CN104434545B - Cosmetics expansible plug and preparation method thereof and detection method - Google Patents
Cosmetics expansible plug and preparation method thereof and detection method Download PDFInfo
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- CN104434545B CN104434545B CN201410620994.7A CN201410620994A CN104434545B CN 104434545 B CN104434545 B CN 104434545B CN 201410620994 A CN201410620994 A CN 201410620994A CN 104434545 B CN104434545 B CN 104434545B
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Abstract
The present invention relates to a kind of cosmetics expansible plug and preparation method thereof and detection method, the expansible plug includes cosmetics, matrix and expandable expandable carrier；Cosmetics form coat with matrix, and are coated in expandable carrier surface, and swell value of the expandable carrier after saturation water suction is more than 1.1；The cosmetics expansible plug is employed cosmetics and structure of the substrate application on expandable carrier so that the cosmetics expansible plug can be applied to vagina, and play the effect of cleaning and moisturizing well；After expandable carrier expansion in expansible plug, the contact area of cosmetics expansible plug and vagina can be improved, coating is more uniform, and cleaning effect is more thorough；And the cosmetics in expansible plug employ special composition, good moisture retention, water lock, vaginal mucosa osmosis and stability are made it have.
Description
Technical field
The invention belongs to cosmetic field, more particularly to a kind of cosmetics expansible plug and preparation method thereof and detection method.
Background technology
It is well known that cosmetics are to smear, spray or other similar modes, any position of human body surface is imposed on, often
See for skin, lip etc., with the product for reaching cleaning, eliminating the purpose of bad smell, skin care, moisturizing, beauty.At present, most
Common is all that face is cleaned and the cosmetics of moisturizing, however do not occur also it is any it is a can be used in vagina, to the moon
Play the cosmetics of cleaning and moisture-keeping function in road.
And the cosmetics listed at present can not play the effect of cleaning and moisturizing well to vagina, because existing
Cosmetics majority be that NMF is added in cosmetics, this cosmetics moistening effect is poor and apt to deteriorate, it is easy to right
Vagina mucosa produces stimulation.
In addition, existing cosmetics have the forms such as liquid, frost, solid, although the cosmetics of these forms can meet difference
Man's Demands, but these forms is used for cosmetic inconvenient at vagina and cumbersome.
The content of the invention
In order to solve the above-mentioned technical problem, the present invention provides a kind of cosmetics of new model, i.e. cosmetics expansible plug, the change
Cosmetic expansible plug can be used for vagina, have the effect of good moisturizing and water lock to vagina mucosa, and without soapy feeling is sticked, simultaneously
Good cleaning action is played to vagina.
Concrete technical scheme of the present invention is as follows：
The present invention provides a kind of cosmetics expansible plug, and the expansible plug includes cosmetics, matrix and expandable expandable carrier；
Cosmetics form coat with matrix, and are coated in expandable carrier surface, and swell value of the expandable carrier after saturation water suction is more than
1.1, the parts by weight of each composition of expansible plug are：
Cosmetics 80-200
Matrix 80-200
Expandable carrier 50-400
Wherein, matrix is selected from fat-soluble matrix and/or water-soluble base；
Fat-soluble matrix is selected from mixed fatty glycerides, propylene glycol stearate, fixed oil, semi-synthetic fatty acid glycerine
Ester, semi-synthetic cocounut oil ester, Witepsol, semi-synthetic palm grease, semi-synthetic fruit of a cubeb litsea tree ester, oleum sapii, spicebush oil, fennel fat,
One or more in Ke Kemu fat, cocoa butter or lanolin；
Water-soluble base is selected from polyethylene glycol 400, polyethylene glycol 1500, Macrogol 4000, Macrogol 6000, glycerine
One or more in gelatin, polysorbate60, polysorbate65, polyoxyl 40 stearate or poloxamer.
Cosmetics expansible plug provided by the invention is to be specifically applied to vagina, and cleaning and moisture-keeping function are played to vagina；Its
" the intravaginal sticking type technology " of original creation is employed, the technology is realized by adding expandable carrier in suppository.Ordinary suppository
Due to the relation of gravity, no matter user is to stand, sitting posture or lying under formula position, always has vagina or less can not to touch painting
Coating, after the expansion of described expandable carrier, coat can contact in 360 ° with vaginal walls, play sufficiently effect, try out face
Product expands 6 times, and coat is directly attached to vagina mucosa, and plicated layer can not be contacted originally by, which making, also can effectively be attached.In addition,
The introducing of expandable carrier applies " lateral leakage protection key " design concept, can be with vaginal wall because the expansion of expandable carrier tail end
It is close to, and then prevents the outflow of coat, reduces the pollution of clothing and keep the valid density of coat.And pass through " inner core
Coefficient of expansion control technology ", swell value of the expandable carrier after saturation water suction can be made to be more than 1..
In addition, some can be added in cosmetics expansible plug provided by the invention plays sterilization, the composition of antiinflammatory action, further
The cosmetics expansible plug is set to play the effect such as anti-inflammatory.
The cosmetics majority of prior art is to add NMF wherein so as to play a part of moisturizing, but its moistening effect
It is unsatisfactory, be not suitable for applying in vagina；In order to improve the moisture retention of cosmetics expansible plug, make it that there is length to vagina mucosa
The moisturizing of time and water lock effect, cosmetics provided by the invention include each composition of following parts by weight：
Methyl acrylate copolymer 2.5-4
Polyvinyl alcohol-chitosan crosslinked thing 10-15
Glycerine 1-3.
