length H of described expandable carrier, then different angles of rolling measure several times, and average Hi;
B., after the clever vaginal expansion plug of described health woman carries out melting the detection of change time limit, expandable carrier expansion rear length h in selected location place in a step is determined at; Different angles of rolling again measure several times, ask average length hi after expanding;
When c. calculating described swell value, calculate according to I formula;
Wherein, pi represent axial swell value, hi represent expand after average length, Hi represent average initial length;
Or described swell value assay method is as follows:
A. first choose a place or some positions an angle along the axis of described health woman spirit vaginal expansion plug, after measuring the initial diameter R of described expandable carrier, then different angles of rolling measure several times, and average Ri;
B., after described health woman spirit vaginal expansion plug carries out melting the detection of change time limit, selected location place expandable carrier expanded diameter r in a step is determined at; Different angles of rolling again measure several times, ask average diameter ri after expanding;
When c. calculating described swell value, calculate by II formula;
Wherein, Pi represents the swell value of radial direction, ri represents the rear average diameter that expands, Ri represents average initial diameter.
Wherein said melt become time limit assay method (existing Chinese Pharmacopoeia two annex) comprising: get described health woman spirit vaginal expansion plug 3, after room temperature places 1 hour, be placed on respectively on lower floor's plectane of 3 metal rack, load in respective sleeve pipe, and with hook fix.Unless otherwise specified, be dipped vertically into respectively by said apparatus in the container filling 37.0 ± 0.5 DEG C of water being no less than 4L, its upper end position at 90mm place, underwater, should fill a rot, overturn this device in the solution once every 10 minutes in container.Above numerical range should not be construed as limitation of the present invention, and the technical scheme not in above-mentioned numerical range is also in protection scope of the present invention.
2) weight differential assay method:
A. get described health woman spirit vaginal expansion plug, take weight M;
B. scrape pastille substrate, expandable carrier is placed in 20-90 DEG C of organic solvent, take out, in 50-150 DEG C of dry 1-10h, take weight m, according to the weight X of pastille substrate as described in III formula calculating
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 health woman spirit vaginal expansion plug, described expandable carrier is cotton sliver, and described detection method comprises following at least one:
1) swell value assay method:
Get described health woman spirit vaginal expansion plug 3, survey its afterbody cotton sliver diameter with slide gauge, roll about 90 ° and survey once again, survey twice for every, obtain every 2 meansigma methods Ri measured; Above-mentioned 3 bolts are used for melt and become after the time limit measures and terminate, take out residue cotton sliver immediately, treat that water is disconnected to drip, all gently be placed on glass plate, the two ends of each cotton sliver and middle three positions are measured with slide gauge, roll after about 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 described health woman spirit vaginal expansion plug 10, accurately weighed weight respectively, gently scrape pastille substrate (cotton sliver must not be lost), cotton sliver is placed in the 200-400ml ethanol of 50-80 DEG C, preferably, cotton sliver is placed in the 300ml ethanol of 60-70 DEG C, and clean 5 minutes at 80khz frequency ultrasound, the stromatolysis of cotton sliver surface residual is removed, take out cotton sliver firmly to extract, 3 times are inhaled again with filter paper, in 105 DEG C of dryings 2 hours, take out, after room temperature places 1 hour, accurately weighed cotton sliver weight respectively, obtain every pastille matrix weight and average pastille matrix weight, every pastille matrix weight compares with average pastille matrix weight, what exceed average pastille matrix weight ± 10% must not more than 2, and 1 overrun 1 times must not be had.
The assay method of the swell value of health woman spirit vaginal expansion plug provided by the present invention adopts multi-angle repetitive measurement method, and improve the accuracy of measurement, add the operability of mensuration, method is easier to judge; When the standard detection performing state-promulgated pharmacopoeia annex weight differential health woman spirit of the present invention vaginal expansion plug, substrate need be scraped off, the scraping degree grasped due to operator is different, cause every scraping degree difference comparatively large, so the present invention adopts the substrate on dissolution with solvents expansible plug surface, through verification experimental verification, when adopting the substrate on hot ethanol cleaning 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 annex VI D high effective liquid chromatography for measuring.
It is high that health woman spirit vaginal expansion plug provided by the present invention has bioavailability, not easily soften and wait beneficial effect, and this health woman spirit vaginal expansion plug have employed seven leading technologies of original creation, expandable carrier in described health woman spirit vaginal expansion plug add " the disposable fill of stype the is integrally formed " technology applying original creation, " control of the inner core coefficient of expansion " technology, " human engineering bolt type " technology, " the clean integration for the treatment of " dosage form, " administration of intravaginal sticking type " technology, " design of lateral leakage protection key " six technology, this expandable carrier can make the pastille substrate of health woman spirit vaginal expansion plug fully contact with vaginal walls, and prevent medicinal liquid from outflowing, also there is effect that cleaning vagina prevents superinfection, after adding Rhizoma Cyperi and Ramulus Cinnamomi two taste medicine in described Chinese medicine composition, described health woman spirit vaginal expansion plug significantly increases colpitic therapeutic effect, to cervical erosion, still there is good therapeutic effect, described maltose alcohol and Emulsifier LM-102 improve the bioavailability of health woman spirit vaginal expansion plug, technology that described acrylic resin and carrageenan apply " prolonged drug layering release ", improves the action time of expansible plug to vagina, extends curative effect.
