CN107998114A - Camphor peppermint willow ester emulsifiable paste and preparation method thereof - Google Patents
Camphor peppermint willow ester emulsifiable paste and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of camphor peppermint willow ester emulsifiable paste and preparation method thereof, it is related to field of medicaments.The camphor peppermint willow ester emulsifiable paste includes：The gaultherolin of 9 12 parts by weight, the menthol of 9 12 parts by weight, the camphor of 9 12 parts by weight, the water base auxiliary material of 13.5 17 parts by weight, the oil base auxiliary material of 14.5 18 parts by weight, the carbomer of 0.6 1 parts by weight, and 136 140 parts by weight water, its stability is high, and main ingredient component is evenly distributed in emulsifiable paste, stable quality, skin-penetrating raising, alleviation swelling, antipruritic, analgesic, antiinflammation are rapider.The preparation method of above-mentioned camphor peppermint willow ester emulsifiable paste, technique is simple and easy to control, suitable for commercial Application, while effectively improves stability and penetration.
Description
Technical field
The present invention relates to field of medicaments, and more particularly to a kind of camphor peppermint willow ester emulsifiable paste and preparation method thereof.
Background technology
Camphor peppermint willow ester emulsifiable paste, indication be for having a headache, it is dizzy, insect bite, mosquito sting, subside a swelling, relieve pain.Wherein, camphor,
Menthol, gaultherolin are skin irritant, can promote local blood circulation to alleviate swelling and have slight antipruritic, only
Bitterly, antiinflammation, compounding use, effectively improves action effect.
There are problems with for the camphor peppermint willow ester emulsifiable paste of the prior art：1st, absorptivity is relatively low, and wave is caused for bulk pharmaceutical chemicals
Take, 2, since this emulsifiable paste formed by water phase, oil phase and emulsifying agent, emulsifiable paste is easily unstable after placing for a long time, easily because of grease
Separate and emulsifiable paste is lost effectiveness；Main ingredient component skewness in emulsifiable paste, makes drug effect unstable.
The content of the invention
It is an object of the invention to provide a kind of camphor peppermint willow ester emulsifiable paste, its stability is high, and main ingredient component is in emulsifiable paste
It is evenly distributed, stable quality, skin-penetrating raising, alleviation swelling, antipruritic, analgesic, antiinflammation are rapider.
Another object of the present invention is to provide a kind of preparation method of camphor peppermint willow ester emulsifiable paste, technique is simple and easy to control
System, suitable for commercial Application, while effectively improves stability and penetration.
The present invention is solved its technical problem and is realized using following technical scheme.
The present invention proposes a kind of camphor peppermint willow ester emulsifiable paste, it includes：
The gaultherolin of 9-12 parts by weight, the menthol of 9-12 parts by weight, the camphor of 9-12 parts by weight, 13.5-17 weights
Measure the water base auxiliary material of part, the oil base auxiliary material of 14.5-18 parts by weight, the carbomer of 0.6-1 parts by weight, and 136-140 parts by weight
Water.
The present invention proposes a kind of preparation method of above-mentioned camphor peppermint willow ester emulsifiable paste, it includes：
Water base auxiliary material, carbomer and water are stirred in 20-30r/min, obtain water phase.
By oil base auxiliary material in 70-80 DEG C of mixing, 25-45min is kept the temperature, obtains oil phase.
By gaultherolin, menthol and camphor in 56-64 DEG C of mixing, main ingredient is obtained.
Water phase, oil phase are mixed in 68-75 DEG C, after first time homogeneous, mixed in 58-63 DEG C with main ingredient, second of homogeneous,
Stirring cooling.