Composition of the present invention using polyvinyl alcohol-chitosan crosslinked thing as cosmetics, serve permanent moisture-keeping function with
Water lock acts on, and will not produce glutinous soapy feeling；It is adapted to apply in vagina.
Further to improve, cosmetics also include each composition of following parts by weight：
Isopropyl cetylate 6-12
Propylene glycol diacetate 0.5-1
Microspherical carrier material 5-9.
Preferably, microspherical carrier material is that ratio of weight and number is 3:1 chitin and the mixture of Arabic gum.
Microballoon of the invention by adding isopropyl cetylate and propylene glycol diacetate in cosmetics expansible plug, carry
The high osmosis of the cosmetics expansible plug, enables the cosmetics expansible plug to be deep into the cuticula in vagina mucosa, more
The moisture-keeping function of cosmetics expansible plug is played profoundly.In addition, using the mixture of chitin and Arabic gum as microballoon
The effect of carrier material is best.
In order to improve the stability of cosmetics expansible plug, cosmetics provided by the invention are 0.2-1 also including parts by weight
The sodium citrate of part and the methyl hydroxybenzoate of 0.1-0.3 parts.
In order to improve the disintegration time limited of expansible plug, excitant of the matrix to vagina is reduced, matrix of the invention also includes accounting for
Matrix gross weight is 5% antierythrite.
Swell value of the expandable carrier of the present invention after saturation water suction is more than 1.5, and the swell value is the expansion of radial direction
Value；Described expandable carrier includes but is not limited to sliver, other sterilizable materials that can be expanded is may also include, such as non-woven fabrics, bullet
Property fiber etc..
The coat of the present invention is coated in Semi surrounding type at the front end 1/5-4/5 of the expandable carrier, according to " human body work
Cheng Xue suppositorys " shape, it is designed to the shapes such as duckbill, spherical, avette, bullet shaped, torpedo, cylinder, cone or rod.
The expandable carrier rear end of cosmetics expansible plug of the present invention is connected with bracing wire.Suppository after expansion, pass through drawing
The bracing wire of expandable carrier rear end, adsorb the virus on expandable carrier, toxin, the dead skin that comes off and also pull out external, examination every time in the lump
It is equal to do once thoroughly cleaning to vagina with the cosmetics expansible plug, prevents the generation of inflammation, play a part of cleaning.
In order to reach the effect that the cosmetics expansible plug of the present invention is met water and can expanded rapidly, after the expandable carrier water suction,
The maximum water absorption of every is not less than 1.5 milliliters.Suitable water absorption, it is ensured that suitable swell value, it is too low or too high
Water absorption, it can all cause bad influence.When water absorption is too low, it is impossible to it is i.e. swollen to ensure that cosmetics expansible plug of the present invention meets water
The characteristics of swollen and make expansion insufficient；When water absorption is too high, absorption cosmetics that expandable carrier can be excessive and limit its diffusion.Cause
This, water absorption is too low or too high, is not the desired expandable carrier of the present invention.
Another aspect of the present invention provides the preparation method of cosmetics expansible plug, and methods described comprises the following steps：
1) preparation of coat：
A. matrix is placed in heat in water-bath and melted, be well mixed, fused mass is made；
B. the preparation of microballoon：
Isopropyl cetylate and propylene glycol diacetate are dispersed in absolute ethyl alcohol by I, and dispersion liquid is made；
II is by dispersion liquid magnetic stirring apparatus in 1000rmin-1, stir at 5 DEG C, suspension be made；
III adds microspherical carrier material in absolute ethyl alcohol, stirs, and oil phase is made；
IV adds suspension made from step II in oil phase made from step III, in 1000rmin-1, stir at 5 DEG C
Uniformly, it is spray-dried, then with petroleum ether three times, drying at room temperature, the microballoon that particle size range is 15-25 μm is made；
C. methyl acrylate copolymer, polyvinyl alcohol-chitosan crosslinked thing and glycerine are well mixed, mixture is made；
D. mixture made from step c is well mixed with microballoon, sodium citrate and methyl hydroxybenzoate, cosmetics is made；
E. cosmetics made from step d are added in fused mass made from step a, be well mixed, coat is made；
2) coat is poured into bolt mould, inserts expandable carrier, cooling and shaping, expansible plug is made.
The preparation method of cosmetics expansible plug of the present invention employs disposable filling integrally formed technology；The preparation
Method is simple, easy to operate, and ensure that the cosmetics expansible plug of preparation has good moisture retention and water lock.
Another aspect of the present invention additionally provides the detection method of cosmetics expansible plug, and the detection method is surveyed including swell value
Determine method, weight differential detection method etc..