Accompanying drawing explanation
The vitro release result of the test of health woman spirit vaginal expansion plug described in Fig. 1 embodiment 7-9;
Fig. 2 and Fig. 3 swell value assay method schematic diagram.
Detailed description of the invention
Embodiment 1
Preparation method:
1) preparation of pastille substrate:
A. semi-synthetic fatty acid glyceride is placed in water-bath heating and melting, obtained fused mass;
B. the preparation of Chinese medicine composition:
I. take the Radix Et Rhizoma Rhei of recipe quantity, pulverize, add 75% alcohol reflux twice, first time adds 10 times that amount of alcohol is Radix Et Rhizoma Rhei weight, backflow 3h, second time adds 5 times that amount of alcohol is Radix Et Rhizoma Rhei weight, and backflow 1.5h, merges backflow, filter, filtrate is condensed into thick paste, and thick paste is spray dried to fine powder;
II. take the Radix Arnebiae (Radix Lithospermi) of recipe quantity, pulverize, decoct with water twice, amount of water is 10 times of Radix Arnebiae (Radix Lithospermi) weight for the first time, decocts 2h, and second time amount of water is 4 times of Radix Arnebiae (Radix Lithospermi) weight, decoct 1.5h, merge decoction liquor, filter, it be 60 DEG C of relative densities is the clear paste of 1.02 that filtrate is concentrated into temperature, add the ethanol of 80%, make alcohol content reach 70%, leave standstill, filter out precipitation, precipitation is spray dried to fine powder;
III. catechu is ground into fine powder;
IV. borneol and grinding is become fine powder;
V. by step I, II, the fine powder mix homogeneously of III and IV, obtained weight is about the Chinese medicine composition of 10g;
C. under stirring, Chinese medicine composition is added in the fused mass of step a, mix homogeneously, obtained pastille substrate;
2) preparation of expansible plug: pastille substrate is poured in bolt mould, insert cotton sliver, cooling and shaping, makes 100 pieces of bullet shaped suppositorys, every piece of heavily about 3.4g;
Embodiment 2
Preparation method: make 100 pieces of clavate suppositorys by method described in embodiment 1, every piece of heavily about 3.0g.
Embodiment 3
Preparation method:
1) preparation of pastille substrate:
A. Ke Kemu fat and glycerol tristearate are placed in water-bath heating and melting, mix homogeneously, obtained fused mass;
B. the preparation of Chinese medicine composition:
I. take the Radix Et Rhizoma Rhei of recipe quantity, pulverize, add 75% alcohol reflux twice, first time adds 10 times that amount of alcohol is Radix Et Rhizoma Rhei weight, backflow 3h, second time adds 5 times that amount of alcohol is Radix Et Rhizoma Rhei weight, and backflow 1.5h, merges backflow, filter, filtrate is condensed into thick paste, and thick paste is spray dried to fine powder;
II. take the Radix Arnebiae (Radix Lithospermi) of recipe quantity, pulverize, decoct with water twice, amount of water is 10 times of Radix Arnebiae (Radix Lithospermi) weight for the first time, decocts 2h, and second time amount of water is 4 times of Radix Arnebiae (Radix Lithospermi) weight, decoct 1.5h, merge decoction liquor, filter, it be 60 DEG C of relative densities is the clear paste of 1.02 that filtrate is concentrated into temperature, add the ethanol of 80%, make alcohol content reach 70%, leave standstill, filter out precipitation, precipitation is spray dried to fine powder;
III. catechu is ground into fine powder;
IV. borneol and grinding is become fine powder;
V. take Rhizoma Cyperi and the Ramulus Cinnamomi of recipe quantity, pulverize, add the alcohol reflux twice of 85%, first time adds 15 times that amount of alcohol is Rhizoma Cyperi and Ramulus Cinnamomi gross weight, backflow 1.5h, second time adds 10 times that amount of alcohol is Radix Et Rhizoma Rhei weight, backflow 1h, merges backflow, filters, filtrate is condensed into thick paste, and thick paste is spray dried to fine powder
VI. by step I, II, III, the fine powder mix homogeneously of IV and V, obtained weight is about the Chinese medicine composition of 35g;
C., under grinding, slowly Chinese medicine composition is mixed homogeneously with maltose alcohol, continue to grind to form pastel;
D. under stirring, pastel is added in the fused mass of step a, mix homogeneously, obtained pastille substrate;
2) preparation of expansible plug: pastille substrate poured in bolt mould, insert cotton sliver, cooling and shaping, makes 100 pieces of torpedo suppositorys, every piece of heavily about 5.0g.