The beneficial effect of the camphor peppermint willow ester emulsifiable paste of the embodiment of the present invention and preparation method thereof is：
Wherein, camphor, menthol, gaultherolin are skin irritant, to promote local blood circulation swollen to alleviate
Swollen and have slight antipruritic, analgesic, antiinflammation, compounding use, effectively improves action effect.Carbomer is bonded alkene for acrylic acid
The high molecular polymer of propyl group sucrose or pentaerythrite allyl ether.As gel-type vehicle, effectively make camphor peppermint willow ester emulsifiable paste
It is dispersed after lotion retrogradation, each material mixing, easy to smear, while the stability of oil phase and water phase is effectively facilitated, at the same time
Make that camphor peppermint willow ester emulsifiable paste is longer in the affected part residence time, and moisturizing is more preferably.
Its preparation method of above-mentioned camphor peppermint willow ester emulsifiable paste is simple and easy to control, suitable for commercial Application, effectively improves at the same time
Stability and penetration.
Embodiment
, below will be in the embodiment of the present invention to make the purpose, technical scheme and advantage of the embodiment of the present invention clearer
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, builds according to normal condition or manufacturer
The condition of view carries out.Reagents or instruments used without specified manufacturer, is the conventional production that can be obtained by commercially available purchase
Product.
Camphor peppermint willow ester emulsifiable paste of the embodiment of the present invention and preparation method thereof is specifically described below.
The present invention provides a kind of camphor peppermint willow ester emulsifiable paste, it includes：
The gaultherolin of 9-12 parts by weight, the menthol of 9-12 parts by weight, the camphor of 9-12 parts by weight, 13.5-17 weights
Measure the water base auxiliary material of part, the oil base auxiliary material of 14.5-18 parts by weight, the carbomer of 0.6-1 parts by weight, and 136-140 parts by weight
Water.
Preferably, camphor peppermint willow ester emulsifiable paste includes：The gaultherolin of 9-11 parts by weight, the peppermint of 10-11 parts by weight
Brain, the camphor of 9-11 parts by weight, the water base auxiliary material of 14-16 parts by weight, the oil base auxiliary material of 18-25 parts by weight, 0.8-1 parts by weight
Carbomer, and the water of 138-140 parts by weight.
It is highly preferred that camphor peppermint willow ester emulsifiable paste includes：The gaultherolin of 10-11 parts by weight, 10-11 parts by weight it is thin
Lotus brain, the camphor of 9-10 parts by weight, the water base auxiliary material of 15-17 parts by weight, the oil base auxiliary material of 19-26 parts by weight, 0.7-0.9 weight
The carbomer of part, and the water of 137-139 parts by weight.
Wherein, camphor, menthol, gaultherolin are skin irritant, to promote local blood circulation swollen to alleviate
Swollen and have slight antipruritic, analgesic, antiinflammation, compounding use, effectively improves action effect.
Carbomer is bonded the high molecular polymer of allyl sucrose or pentaerythrite allyl ether for acrylic acid.As gel base
Matter, effectively makes dispersed after the lotion retrogradation of camphor peppermint willow ester emulsifiable paste, each material mixing, easy to smear, while effectively promotees
Into oil phase and the stability of water phase, while make that camphor peppermint willow ester emulsifiable paste is longer in the affected part residence time, and moisturizing is more preferably.
Preferably, water base auxiliary material is followed successively by 0.015-0.025 including weight ratio：0.015-0.025：13-15：0.5-2's
Disodium ethylene diamine tetraacetate, ethyl hydroxy benzoate, sorbierite and triethanolamine.
Wherein, disodium ethylene diamine tetraacetate, is usually called EDTA, is a kind of organic compound, for increasing camphor peppermint
The chemicals of the stability of willow ester emulsifiable paste, have slow down reaction, keep chemical balance, reduce surface tension and prevent light,
The effect such as thermal decomposition or oxygenolysis.
On the one hand ethyl hydroxy benzoate coordinates with camphor, menthol, gaultherolin, carry out anti-inflammatory, on the other hand, has and suppresses
Fungi and the effect of bacterium, as bacteriostatic preservative, improve camphor peppermint willow ester emulsifiable paste antiseptic property, extend camphor peppermint willow
The shelf life of ester emulsifiable paste.
Sorbierite, by acting synergistically with disodium ethylene diamine tetraacetate, effectively improves antioxygenic property as antioxidant.