Wherein described swell value assay method includes：
If a. choosing a little or doing along the radial direction of the cosmetics expansible plug end face, the initial of the expandable carrier is determined
Length H；
B. after the cosmetics expansible plug saturation water suction, the length after expandable carrier expands at selected location during a is walked is determined
h；
When c. calculating the swell value, calculated according to I formulas；
Wherein, p represents that the swell value of axial direction, h represent length, H expression initial lengths after expansion；Or, the swell value is surveyed
It is as follows to determine method：
A. choose at one along the axial direction of the cosmetics expansible plug or some positions, determine the initial straight of the expandable carrier
Footpath R；
B. after cosmetics expansible plug saturation water suction, expandable carrier expanded diameter at selected location is determined in a steps
r；
When c. calculating the swell value, calculated by II formulas；
Wherein, P represents that the swell value of radial direction, r represent that expanded diameter, R represent initial diameter；The weight differential measure
Method includes：
A. the cosmetics expansible plug is taken, weighs weight M；
B. the expandable carrier in the cosmetics expansible plug for scraping coat is taken, dries, weight m is weighed, according to such as III
Formula calculates the weight X of the coat：
X=M-m
(Ⅲ)。
Further, in the detection method of cosmetics expansible plug of the present invention, the detection method is included as follows at least
A kind of method：
1) it is as follows to expand values determination method：
If a. first choosing a little or doing along the radial direction of the cosmetics expansible plug end face, the first of the expandable carrier is determined
After beginning length H, then roll different angle measurement several times, average Hi；
B. the cosmetics expansible plug melt become time limit detection after, determine in a steps that expandable carrier is swollen at selected location
Length h after swollen；Different angle measurement is rolled again several times, seeks average length hi after expansion；
When c. calculating the swell value, calculated according to I formulas；
Wherein, pi represents that the swell value of axial direction, hi represent average length, the average initial length of Hi expressions after expansion；
Or, it is described expansion values determination method it is as follows：
A. first an angle along the cosmetics expansible plug axial direction choose one at or some positions, determine the expansion
After the initial diameter R of carrier, then roll different angle measurement several times, average Ri；
B. the cosmetics expansible plug melt become time limit detection after, determine in a steps that expandable carrier is swollen at selected location
Diameter r after swollen；Different angle measurement is rolled again several times, seeks average diameter ri after expansion；
When c. calculating the swell value, calculated by II formulas；
Wherein, Pi represents that the swell value of radial direction, ri represent average diameter, the average initial diameter of Ri expressions after expansion.
The wherein described change time limit assay method that melts includes：The cosmetics expansible plug 3 is taken, after room temperature is placed 1 hour,
It is individually placed on lower floor's plectane of 3 metal frames, loads in respective sleeve pipe, and is fixed with hook.Unless otherwise specified, will be upper
State device and be respectively perpendicular and immerse in the container for filling 37.0 ± 0.5 DEG C of water no less than 4L, its upper end position should be in underwater
A rot is filled at 90mm, in container, the device was overturn in the solution once every 10 minutes.Above number range should not be understood
For limitation of the present invention, the technical scheme in above-mentioned number range is not within the scope of the present invention yet.
2) weight differential assay method：
A. the cosmetics expansible plug is taken, weighs weight M；
B. coat is scraped, expandable carrier is placed in 20-90 DEG C of organic solvent, is taken out, in 50-150 DEG C of dry 1-
10h, weight m is weighed, according to the weight X of the coat as described in the calculating of III formula
X=M-m (III)
Wherein, one or more of the organic solvent in ethanol, methanol or isopropanol.
Further, in the detection method of cosmetics expansible plug of the present invention, the expandable carrier is sliver, described
Detection method includes following at least one method：
1) values determination method is expanded：
The cosmetics expansible plug 3 is taken, its afterbody sliver diameter is surveyed with slide measure, rolls 90 ° and survey again once, every
Survey 2 average value Ri for twice, obtaining every measure；Above-mentioned 3 bolts are used to melt and become after time limit measure terminates, are taken out immediately surplus
Remaining sliver, the disconnected drop of water is treated, is gently placed on glass plate, the both ends of each sliver and middle three portions are determined with slide measure
Position, three positions is determined again after rolling 90 °, each sliver obtains six data altogether, obtains 6 average value r of measurei, calculate
The swell value P of everyi, the swell value of three bolts should be greater than 1.5.
2) weight differential assay method：
The cosmetics expansible plug 10 is taken, accurately weighed weight, gently scrapes coat, must not lose sliver respectively, will
Sliver is placed in 50-80 DEG C of 200-400ml ethanol, it is preferable that sliver is placed in 60-70 DEG C of 300ml ethanol, and
80khz frequency ultrasounds clean 5 minutes, remove the stromatolysis of sliver surface residual, take out sliver and firmly extract, then use filter paper
Inhale 3 times, dried 2 hours in 105 DEG C, taken out, after room temperature is placed 1 hour, accurately weighed sliver weight, obtains every coating respectively
Layer weight is with averagely coating layer weight, and every coating layer weight is compared with averagely coating layer weight, beyond average coating layer weight
± 10% must not be more than 2, and must not have 11 times of overrun.
The assay method of the swell value of cosmetics expansible plug provided by the present invention uses the multiple measuring method of multi-angle, carries
The high degree of accuracy of measurement, adds the operability of measure, and method is easier to judge.
Cosmetics expansible plug provided by the present invention is employed cosmetics and structure of the substrate application on expandable carrier,
So that the cosmetics expansible plug can be applied to vagina, and play the effect of cleaning and moisturizing well；Expansion in expansible plug
After carrier expansion, the contact area of cosmetics expansible plug and vagina can be improved, coating is more uniform, and cleaning effect is more thorough；
And the cosmetics in expansible plug employ special composition, good moisture retention, water lock, vaginal mucosa osmosis are made it have
Property and stability.