Embodiment 4
Preparation method:
1) preparation of pastille substrate:
A. Oleum Linderae and trilaurin are placed in water-bath heating and melting, mix homogeneously, obtained fused mass;
B. the preparation of Chinese medicine composition: obtain the Chinese medicine composition that weight is about 10g by the method for the Chinese medicine composition described in embodiment 1;
C., under grinding, slowly Chinese medicine composition is mixed homogeneously with maltose alcohol, Emulsifier LM-102, continue to grind to form pastel;
D. under stirring, mixed pastel is added in the fused mass described in step a, mix homogeneously, obtained pastille substrate;
2) preparation of expansible plug: pastille substrate poured in bolt mould, insert cotton sliver, cooling and shaping, makes 100 pieces of duckbill suppositorys, every piece of heavily about 1.9g.
Embodiment 5
Preparation method:
1) preparation of pastille substrate:
A. cocoa butter and glycerol three Colophonium grease are placed in water-bath heating and melting, mix homogeneously, obtained fused mass;
B. the preparation of Chinese medicine composition: obtain the Chinese medicine composition that weight is about 6g by the method for the Chinese medicine composition described in embodiment 3;
C., under grinding, slowly Chinese medicine composition is mixed homogeneously with maltose alcohol, Emulsifier LM-102, continue to grind to form pastel;
D. under stirring, mixed pastel is added in the fused mass described in step a, mix homogeneously, obtained pastille substrate;
2) preparation of expansible plug: pastille substrate poured in bolt mould, insert cotton sliver, cooling and shaping, makes 100 pieces of cylindrical suppositorys, every piece of heavily about 2.6g.
Embodiment 6
Preparation method: make 100 pieces of avette suppositorys by method described in embodiment 5, every piece of heavily about 3.1g.
Embodiment 7
Preparation method:
1) preparation of pastille substrate:
A. PEG400, polyethylene glycol 6000 and polysorbate60 are placed in water-bath heating and melting, mix homogeneously, obtained fused mass;
B. the preparation of Chinese medicine composition: obtain the Chinese medicine composition that weight is about 7g by the method for the Chinese medicine composition described in embodiment 1;
C., under grinding, slowly Chinese medicine composition is mixed homogeneously with maltose alcohol, Emulsifier LM-102, continue to grind to form pastel;
D. carrageenan is placed in water-bath heating and melting, adds acrylic resin under stirring, mix homogeneously, continue to stir, add the pastel of step c, mix homogeneously, obtained mixture;
E. under stirring, the mixture of steps d is added in the fused mass of step a, mix homogeneously, obtained pastille substrate;
2) preparation of expansible plug: pastille substrate poured in bolt mould, insert cotton sliver, cooling and shaping, makes 100 pieces of conical suppositorys, every piece of heavily about 4.3g.
Embodiment 8
Preparation method: make 100 pieces of spherical suppositorys by method described in embodiment 7, every piece of heavily about 3.1g.
Embodiment 9
Preparation method:
1) preparation of pastille substrate:
A. oleum sapii and trilaurin are placed in water-bath heating and melting, mix homogeneously, obtained fused mass;
B. the preparation of Chinese medicine composition: obtain the Chinese medicine composition that weight is about 20g by the method for the Chinese medicine composition described in embodiment 3;
C., under grinding, slowly Chinese medicine composition is mixed homogeneously with maltose alcohol, Emulsifier LM-102, continue to grind to form pastel;
D. carrageenan is placed in water-bath heating and melting, adds acrylic resin under stirring, mix homogeneously, continue to stir, add the pastel of step c, mix homogeneously, obtained mixture;
E. under stirring, the mixture of steps d is added in the fused mass of step a, mix homogeneously, obtained pastille substrate;
2) preparation of expansible plug: pastille substrate poured in bolt mould, insert cotton sliver, cooling and shaping, makes 100 pieces of clavate suppositorys, every piece of heavily about 3.6g.
Test example 1 stability test
1. accelerated test
Health woman spirit vaginal expansion plug described in Example 3-9 and common health woman spirit bolt, all at constant temperature 30 DEG C ± 2 DEG C, relative humidity is place 6 months under the constant humidity condition of 65% ± 5%, duration of test 1 month, 2 months, 3 months, 6 the end of month sample once respectively, by the regulation in Chinese Pharmacopoeia, detect the shape of expansible plug, containing the labelled amount (%) of emodin, melt and become the time limit, the accelerated test of the health woman spirit vaginal expansion plug described in embodiment 3-7 the results are shown in Table 1, the accelerated test of the health woman spirit vaginal expansion plug described in embodiment 8-9 and common health woman spirit bolt the results are shown in Table 2.