Sorbierite has good performance of keeping humidity, makes residence time of the lotion in affected part longer, drug effect absorptivity higher, while improves camphor tree
The institutional framework of brain peppermint willow ester emulsifiable paste, and reduce hardening dusting.
To sum up, acted synergistically by disodium ethylene diamine tetraacetate and sorbierite, effectively improve camphor peppermint willow ester emulsifiable paste
On the one hand inoxidizability, ethyl hydroxy benzoate further coordinate with camphor, menthol, gaultherolin, carry out anti-inflammatory, on the other hand,
Effective Shelf-life.
Oil base auxiliary material is followed successively by 6-8 including weight ratio：1-3：1.5-3：1.5-3：Stearic acid, the glycerol stearate of 1.5-3
Ester and polyethylene glycol stearate, peregal, octadecyl alcolol and hexadecanol.
Wherein, stearic addition, further stablizes the stability between water phase, oil phase and main ingredient, it is not easy point
Layer.
Tristerin and polyethylene glycol stearate are tristerin and (polyethylene glycol 100) stearate,
And peregal, tristerin, polyethylene glycol stearate and polysorbate are worked in coordination, oil base auxiliary material is effectively facilitated
It is uniformly mixed with water base auxiliary material, gaultherolin, menthol and camphor are uniformly scattered in oil base auxiliary material, water base auxiliary material, water
Mixture in, make effective component uniform, while under the conditions of aforementioned proportion, effectively prevent water phase and oil phase to be layered, further
The stability of drug effect is improved, it is rapidly and uniformly absorbed by the skin.
Due to providing cream, during in order to make camphor peppermint willow ester emulsifiable paste be coated on affected part, ensure the comfortable of affected part
Degree, and make the continual and steady release of drug effect, peregal has good wet performance, both effectively make camphor peppermint willow ester newborn
Cream is moistened skin when being coated on affected part, is made skin absorption preferable, is made the release that drug effect is continual and steady, while prevent coating position
Moisture evaporation stimulates affected part, causes itch to aggravate.
Hexadecanol, octadecyl alcolol and carbomer etc. cooperate with, collectively as the matrix of camphor peppermint willow ester emulsifiable paste.
By the cooperation of disodium ethylene diamine tetraacetate, ethyl hydroxy benzoate, sorbierite and triethanolamine etc., stabilization is effectively improved
Property and drug effect is played stably, avoid the waste of bulk pharmaceutical chemicals, and under the conditions of aforementioned proportion, functionalities.
Alternatively, oil base auxiliary material further includes 2.6- di-tert-butyl p-cresol, 2.6- di-tert-butyl p-cresol with it is stearic
Weight ratio is 0.01-0.03：6-8.
Cooperateing with for 2.6- di-tert-butyl p-cresol and disodium ethylene diamine tetraacetate and sorb sodium alkoxide, it is thin to effectively improve camphor
The inoxidizability of lotus willow ester emulsifiable paste, effectively improves the efficacy stability phase of camphor peppermint willow ester emulsifiable paste, and under the conditions of aforementioned proportion, makees
With optimization.
Alternatively, camphor peppermint willow ester emulsifiable paste further includes the dimethyl sulfoxide (DMSO) of 1-3 parts by weight, and 0.1-0.6 parts by weight
Natrium adetate.
Wherein, natrium adetate coordinates with sorbierite, and on the one hand collaboration promotes the antioxygenic property of sorbierite, improves camphor
The shelf-life of peppermint willow ester emulsifiable paste, on the other hand, natrium adetate are used to avoid when camphor peppermint willow ester emulsifiable paste is coated on affected part
When, it can also prevent bacterium from trace metal ion necessary to obtaining growth and development with the metal ion-chelant in affected part,
Collaboration promotes camphor, menthol, the effects of antiinflammation and bacteriostasis of gaultherolin.Peregal of natrium adetate collaboration at the same time etc. improves camphor tree
The moisturizing of brain peppermint willow ester emulsifiable paste.At the same time within the above range, have no adverse effects to human body or harmful effect is low, effectively facilitate
The stability of camphor peppermint willow ester emulsifiable paste.