Brief description of the drawings
Fig. 1 uses vagina mucosa transepidermal water content results after test sample；
The schematic diagram of Fig. 2 and Fig. 3 expansion values determination methods.
Embodiment
Embodiment 1
Preparation method：
1) preparation of coat：
A. semi-synthetic fatty glyceride is placed in heat in water-bath and melted, be well mixed, fused mass is made；
B. methyl acrylate copolymer, polyvinyl alcohol-chitosan crosslinked thing and glycerine are well mixed, cosmetics is made；
C. cosmetics made from step c are added in fused mass made from step a, be well mixed, coat is made；
2) coat is poured into bolt mould, inserts sliver, cooling and shaping, 100 pieces of bullet shaped expansible plugs are made, every piece weighs about
2.3g。
Embodiment 2
Preparation method：100 pieces of spherical expansible plugs are made in method according to embodiment 1, and every piece weighs about 5.0g.
Embodiment 3
Preparation method：
1) preparation of coat：
A. polyoxyl 40 stearate is placed in heat in water-bath and melted, be well mixed, fused mass is made；
B. the preparation of microballoon：
Isopropyl cetylate and propylene glycol diacetate are dispersed in absolute ethyl alcohol by I, and dispersion liquid is made；
II is by dispersion liquid magnetic stirring apparatus in 1000rmin-1, stir at 5 DEG C, suspension be made；
III adds microspherical carrier material in absolute ethyl alcohol, stirs, and oil phase is made；
IV adds suspension made from step II in oil phase made from step III, in 1000rmin-1, stir at 5 DEG C
Uniformly, it is spray-dried, then with petroleum ether three times, drying at room temperature, the microballoon that particle size range is 15-25 μm is made；
C. methyl acrylate copolymer, polyvinyl alcohol-chitosan crosslinked thing and glycerine are well mixed, mixture is made；
D. mixture made from step c is well mixed with microballoon, cosmetics is made；
E. cosmetics made from step d are added in fused mass made from step a, be well mixed, coat is made；
2) coat is poured into bolt mould, inserts sliver, cooling and shaping, 100 pieces of rod expansible plugs are made, every piece weighs about
4.2g。
Embodiment 4
Preparation method：100 pieces of avette expansible plugs are made in method according to embodiment 3, and every piece weighs about 4.8g.
Embodiment 5
Preparation method：
1) preparation of coat：
A. poloxamer and polysorbate60 are placed in heat in water-bath and melted, be well mixed, fused mass is made；
B. the preparation of microballoon：
Isopropyl cetylate and propylene glycol diacetate are dispersed in absolute ethyl alcohol by I, and dispersion liquid is made；
II is by dispersion liquid magnetic stirring apparatus in 1000rmin-1, stir at 5 DEG C, suspension be made；
III adds microspherical carrier material in absolute ethyl alcohol, stirs, and oil phase is made；
IV adds suspension made from step II in oil phase made from step III, in 1000rmin-1, stir at 5 DEG C
Uniformly, it is spray-dried, then with petroleum ether three times, drying at room temperature, the microballoon that particle size range is 15-25 μm is made；
C. methyl acrylate copolymer, polyvinyl alcohol-chitosan crosslinked thing and glycerine are well mixed, mixture is made；
D. mixture made from step c is well mixed with microballoon, sodium citrate and methyl hydroxybenzoate, cosmetics is made；
E. cosmetics made from step d are added in fused mass made from step a, be well mixed, coat is made；
2) coat is poured into bolt mould, inserts expandable carrier, cooling and shaping is made 100 pieces of cylindrical expansible plugs, every piece
Weigh about 6.3g.
Embodiment 6
Preparation method：100 pieces of torpedo expansible plugs are made in method according to embodiment 5, and every piece weighs about 4.8g.
Embodiment 7
Preparation method：100 pieces of duckbill expansible plugs are made according to the method for embodiment 5, every piece weighs about 3.2g.
Embodiment 8
Preparation method：100 pieces of bullet shaped expansible plugs are made according to the method for embodiment 5, every piece weighs about 4.8g.
Comparative examples 1
Preparation method：Prepared according to the method for embodiment 1.
Comparative examples 2
Preparation method：Preparation method：
1) preparation of coat：
A. polyoxyl 40 stearate is placed in heat in water-bath and melted, be well mixed, fused mass is made；
B. methyl acrylate copolymer, polyvinyl alcohol-chitosan crosslinked thing and glycerine are well mixed, mixture is made；
C. mixture made from step b is well mixed with isopropyl cetylate and propylene glycol diacetate, is made and makes up
Product；
D. cosmetics made from step c are added in fused mass made from step a, be well mixed, coat is made；
2) coat is poured into bolt mould, inserts sliver, cooling and shaping, 100 pieces of rod expansible plugs are made, every piece weighs about
4.2g。
Comparative examples 3
Preparation method：Prepared according to the method for embodiment 5.