The accelerated test result of the health woman spirit vaginal expansion plug of table 1 embodiment 3-7
The health woman spirit vaginal expansion plug of table 2 embodiment 8-9 and the accelerated test result of health woman spirit suppository
As can be seen from the table described in embodiment of the present invention 3-9 health woman spirit vaginal expansion plug, under the environment of constant temperature high humidity, places after 6 months, the color of described expansible plug, the labelled amount containing emodin, melt change the time limit all there is not obvious change; And common health woman spirit suppository is placed after 6 months under high humidity, suppository color changes, and speckle appears in suppository surface, part suppository generation fracture phenomena; And in described health woman spirit suppository, the content of emodin obviously declines, and melts change duration; Show that health woman of the present invention spirit vaginal expansion plug stability compared with health woman spirit suppository significantly improves.
2. long term test
Health woman spirit vaginal expansion plug described in Example 3-9 and health woman spirit bolt, at temperature 25 DEG C ± 2 DEG C, relative humidity is place 36 months under the condition of 60% ± 10%, 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, containing the labelled amount (%) of emodin, 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 detects, and testing result compared with 0 month, the long-term test results of the health woman spirit vaginal expansion plug described in embodiment 3-6 is in table 3, the long-term test results of the health woman spirit vaginal expansion plug described in embodiment 7-9 and health woman spirit bolt is in table 4.
The long-term test results of the health woman spirit vaginal expansion plug of table 3 embodiment 3-6
The health woman spirit vaginal expansion plug of table 4 embodiment 7-9 and the long-term test results of common health woman spirit suppository
As can be seen from the table described in embodiment 3-9 health woman spirit vaginal expansion plug, under the environment of constant temperature high humidity, places after 36 months, the color of described expansible plug, the labelled amount containing emodin, melt change the time limit all there is not obvious change; And after common health woman spirit suppository places 9 months, suppository color changes, and places after 18 months, and speckle appears in suppository surface, and part suppository breaks; And in health woman spirit suppository, the content of emodin significantly declines, and melts and becomes time limit significant prolongation; Show that health woman of the present invention spirit vaginal expansion plug stability compared with health woman spirit suppository significantly improves.
Test example 2 vitro release determination test
The drug release rate of suppository detects: check with reference to 2010 editions " Chinese Pharmacopoeia " annex XIXD vitro drug release degree.
Get the health woman spirit vaginal expansion plug described in above embodiment 7-9 respectively, put in medicament dissolution instrument, sample respectively in 1h, 2h, 4h, 6h, 12h, 16h, 24h, detect stripping percentage rate by high performance liquid chromatography, and calculate the cumulative release percentage rate of medicine, the results are shown in Figure 1.
As can be seen from the figure health woman spirit vaginal expansion plug slow releasing in 24h described in embodiment 7-9.
Test example 3 swell value determination test
Method one
Get described health woman spirit vaginal expansion plug 3, survey its afterbody cotton sliver diameter with slide gauge, roll about 90 ° and survey once again, survey twice for every, obtain every 2 meansigma methods Ri measured; Above-mentioned 3 bolts are used for melt and become after the time limit measures and terminate, take out residue cotton sliver immediately, treat that water is disconnected to drip, all gently be placed on glass plate, measure the two ends of each cotton sliver and middle three positions with slide gauge, roll after about 90 ° and measure three positions again, each cotton sliver obtains six data altogether, obtain 6 meansigma methods ri of mensuration, calculate the swell value Pi of every, the swell value of three bolts is all greater than 1.5.