Dimethyl sulfoxide (DMSO) is a kind of colourless liquid, is important polar non-solute, it can with many organic solvents and
Water dissolves each other, while dimethyl sulfoxide (DMSO) has the special nature of easily skin permeation, contributes to medicine to be permeated to human body, make camphor,
The active ingredient such as menthol, gaultherolin rapid osmotic is into human skin, while dimethyl sulfoxide (DMSO) has anti-inflammatory analgetic, town in itself
Wait quietly acting on, can further improve the drug effect of camphor peppermint willow ester emulsifiable paste, and dimethyl sulfoxide (DMSO) can also effectively improve camphor
The stability in cold environment of peppermint willow ester emulsifiable paste.
The present invention also provides a kind of preparation method of above-mentioned camphor peppermint willow ester emulsifiable paste, it includes：
S1. water base auxiliary material, carbomer and water are stirred in 20-30r/min, obtain water phase.
Water phase in-tank mixing is preferable over, it is simple and convenient.
Specifically, the blend step of water phase is as follows：
First water disodium ethylene diamine tetraacetate, ethyl hydroxy benzoate are mixed, carbomer is added under stirring, overnight, makes card
Ripple nurse fully expands dissolving.Then after filtering, for example, filtrate decompression can be transferred in emulsion tank, stirred in filtrate
Speed adds sorbierite, triethanolamine under conditions of being 20-30r/min, continues stirring after five minutes, is heated to 65-75 DEG C.
Alternatively, after being heated to 65-75 DEG C, stir speed (S.S.) be 20-25r/min under conditions of, with dimethyl sulfoxide (DMSO) with
And natrium adetate mixing.
S2. by oil base auxiliary material, such as in oil phase tank, in 70-80 DEG C of mixing, 25-45min is kept the temperature, obtains oil phase.
S3. gaultherolin, menthol and camphor are obtained into main ingredient in 56-64 DEG C of mixing.
S4. water phase, oil phase are mixed in 68-75 DEG C, after first time homogeneous, is mixed in 58-63 DEG C with main ingredient, second
Matter, stirring cooling.
Alternatively, in the filtrate decompression suction emulsion tank after oil phase is filtered, mutually mixed with water under the conditions of 28-35r/min
Close, for example, stirring 10min is sufficiently mixed it, the first time homogeneous 4-7min under conditions of 2300-2800r/min.
Alternatively, second of homogeneous carries out 2-4min under conditions of 2300-2800r/min.
Alternatively, 4-6min is stirred under conditions of 28-35r/min with main ingredient in 58-63 DEG C, is sufficiently mixed it.
Alternatively, dress, sealing are further included after S4 steps, specifically, Full automatic soft pipe conduit loading tail sealing machine is opened, then adjusts
It is no less than 20g/ branch to save loading amount；A loading quantity inspection (tare weight setting was carried out in pouring process every 20 minutes：By randomly selecting
5 empty aluminum pipes the weight for most weighing one subject to；5, sample is extracted every time, respectively accurately weighed weight), and record is performed,
If loading amount is undesirable, hard stop is answered to debug, until qualification can continue to produce；Filling certified products are completed to be taken
Sample, censorship, and certified products are transmitted to outer packing.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
A kind of camphor peppermint willow ester emulsifiable paste, it is made by following methods：
S1. water base auxiliary material, carbomer are mixed with water, is specially：First water disodium ethylene diamine tetraacetate, ethyl hydroxy benzoate are mixed
Close, carbomer is added under stirring, overnight, after filtering, added in filtrate under conditions of stir speed (S.S.) is 25r/min
Sorbierite, triethanolamine, continue stirring after five minutes, are heated to 65 DEG C.
Wherein, water base auxiliary material is followed successively by 0.015 including weight ratio：0.015：15：1.2 disodium ethylene diamine tetraacetate, hydroxyl
Phenethyl ester, sorbierite and triethanolamine.