The moisture retention of test example 1 is tested
1.1 test apparatus
Corneometer CM 825 (CK Electronic GmbH, Germany) moisture tester, computer, thermometer and
Hygrometer；
1.2 test sample
Embodiment 1, embodiment 3, comparative examples 1 and the cosmetics expansible plug of comparative examples 2, and ordinary cosmetics are made
Expansible plug；
1.3 test method
1. tested crowd：25 people, age 20-40 year, sex female；
2. testing experiment
Test environment temperature is 25 DEG C, and relative humidity (RH) is 65%, and tested crowd is randomly divided into 5 groups, every group of 5 people,
And it is 3 groups of 1 group of 1 group of experiment, 2 groups of experiment and control, 2 groups of control and control to be numbered；Test 1 group and 2 groups of experiment makes respectively
With the cosmetics expansible plug of the embodiment of the present invention 1 and embodiment 3,3 groups of 1 group of control, 2 groups of control and control use to according to the facts respectively
Apply expansible plug made of the cosmetics expansible plug and ordinary cosmetics of example 1, comparative examples 2；Before use, with
The testers of Corneometer CM 825 are determined by the cuticula moisture of intravaginal；Take 1 piece of above-mentioned test sample, insertion the moon
In road, measured, tested out respectively using the testers of Corneometer CM 825 in 0.5h, 1h, 2h, 3h, 6h, 12h
Vagina mucosa keratoderma moisture content value, unit a.u.；Test result is shown in Fig. 1.
From figure 1 it appears that polyvinyl alcohol-chitosan crosslinked thing is added in cosmetics expansible plug can significantly improve the moon
Moisture in road mucous membrane cuticula, there is good moisture retention, when polyvinyl alcohol and chitosan are not in the form of cross-linking agent
In the presence of in expansible plug, its moisture retention is remarkably decreased；And after lacking one of composition, moisture retention is also with decline；Add simultaneously
The microballoon entered can further improve the moisture retention of expansible plug, and the cuticula of vagina mucosa can be penetrated into deeper into ground.
The stability test of test example 2
1. accelerated test
The cosmetics expansible plug described in cosmetics expansible plug and comparative examples 3 described in Example 1,3,5, in perseverance
Temperature 30 DEG C ± 2 DEG C at, relative humidity be 65% ± 5% constant humidity under the conditions of place 6 months, 1 month during experiment, 2 months,
3 months, 6 the end of month it is separately sampled once, detect the character of expansible plug, as a result find, the stability of the expansible plug of embodiment 5 is most
It is good, and there is spot in the expansible plug surface of embodiment 1 and embodiment 3 and comparative example 3 batch, and demi-inflation bolt splits
Trace.
2. long term test
The cosmetics expansible plug described in cosmetics expansible plug and comparative examples 3 described in Example 1,3,5, in temperature
Degree 25 DEG C ± 2 DEG C, humidity be 60% ± 10% under conditions of place 24 months, 0 month during experiment, 3 months, 6 months, 9
Individual month, 12 months, 18 months, 24 the end of month it is separately sampled once, detect the character of expansible plug, as a result find, embodiment 5 it is swollen
The stability of swollen bolt is best, and spot, and portion occurs in the expansible plug surface of embodiment 1 and embodiment 3 and comparative example 3 batch
Expansible plug is divided slight crack occur.
By accelerated test and long term test, the mixture of sodium citrate and methyl hydroxybenzoate being capable of significantly improving
The stability of cosmetic expansible plug, lacks one of which composition, and stability declines.
The swell value of test example 3 determines
Method one
The cosmetics expansible plug 3 is taken, its afterbody sliver diameter is surveyed with slide measure, rolls about 90 ° and survey again once, often
Grain surveys 2 average value Ri for twice, obtaining every measure；By above-mentioned 3 bolts be used for melt become the time limit measure terminate after, take out immediately
Remaining sliver, the disconnected drop of water is treated, is gently placed on glass plate, the both ends of each sliver and middle three portions are determined with slide measure
Position, three positions is determined again after rolling about 90 °, each sliver obtains six data altogether, obtains 6 average value r of measurei, meter
Calculate the swell value P of everyi, the swell value of three bolts is all higher than 1.5.