The swell value measuring health woman spirit vaginal expansion plug described in embodiment 1-9 according to above-mentioned swell value assay method is as shown in table 5;
The swell value of the health woman spirit vaginal expansion plug described in table 5 embodiment 1-9
| Embodiment | Average diameter (mm) before expanding | Average diameter (mm) after expanding | Swell value (doubly) | Result |
| Embodiment 1 | 11.98 | 21.75 | 1.82 | Qualified |
| Embodiment 2 | 11.86 | 20.36 | 1.72 | Qualified |
| Embodiment 3 | 11.95 | 21.08 | 1.76 | Qualified |
| Embodiment 4 | 12.17 | 22.74 | 1.87 | Qualified |
| Embodiment 5 | 12.03 | 21.69 | 1.80 | Qualified |
| Embodiment 6 | 11.91 | 21.33 | 1.79 | Qualified |
| Embodiment 7 | 12.08 | 22.17 | 1.84 | Qualified |
| Embodiment 8 | 12.12 | 22.49 | 1.86 | Qualified |
| Embodiment 9 | 12.21 | 22.25 | 1.82 | Qualified |
Method two
As shown in Figures 2 and 3, the detection method of vaginal expansion plug:
1) swell value assay method:
A. first C1, C2, C3 tri-points are chosen along the radial direction of described vaginal expansion plug end face, measure initial length H1, H2, H3 of described expandable carrier with slide gauge after, roll again 90 ° and measure, choose after C1, C4, C5 tri-some slide gaugies measure initial length H4, H5, H6 of described expandable carrier along the radial direction of described vaginal expansion plug end face, ask the meansigma methods Hi of H1, H2, H3, H4, H5 and H6;
B., after described vaginal expansion plug carries out melting the detection of change time limit, C1, C2, C3 selected in a step tri-rear length h1 of position expandable carrier expansion, h2, h3 is determined at slide gauge; Roll 90 ° again, be determined at C1, C4, C5 selected in a step tri-rear length h4 of position expandable carrier expansion, h5, h6 with slide gauge, ask the average length of h1, h2, h3, h4, h5 and h6, be average length hi after expanding;
When c. calculating described swell value, calculate according to I formula;
Wherein, pi represent axial swell value, hi represent expand after average length, Hi represent average initial length;
Or, swell value assay method:
D. first A1, A2 and A3 tri-points are chosen an angle along the axis of described vaginal expansion plug, measure initial diameter R1, R2 and R3 of described expandable carrier with slide gauge after, roll 90 ° again, axis along described vaginal expansion plug chooses B1, B2 and B3 tri-points, measure initial diameter R4, R5 and R6 of described expandable carrier with slide gauge after, ask the meansigma methods Ri of R1, R2, R3, R4, R5 and R6 six initial diameters;
E., after described vaginal expansion plug carries out melting the detection of change time limit, be determined at selected A1, A2 and A3 position expandable carrier expanded diameter in d step and be respectively r1, r2 and r3; B1, B2 and B3 position expandable carrier expanded diameter measured selected by d step that rolls again 90 ° is respectively r4, r5 and r6, asks the meansigma methods of r1, r2, r3, r4, r5 and r6, average diameter ri after must expanding;
When f. calculating described swell value, calculate by II formula;
Wherein, Pi represents the swell value of radial direction, ri represents the rear average diameter that expands, Ri represents average initial diameter.
Test example 4 weight differential determination test
Get described health woman spirit vaginal expansion plug 10, accurately weighed weight respectively, gently scrape pastille substrate (cotton sliver must not be lost), cotton sliver is placed in the 300ml ethanol of 60-70 DEG C, and clean 5 minutes at 80khz frequency ultrasound, the stromatolysis of cotton sliver surface residual is removed, take out cotton sliver firmly to extract, 3 times are inhaled again with filter paper, in 105 DEG C of dryings 2 hours, take out, after room temperature places 1 hour, accurately weighed cotton sliver weight respectively, obtain every pastille matrix weight and average pastille matrix weight, every pastille matrix weight compares with average pastille matrix weight, what exceed average pastille matrix weight ± 10% must not more than 2, and 1 overrun 1 times must not be had.
Repeat aforesaid operations, detect the health woman spirit vaginal expansion plug described in embodiment 1-9, the equal conformance with standard of its weight differential.
Test example 5 is to colpitic therapeutic effect
1. test case: accept for medical treatment patient totally 70 example, be all diagnosed as vaginitis through gynecologial examination, the age 21-60 year between.
2. diagnostic criteria: all patients is all made a definite diagnosis according to medical history, vulvar secretions lab testing; Disease is pudendum, pruritus of vagina, pain, and vaginal secretions increases, can with frequent micturition, dysurea; Gynecologial examination: vaginal secretions can be had to increase, the congested or visible speckles of vaginal mucosa, there is leucorrhea vagina depths, in lark or yellow purulent secretion; The visible edema of pudendum, scratch;
3. grouping and administration: 70 routine patients are divided at random treatment group 47 example and matched group 23 example, treatment group gives the vaginal expansion plug of the health woman spirit described in embodiment 9, and matched group gives health woman spirit bolt, and two groups of administrations are once a day, within 7 days, are a course for the treatment of;
4. efficacy assessment standard:
Recovery from illness: transference cure, gynecologial examination is normal;
Effective: symptom obviously alleviates, gynecologial examination is clearly better;
Effective: symptom alleviates to some extent, gynecologial examination takes a turn for the better;
Invalid: symptom is without improvement, and gynecologial examination does not change;
5. result: the observation carrying out 4 courses for the treatment of by a definite date to 70 routine patients, the results are shown in Table 6;
Table 6 liang group compares colpitic therapeutic effect
As can be seen from the table, the health woman spirit vaginal expansion plug described in the embodiment of the present invention has significant therapeutic effect to vaginitis, and effective percentage is 97.9%, significant difference (P<0.05) compared with matched group; And in experimentation, there is not toxic and side effects.