S2. oil base auxiliary material is kept the temperature 28min, obtains oil phase in 74 DEG C of mixing.
Oil base auxiliary material is followed successively by 8 including weight ratio：3：3：3：2 stearic acid, tristerin and polyethylene glycol is stearic
Acid esters, peregal, octadecyl alcolol and hexadecanol.
S3. gaultherolin, menthol and camphor are obtained into main ingredient in 62 DEG C of mixing.
Wherein, camphor peppermint willow ester emulsifiable paste includes：The gaultherolin of 11 parts by weight, the menthol of 11 parts by weight, 12 weights
Measure the camphor of part, the water base auxiliary material of 15 parts by weight, the oil base auxiliary material of 17 parts by weight, the carbomer of 0.7 parts by weight, and 139 weights
Measure the water of part.
S4. in 70 DEG C, after oil phase is filtered in decompression suction emulsion tank, mutually stirred with water under conditions of 32r/min mixed
Close, the first time homogeneous 6min under conditions of 2500r/min.Then in 60 DEG C, 3.5min and master are stirred under conditions of 33r/min
Medicine mixes, second of homogeneous 4min under conditions of 2500r/min, and cooling is stirred under conditions of 25r/min, treats temperature in tank
When dropping to 30 DEG C, you can discharging.
Embodiment 2
A kind of camphor peppermint willow ester emulsifiable paste, it is made by following methods：
S1. water base auxiliary material, carbomer are mixed with water, is specially：First water disodium ethylene diamine tetraacetate, ethyl hydroxy benzoate are mixed
Close, carbomer is added under stirring, overnight, after filtering, added in filtrate under conditions of stir speed (S.S.) is 20r/min
Sorbierite, triethanolamine, continue stirring after five minutes, are heated to 68 DEG C.
Wherein, water base auxiliary material is followed successively by 0.02 including weight ratio：0.015：14：1.5 disodium ethylene diamine tetraacetate, oxybenzene
Ethyl ester, sorbierite and triethanolamine.
S2. oil base auxiliary material is kept the temperature 30min, obtains oil phase in 76 DEG C of mixing.
Oil base auxiliary material is followed successively by 7 including weight ratio：2：2：2.5：2.5 stearic acid, tristerin and polyethylene glycol
Stearate, peregal, octadecyl alcolol and hexadecanol.
S3. gaultherolin, menthol and camphor are obtained into main ingredient in 61 DEG C of mixing.
Wherein, camphor peppermint willow ester emulsifiable paste includes：The gaultherolin of 10 parts by weight, the menthol of 12 parts by weight, 9 weight
The camphor of part, the water base auxiliary material of 16 parts by weight, the oil base auxiliary material of 17 parts by weight, the carbomer of 0.6 parts by weight, and 137 weight
The water of part.
S4. in 69 DEG C, after oil phase is filtered in decompression suction emulsion tank, and water mutually mixing under conditions of 28r/min,
The first time homogeneous 5min under conditions of 2400r/min.Then in 61 DEG C, under conditions of 33r/min 4min is stirred to mix with main ingredient
Close, second of homogeneous 3min under conditions of 2600r/min, cooling is stirred under conditions of 25r/min, treats that temperature drops in tank
At 30 DEG C, you can discharging.
S5. Full automatic soft pipe conduit loading tail sealing machine is opened, it is no less than 20g/ branch then to adjust loading amount；In pouring process every
Carrying out within 20 minutes a loading quantity inspection, (tare weight is set：Subject to the weight for most weighing one by 5 randomly selected empty aluminum pipes；Often
Secondary 5, sample of extraction, the accurately weighed weight of difference), and record is performed, if loading amount is undesirable, answer hard stop to debug, directly
It can continue to produce to qualification；Complete filling certified products to be sampled, censorship, and certified products are transmitted to outer packing.