The swell value such as table 1 of cosmetics expansible plug shows according to above-mentioned expansion values determination method determines embodiment 1-8；
The swell value of the embodiment 1-8 cosmetics expansible plugs of table 1
| Embodiment | Average diameter (mm) before expansion | Average diameter (mm) after expansion | Swell value (again) | As a result |
| Embodiment 1 | 11.84 | 20.74 | 1.75 | It is qualified |
| Embodiment 2 | 12.13 | 22.77 | 1.88 | It is qualified |
| Embodiment 3 | 12.08 | 21.58 | 1.79 | It is qualified |
| Embodiment 4 | 12.21 | 23.09 | 1.89 | It is qualified |
| Embodiment 5 | 11.78 | 21.32 | 1.81 | It is qualified |
| Embodiment 6 | 11.96 | 20.95 | 1.75 | It is qualified |
| Embodiment 7 | 12.26 | 23.31 | 1.90 | It is qualified |
| Embodiment 8 | 12.11 | 22.45 | 1.85 | It is qualified |
Method two
As shown in Figures 2 and 3：
1) values determination method is expanded：
A. tri- C 1, C2, C3 points first are chosen along the radial direction of the cosmetics expansible plug end face, institute is determined with slide measure
After initial length H1, H2, H3 for stating expandable carrier, then 90 ° of measurements are rolled, chosen along the radial direction of the cosmetics expansible plug end face
After tri- points of C1, C4, C5 determine initial length H4, H5, H6 of the expandable carrier with slide measure, H1, H2, H3, H4, H5 are asked
With H6 average value Hi；
B. the cosmetics expansible plug melt become time limit detection after, with slide measure measure C1 selected in a steps,
Length h1, h2, h3 after tri- opening position expandable carrier expansions of C2, C3；90 ° are rolled again, are determined with slide measure selected in a steps
The expansion of tri- opening position expandable carriers of C1, C4, C5 after length h4, h5, h6, seek h1, h2, h3, h4, h5 and h6 average length
Degree, average length hi after as expanding；
When c. calculating the swell value, calculated according to I formulas；
Wherein, pi represents that the swell value of axial direction, hi represent average length, the average initial length of Hi expressions after expansion；
Or, expansion values determination method：
D. tri- points of A1, A2 and A3 first are chosen along the axial direction of the cosmetics expansible plug in an angle, uses slide measure
After initial diameter R1, R2 and R3 for determining the expandable carrier, then 90 ° are rolled, chosen along the axial direction of the cosmetics expansible plug
Tri- points of B1, B2 and B3, after initial diameter R4, R5 and R6 that the expandable carrier is determined with slide measure, ask R1, R2, R3,
The average value Ri of six initial diameters of R4, R5 and R6；
E. the cosmetics expansible plug is carried out after melting the detection of change time limit, determines selected A1, A2 and A3 opening position in d steps
Expandable carrier expanded diameter is respectively r1, r2 and r3,；It is swollen that B1, B2 and B3 opening position selected in 90 ° of measurement d steps is rolled again
Swollen carrier expanded diameter is respectively r4, r5 and r6, seeks r1, r2, r3, r4, r5 and r6 average value, average diameter after must expanding
ri；
When f. calculating the swell value, calculated by II formulas；
Wherein, Pi represents that the swell value of radial direction, ri represent average diameter, the average initial diameter of Ri expressions after expansion.
The weight differential determination test of test example 4
The cosmetics expansible plug 10 is taken, accurately weighed weight, gently scrapes coat, must not lose sliver respectively, will
Sliver is placed in 60-70 DEG C of 300ml ethanol, and is cleaned 5 minutes in 80kHz frequency ultrasounds, makes the matrix of sliver surface residual
Dissolving removing, take out sliver and firmly extract, then inhaled 3 times with filter paper, dried 2 hours in 105 DEG C, taken out, room temperature is placed 1 hour
Afterwards, the accurately weighed sliver weight of difference, obtain every coating layer weight and averagely coat layer weight, every coating layer weight is with putting down
It is coated with layer weight to compare, 2 must not be more than beyond average coating layer weight ± 10%, and there must not be 1 overrun 1
Times.
Aforesaid operations, the cosmetics expansible plug described in detection embodiment 1-8 are repeated, its weight differential meets standard.
Irritation test of the cosmetics expansible plug of test example 5 to rabbit vagina mucous membrane
Rabbit 12 is taken, 3 groups is randomly divided into, every group 4, is divided into tested group 1, tested group 2 and control group；Described tested group
1 and the tested group 2 cosmetics expansible plug for giving embodiment 1 and embodiment 7 respectively, 1 time a day, successive administration 7 days, control group is given
Suppository made of common cosmetics is given, 1 time a day, successive administration 7 days；The general signs of fore-and-aft observing rabbit are administered daily,
Including appetite, hair color, whether there is abnormal secretion etc.；Each group is showed no obvious abnormalities phenomenon during administration；Last dose 24h takes out
Vagina tissue, for tested group 1 and tested group 2, visually observe smooth mucosal, no hyperemia, oedema, bleeding, ulcer and erosion etc.
Phenomenon, pathological examination mucous membrane structural integrity, no ulcer, inflammation and rotten to the corn formation；For control group, it is thicker to visually observe mucous membrane
It is rough, there are hyperemia, oedema, phenomenon, pathological examination mucous membrane structural integrity, but have ulcer and rotten to the corn formation；Show the change of the present invention
Cosmetic expansible plug is nonirritant to mucous membrane.
Claims (8)
1. a kind of cosmetics expansible plug, it is characterised in that the expansible plug includes cosmetics, matrix and expandable expansion and carried
Body；The cosmetics form coat with matrix, and are coated in expandable carrier surface, and the expandable carrier is after saturation water suction
Swell value is more than 1.1, and the parts by weight of each composition of expansible plug are：
Cosmetics 80-200
Matrix 80-200
Expandable carrier 50-400
The matrix is selected from fat-soluble matrix and/or water-soluble base；
The fat-soluble matrix is selected from mixed fatty glycerides, propylene glycol stearate, semi-synthetic fatty glyceride, hemizygous
Into cocounut oil ester, semi-synthetic palm grease, semi-synthetic fruit of a cubeb litsea tree ester, oleum sapii, spicebush oil, fennel fat, Ke Kemu fat, cocoa butter
Or the one or more in lanolin；
The water-soluble base is selected from polyethylene glycol 400, polyethylene glycol 1500, Macrogol 4000, Macrogol 6000, glycerine
One or more in gelatin, polysorbate60, polysorbate65, polyoxyl 40 stearate or poloxamer；The cosmetics include
Each composition of following parts by weight：
The isopropyl cetylate and propylene glycol diacetate form microballoon with microspherical carrier material.