The therapeutic effect of test example 6 pairs of cervical erosion
1. test case: accept for medical treatment patient totally 80 example, be all diagnosed as patients of cervical ruin, the age 25-55 year between, get rid of gestation, age of sucking patient;
2. diagnostic criteria: cervical erosion: cervical surface takes on a red color, is that squamous epithelial cancer comes off, is replaced by columnar epithelium, the result that upper veins beneath the skin appears; The Normal squamous epithelium of rotten to the corn face and surrounding has clearly boundary, is coated with iodine liquid not painted; Divide gently according to the size of rotten to the corn area, in, weigh three degree;
Slight erosion: cervical erosion face accounts for cervix uteri area and is less than 1/3;
Moderate is rotten to the corn: cervical erosion face accounts for the 1/3-2/3 of whole cervix uteri area;
Severe is rotten to the corn: cervical erosion face exceedes 2/3 of cervix uteri area;
According to rotten to the corn face, inflammatory degree, vaginal secretions cleannes and symptom scores, comprehensive grading integration summation, 3-6 is divided into slightly, and 7-11 is divided into moderate, and more than 12 points is severe;
3. grouping and administration: 80 routine patients are divided at random treatment group 55 example and matched group 25 example, treatment group gives the vaginal expansion plug of the health woman spirit described in embodiment 9, and matched group gives health woman spirit bolt, and two groups of administrations are once a day, within 7 days, are a course for the treatment of;
4. observation item
Observation of curative effect: symptom; Gynecologial examination, comprises the inspection of cervix uteri, pudendum, vagina and vaginal secretions; Lab testing, under comprising mirror to vaginal secretions inspection and smear;
5. efficacy assessment standard:
Cervical erosion: main detection cervical erosion face changes, degree of inflammation changes, and vagina cleanness degree changes, and clinical symptoms etc. change and compare in conjunction with before and after standards of grading, treatment:
Recovery from illness: cervical erosion face is covered by squamous epithelial cancer, heal completely, be coated with iodine liquid all coloring, inflammation disappears, and clinical symptoms disappears;
Effective: cervical erosion face reduces 1/3-2/3 before comparatively treating, various disease integration drops to less than 1/3 before treatment;
Effective: cervical erosion face reduces 1/3 before comparatively treating, various disease integration drops to less than 2/3 before treatment;
Invalid: treatment after cervical erosion face and various disease all unchanged, symptom is without improvement;
6. result: the observation carrying out 4 courses for the treatment of by a definite date to 80 routine patients, the results are shown in shown in following table;
The therapeutic effect of table 7 liang group to cervical erosion compares
Can find out that treatment group is obviously better than matched group (P<0.01) by table;
Table 8 liang group is to integration situation of change before and after cervical erosion treatment
Treatment group and matched group compare and there is significant difference (P<0.01);
Table 9 liang group compares cervical erosion therapeutic effect in various degree
Treatment group is obviously better than contrasting (P<0.01) to the curative effect of cervical erosion as can be seen from the table;
7. result: health woman spirit vaginal expansion plug has good therapeutic effect to cervical erosion, and total effective rate reaches more than 98%, compared with matched group, raising evident in efficacy; In its curative effect process of checking, do not find the abnormal phenomena caused by expansible plug and untoward reaction.
Claims (10)
1. a health woman spirit vaginal expansion plug, it is characterized in that, described expansible plug comprises the Chinese medicine composition that weight portion is 6-35 part, weight portion is the substrate of 70-220 part, 3-7.5 the maltose alcohol of part, the Emulsifier LM-102 of 0.7-2.3 part, the acrylic resin of 1-4 part and the carrageenan of 0.5-2 part and weight portion are the expandable expandable carrier of 60-400 part, described Chinese medicine composition and substrate and maltose alcohol, Emulsifier LM-102, the pastille substrate that acrylic resin and carrageenan are formed is coated in expandable carrier surface, the swell value of described expandable carrier after saturated water suction is greater than 1.1, described Chinese medicine composition is prepared from through processing primarily of the crude drug of following weight portion:
Radix Et Rhizoma Rhei 30-150 catechu 1-10 Radix Arnebiae (Radix Lithospermi) 15-100
Borneolum Syntheticum 0.5-4
Described substrate is the mixture of natural acid ester and glyceride, and the ratio of weight and number of described natural acid ester and glyceride is 3-7:1;
Described natural acid ester be selected from oleum sapii, Oleum Linderae, Fructus Foeniculi fat, Ke Kemu fat or cocoa butter one or more;
Described glyceride be selected from tripalmitin, glycerol tristearate, glycerol three rosin ester or trilaurin one or more.