2. cosmetics expansible plug as claimed in claim 1, it is characterised in that the microspherical carrier material is that ratio of weight and number is
3:1 chitin and the mixture of Arabic gum.
3. cosmetics expansible plug as claimed in claim 1, it is characterised in that the cosmetics are 0.2- also including parts by weight
1 part of sodium citrate and the methyl hydroxybenzoate of 0.1-0.3 parts.
4. the cosmetics expansible plug as described in claim 1-3 is any, it is characterised in that the expandable carrier is after saturation water suction
Swell value be more than 1.5, the swell value be radial direction swell value；The expandable carrier is sliver；The coat wraps in half
Enclose at front end 1/5-4/5 of the formula coated in the expandable carrier, the rear end of the expandable carrier is connected with bracing wire；The expandable carrier
After water suction, the maximum water absorption of every is not less than 1.5 milliliters.
5. the preparation method of cosmetics expansible plug as claimed in claim 3, it is characterised in that methods described includes following step
Suddenly：
1) preparation of coat：
A. matrix is placed in heat in water-bath and melted, be well mixed, fused mass is made；
B. the preparation of microballoon：
Isopropyl cetylate and propylene glycol diacetate are dispersed in absolute ethyl alcohol by I, and dispersion liquid is made；
II is by dispersion liquid magnetic stirring apparatus in 1000rmin-1, stir at 5 DEG C, suspension be made；
III adds microspherical carrier material in absolute ethyl alcohol, stirs, and oil phase is made；
IV adds suspension made from step II in oil phase made from step III, in 1000rmin-1, stir at 5 DEG C,
Spray drying, then with petroleum ether three times, drying at room temperature, the microballoon that particle size range is 15-25 μm is made；
C. methyl acrylate copolymer, polyvinyl alcohol-chitosan crosslinked thing and glycerine are well mixed, mixture is made；
D. mixture made from step c is well mixed with microballoon, sodium citrate and methyl hydroxybenzoate, cosmetics is made；
E. cosmetics made from step d are added in fused mass made from step a, be well mixed, coat is made；
2) coat is poured into bolt mould, inserts expandable carrier, cooling and shaping, expansible plug is made.
6. the detection method of the cosmetics expansible plug as described in claim 1-3 is any, it is characterised in that the detection method bag
Include following at least one method：
1) it is as follows to expand values determination method：
If a. choosing a little or doing along the radial direction of the cosmetics expansible plug end face, the initial length of the expandable carrier is determined
H；
B. after the cosmetics expansible plug saturation water suction, the length h after expandable carrier expands at selected location during a is walked is determined；
When c. calculating the swell value, calculated according to I formulas；
<mrow>
<mi>p</mi>
<mo>=</mo>
<mfrac>
<mi>h</mi>
<mi>H</mi>
</mfrac>
<mo>-</mo>
<mo>-</mo>
<mo>-</mo>
<mrow>
<mo>(</mo>
<mi>I</mi>
<mo>)</mo>
</mrow>
</mrow>
Wherein, p represents that the swell value of axial direction, h represent length, H expression initial lengths after expansion；
Or, expansion values determination method is as follows：
A. choose at one along the axial direction of the cosmetics expansible plug or some positions, determine the initial diameter R of the expandable carrier；
B. after cosmetics expansible plug saturation water suction, expandable carrier expanded diameter r at selected location is determined in a steps；
When c. calculating the swell value, calculated by II formulas；
<mrow>
<mi>P</mi>
<mo>=</mo>
<mfrac>
<mi>r</mi>
<mi>R</mi>
</mfrac>
<mo>-</mo>
<mo>-</mo>
<mo>-</mo>
<mrow>
<mo>(</mo>
<mi>I</mi>
<mi>I</mi>
<mo>)</mo>
</mrow>
</mrow>
Wherein, P represents that the swell value of radial direction, r represent that expanded diameter, R represent initial diameter；
2) weight differential assay method：
A. the cosmetics expansible plug is taken, weighs weight M；
B. the expandable carrier in the cosmetics expansible plug for scraping coat is taken, dries, weight m is weighed, according to such as formula III meter
Calculate the weight X of the coat：
X=M-m
(Ⅲ)。
7. the detection method of the cosmetics expansible plug as described in claim 1-3 is any, it is characterised in that the detection method bag
Include following at least one method：
1) it is as follows to expand values determination method：
If a. first choosing a little or doing along the radial direction of the cosmetics expansible plug end face, the initial length of the expandable carrier is determined
After spending H, then roll different angle measurement several times, average Hi；
B. the cosmetics expansible plug is carried out after melting the detection of change time limit, is determined after expandable carrier expands at selected location during a is walked
Length h；Different angle measurement is rolled again several times, seeks average length hi after expansion；
When c. calculating the swell value, calculated according to I-1 formulas；
<mrow>
<mi>p</mi>
<mi>i</mi>
<mo>=</mo>
<mfrac>
<mrow>
<mi>h</mi>
<mi>i</mi>
</mrow>
<mrow>
<mi>H</mi>
<mi>i</mi>