2. health woman spirit vaginal expansion plug as claimed in claim 1, is characterized in that, prepares the Ramulus Cinnamomi that the raw materials used medicine of described Chinese medicine composition also comprises Rhizoma Cyperi that parts by weight are 30-150 part and 15-100 part.
3. health woman spirit vaginal expansion plug as claimed in claim 1, is characterized in that, described natural acid ester to be weight portion the be Fructus Foeniculi fat of 75 parts, described glyceride to be weight portion the be tripalmitin of 15 parts; The weight portion of described Chinese medicine composition is 10 parts, and the weight portion of described expandable carrier is 200 parts, and the parts by weight preparing the raw materials used medicine of described Chinese medicine composition are:
Radix Et Rhizoma Rhei 67.4 catechu 2.74 Radix Arnebiae (Radix Lithospermi) 27.4
Borneolum Syntheticum 1.92.
4. the health woman spirit vaginal expansion plug as described in as arbitrary in claim 1-3, it is characterized in that, the swell value of described expandable carrier after saturated water suction is greater than 1.5, and described swell value is radial swell value; Described expandable carrier is cotton sliver; Described pastille substrate is the 1/5-4/5 place, front end that Semi surrounding type is coated in described expandable carrier, and the rear end of described expandable carrier is connected with bracing wire; After described expandable carrier water suction, the maximum water absorption of every is not less than 1.5 milliliters.
5. the preparation method of health woman spirit vaginal expansion plug as claimed in claim 1, it is characterized in that, described method comprises the steps:
1) preparation of pastille substrate:
A. substrate is placed in water-bath heating and melting, mix homogeneously, obtained fused mass;
B. the preparation of Chinese medicine composition:
I. take the Radix Et Rhizoma Rhei of recipe quantity, pulverize, add 75% alcohol reflux twice, first time adds 10 times that amount of alcohol is Radix Et Rhizoma Rhei weight, backflow 3h, second time adds 5 times that amount of alcohol is Radix Et Rhizoma Rhei weight, and backflow 1.5h, merges backflow, filter, filtrate is condensed into thick paste, and thick paste is spray dried to fine powder;
II. take the Radix Arnebiae (Radix Lithospermi) of recipe quantity, pulverize, decoct with water twice, amount of water is 10 times of Radix Arnebiae (Radix Lithospermi) weight for the first time, decocts 2h, and second time amount of water is 4 times of Radix Arnebiae (Radix Lithospermi) weight, decoct 1.5h, merge decoction liquor, filter, it be 60 DEG C of relative densities is the clear paste of 1.02 that filtrate is concentrated into temperature, add the ethanol of 80%, make alcohol content reach 70%, leave standstill, filter out precipitation, precipitation is spray dried to fine powder;
III. catechu is ground into fine powder;
IV. borneol and grinding is become fine powder;
V. by step I, II, the fine powder mix homogeneously of III and IV, obtained Chinese medicine composition;
C., under grinding, slowly Chinese medicine composition is mixed homogeneously with maltose alcohol, Emulsifier LM-102, continue to grind to form pastel;
D. carrageenan is placed in water-bath heating and melting, adds acrylic resin under stirring, mix homogeneously, continue to stir, add the pastel of step c, mix homogeneously, obtained mixture;
E. under stirring, the mixture of steps d is added in the fused mass of step a, mix homogeneously, obtained pastille substrate;
2) preparation of expansible plug: pastille substrate poured in bolt mould, insert expandable carrier, cooling and shaping, makes suppository.
6. the preparation method of rehabilitation spirit vaginal expansion plug as claimed in claim 5, it is characterized in that, the preparation method of described Chinese medicine composition also comprises step Rhizoma Cyperi and Ramulus Cinnamomi being made fine powder, described step is as follows: the Rhizoma Cyperi and the Ramulus Cinnamomi that take recipe quantity, pulverize, add the alcohol reflux twice of 85%, first time adds 15 times that amount of alcohol is Rhizoma Cyperi and Ramulus Cinnamomi gross weight, backflow 1.5h, second time adds 10 times that amount of alcohol is Radix Et Rhizoma Rhei weight, backflow 1h, merge backflow, filter, filtrate is condensed into thick paste, and thick paste is spray dried to fine powder.
7. the detection method of the health woman spirit vaginal expansion plug as described in as arbitrary in claim 1-3, it is characterized in that, described detection method comprises following at least one method:
1) swell value assay method is as follows:
A. the radial direction along described health woman spirit vaginal expansion plug end face is chosen a bit or some points, measures the initial length H of described expandable carrier;
B., after the saturated water suction of described health woman spirit vaginal expansion plug, expandable carrier expansion rear length h in selected location place in a step is determined at;
When c. calculating described swell value, calculate according to I formula;
(I)
Wherein, p represent axial swell value, h represent expand after length, H represent initial length; Or swell value assay method is as follows:
A. the axis along described health woman spirit vaginal expansion plug chooses a place or some positions, measures the initial diameter R of described expandable carrier;
B., after the saturated water suction of described health woman spirit vaginal expansion plug, selected location place expandable carrier expanded diameter r in a step is determined at;
When c. calculating described swell value, calculate by II formula;
(II)
Wherein, P represents the swell value of radial direction, r represents expanded diameter, R represents initial diameter;
2) weight differential assay method:
A. get described health woman spirit vaginal expansion plug, take weight M;
B. the expandable carrier scraped in the described health woman spirit vaginal expansion plug of pastille substrate is got, dry, take weight m, the weight X according to pastille substrate as described in formula III calculating:
X＝M-m
(Ⅲ)。
8. the detection method of health woman spirit vaginal expansion plug as claimed in claim 7, is characterized in that, after carrying out melting the detection of change time limit, then carries out following at least one detection method:
1) swell value assay method is as follows:
A. first choose a bit or some points along the radial direction of described health woman spirit vaginal expansion plug end face, after measuring the initial length H of described expandable carrier, then different angles of rolling measure several times, and average Hi;
B., after the clever vaginal expansion plug of described health woman carries out melting the detection of change time limit, expandable carrier expansion rear length h in selected location place in a step is determined at; Different angles of rolling again measure several times, ask average length hi after expanding;
When c. calculating described swell value, calculate according to I formula;
(I)
Wherein, pi represent axial swell value, hi represent expand after average length, Hi represent average initial length;
Or swell value assay method is as follows:
A. first choose a place or some positions an angle along the axis of described health woman spirit vaginal expansion plug, after measuring the initial diameter R of described expandable carrier, then different angles of rolling measure several times, and average Ri;
B., after described health woman spirit vaginal expansion plug carries out melting the detection of change time limit, selected location place expandable carrier expanded diameter r in a step is determined at; Different angles of rolling again measure several times, ask average diameter ri after expanding;
When c. calculating described swell value, calculate by II formula;
(II)
Wherein, Pi represents the swell value of radial direction, ri represents the rear average diameter that expands, Ri represents average initial diameter;
2) weight differential assay method:
A. get described health woman spirit vaginal expansion plug, take weight M;
B. scrape pastille substrate, expandable carrier is placed in 20-90 DEG C of organic solvent, take out, in 50-150 DEG C of dry 1-10h, take weight m, according to the weight X of pastille substrate as described in III formula calculating
X＝M-m(Ⅲ)
Wherein, described organic solvent is selected from one or more in ethanol, methanol or isopropyl alcohol.
9. the detection method of health woman spirit vaginal expansion plug as claimed in claim 8, it is characterized in that, described expandable carrier is cotton sliver, and described detection method comprises following at least one method:
1) swell value assay method:
Get described health woman spirit vaginal expansion plug 3, survey its afterbody cotton sliver diameter with slide gauge, roll 90 ° and survey again once, survey twice for every, obtain every 2 meansigma methods Ri measured; Above-mentioned 3 bolts are used for melt and become after the time limit measures and terminate, take out residue cotton sliver immediately, treat that water is disconnected to drip, all gently be placed on glass plate, the two ends of each cotton sliver and middle three positions are measured with slide gauge, roll 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 described health woman spirit vaginal expansion plug 10, accurately weighed weight respectively, gently scrape pastille substrate, cotton sliver must not be lost, cotton sliver is placed in the 200-400ml ethanol of 50-80 DEG C, and clean 5 minutes at 80khz frequency ultrasound, the stromatolysis of cotton sliver surface residual is removed, take out cotton sliver firmly to extract, 3 times are inhaled again with filter paper, in 105 DEG C of dryings 2 hours, take out, after room temperature places 1 hour, accurately weighed cotton sliver weight respectively, obtain every pastille matrix weight and average pastille matrix weight, every pastille matrix weight compares with average pastille matrix weight, what exceed average pastille matrix weight ± 10% must not more than 2, and 1 overrun 1 times must not be had.
10. the detection method of health woman spirit vaginal expansion plug as claimed in claim 9, is characterized in that, cotton sliver is placed in the 300ml ethanol of 60-70 DEG C.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101455729A (en) * | 2009-01-14 | 2009-06-17 | 通化百信药业有限公司 | Kangfulingshuan medicine production technique |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101455729A (en) * | 2009-01-14 | 2009-06-17 | 通化百信药业有限公司 | Kangfulingshuan medicine production technique |
| 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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Effective date of registration: 20211118 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: Kangfuling vaginal expansion suppository and its preparation and detection method Effective date of registration: 20230908 Granted publication date: 20160113 Pledgee: China Merchants Bank Co.,Ltd. Harbin Branch Pledgor: Harbin Tianmei Pharmaceutical Co.,Ltd. Registration number: Y2023230000075 |