</mrow>
</mfrac>
<mo>-</mo>
<mo>-</mo>
<mo>-</mo>
<mrow>
<mo>(</mo>
<mi>I</mi>
<mo>-</mo>
<mn>1</mn>
<mo>)</mo>
</mrow>
</mrow>
Wherein, pi represents that the swell value of axial direction, hi represent average length, the average initial length of Hi expressions after expansion；
Or, expansion values determination method is as follows：
A. first an angle along the cosmetics expansible plug axial direction choose one at or some positions, determine the expandable carrier
Initial diameter R after, then roll different angle measurement several times, average Ri；
B. the cosmetics expansible plug is carried out after melting the detection of change time limit, is determined after expandable carrier expands at selected location during a is walked
Diameter r；Different angle measurement is rolled again several times, seeks average diameter ri after expansion；
When c. calculating the swell value, calculated by II-1 formulas；
<mrow>
<msub>
<mi>P</mi>
<mi>i</mi>
</msub>
<mo>=</mo>
<mfrac>
<mrow>
<mi>r</mi>
<mi>i</mi>
</mrow>
<mrow>
<mi>R</mi>
<mi>i</mi>
</mrow>
</mfrac>
<mo>-</mo>
<mo>-</mo>
<mo>-</mo>
<mrow>
<mo>(</mo>
<mrow>
<mi>I</mi>
<mi>I</mi>
<mo>-</mo>
<mn>1</mn>
</mrow>
<mo>)</mo>
</mrow>
</mrow>
Wherein, Pi represents that the swell value of radial direction, ri represent average diameter, the average initial diameter of Ri expressions after expansion；
2) weight differential assay method：
A. the cosmetics expansible plug is taken, weighs weight M；
B. coat is scraped, expandable carrier is placed in 20-90 DEG C of organic solvent, is taken out, in 50-150 DEG C of dry 1-10h, is claimed
Weight m is taken, according to the weight X of the coat as described in the calculating of III -1 formula
X=M-m (III -1)
Wherein, the organic solvent includes the one or more in ethanol, methanol or isopropanol.
8. the detection method of cosmetics expansible plug as claimed in claim 7, it is characterised in that the expandable carrier is sliver,
The detection method includes following at least one method：
1) values determination method is expanded：
The cosmetics expansible plug 3 is taken, its afterbody sliver diameter is surveyed with slide measure, rolls 90 ° and survey again once, every is surveyed two
It is secondary, obtain 2 average value Ri of every measure；By above-mentioned 3 bolts be used for melt become the time limit measure terminate after, take out remaining cotton immediately
Bar, the disconnected drop of water is treated, is gently placed on glass plate, the both ends of each sliver and middle three positions, rolling are determined with slide measure
Three positions are determined again after dynamic 90 °, and each sliver obtains six data altogether, obtains 6 average value r of measurei, calculate every
Swell value Pi, the swell value of three bolts should be greater than 1.5；
2) weight differential assay method：
The cosmetics expansible plug 10 is taken, accurately weighed weight, gently scrapes coat, must not lose sliver, by sliver respectively
It is placed in 50-80 DEG C of 200-400ml ethanol, and is cleaned 5 minutes in 80kHz frequency ultrasounds, makes the matrix of sliver surface residual
Dissolving removing, take out sliver and firmly extract, then inhaled 3 times with filter paper, dried 2 hours in 105 DEG C, taken out, room temperature is placed 1 hour
Afterwards, the accurately weighed sliver weight of difference, obtain every coating layer weight and averagely coat layer weight, every coating layer weight is with putting down
It is coated with layer weight to compare, 2 must not be more than beyond average coating layer weight ± 10%, and there must not be 1 overrun 1
Times.
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|---|---|---|---|---|
| CN102961260A (en) * | 2012-11-29 | 2013-03-13 | 哈尔滨欧替药业有限公司 | Expansion carrier bearing active components and application thereof |
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| CN103520339A (en) * | 2013-10-11 | 2014-01-22 | 哈尔滨欧替药业有限公司 | Funing expandable vaginal suppository, and preparation method and detection method thereof |
| CN103751096A (en) * | 2013-12-31 | 2014-04-30 | 哈尔滨欧替药业有限公司 | Carboprost methylate vaginal swelling suppository, as well as preparation method and detection method thereof |
-
2014
- 2014-11-06 CN CN201410620994.7A patent/CN104434545B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102961260A (en) * | 2012-11-29 | 2013-03-13 | 哈尔滨欧替药业有限公司 | Expansion carrier bearing active components and application thereof |
| CN103285055A (en) * | 2013-05-17 | 2013-09-11 | 哈尔滨欧替药业有限公司 | Compound metronidazole expansion suppository, preparation technology and detection method thereof |
| CN103520339A (en) * | 2013-10-11 | 2014-01-22 | 哈尔滨欧替药业有限公司 | Funing expandable vaginal suppository, and preparation method and detection method thereof |
| CN103751096A (en) * | 2013-12-31 | 2014-04-30 | 哈尔滨欧替药业有限公司 | Carboprost methylate vaginal swelling suppository, as well as preparation method and detection method thereof |
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| 丙烯酸酯类共聚物乳液的研究进展;张心亚等;《化学工业与工程》;20030430;第20卷(第2期);84-88、103 * |
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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 |