Embodiment 3
A kind of camphor peppermint willow ester emulsifiable paste, it is made by following methods：
S1. water base auxiliary material, carbomer are mixed with water, is specially：First water disodium ethylene diamine tetraacetate, ethyl hydroxy benzoate are mixed
Close, carbomer is added under stirring, overnight, after filtering, added in filtrate under conditions of stir speed (S.S.) is 28r/min
Sorbierite, triethanolamine, continue stirring after five minutes, are heated to 72 DEG C, under conditions of stir speed (S.S.) is 24r/min, with diformazan
Base sulfoxide and natrium adetate mixing.
Wherein, water base auxiliary material is followed successively by 0.023 including weight ratio：0.023：14：2 disodium ethylene diamine tetraacetate, oxybenzene
Ethyl ester, sorbierite and triethanolamine.
S2. oil base auxiliary material is kept the temperature 33min, obtains oil phase in 76 DEG C of mixing.
Oil base auxiliary material is followed successively by 7 including weight ratio：2.5：1.7：2：2 stearic acid, tristerin and polyethylene glycol
Stearate, peregal, octadecyl alcolol and hexadecanol.
S3. gaultherolin, menthol and camphor are obtained into main ingredient in 58 DEG C of mixing.
Wherein, camphor peppermint willow ester emulsifiable paste includes：The gaultherolin of 11 parts by weight, the menthol of 11 parts by weight, 11 weights
Measure the camphor of part, the water base auxiliary material of 16 parts by weight, the oil base auxiliary material of 15.5 parts by weight, the carbomer of 0.9 parts by weight, 2 parts by weight
Dimethyl sulfoxide (DMSO), the natrium adetate of 0.5 parts by weight, and the water of 140 parts by weight.
S4. in 72 DEG C, after oil phase is filtered in decompression suction emulsion tank, and water mutually mixing under conditions of 30r/min,
The first time homogeneous 7min under conditions of 2650r/min.Then in 60 DEG C, under conditions of 29r/min 6min is stirred to mix with main ingredient
Close, second of homogeneous 3min under conditions of 2800r/min, cooling is stirred under conditions of 25r/min, treats that temperature drops in tank
At 30 DEG C, you can discharging.
Embodiment 4
A kind of camphor peppermint willow ester emulsifiable paste, it is made by following methods：
S1. water base auxiliary material, carbomer are mixed with water, is specially：First water disodium ethylene diamine tetraacetate, ethyl hydroxy benzoate are mixed
Close, carbomer is added under stirring, overnight, after filtering, added in filtrate under conditions of stir speed (S.S.) is 25r/min
Sorbierite, triethanolamine, continue stirring after five minutes, are heated to 70 DEG C.
Wherein, water base auxiliary material is followed successively by 0.02 including weight ratio：0.02：14：1 disodium ethylene diamine tetraacetate, oxybenzene second
Ester, sorbierite and triethanolamine.
S2. oil base auxiliary material is kept the temperature 30min, obtains oil phase in 75 DEG C of mixing.
Oil base auxiliary material is followed successively by 7 including weight ratio：2：2：2：2：0.2 stearic acid, tristerin and polyethylene glycol
Stearate, peregal, octadecyl alcolol, hexadecanol and 2.6- di-t-butyls.
S3. gaultherolin, menthol and camphor are obtained into main ingredient in 60 DEG C of mixing.
Wherein, camphor peppermint willow ester emulsifiable paste includes：The gaultherolin of 10 parts by weight, the menthol of 10 parts by weight, 10 weights
The camphor of amount part, the water base auxiliary material of 15.04 parts by weight, the oil base auxiliary material of 15.2 parts by weight, the carbomer of 0.8 parts by weight, and
138.78 the water of parts by weight.
S4. it is mutually mixed under conditions of 30r/min with water after oil phase is filtered in decompression suction emulsion tank in 68-75 DEG C
Close 10min, the first time homogeneous 5min under conditions of 2500r/min.Then in 60 DEG C, 5min is stirred under conditions of 30r/min
Mixed with main ingredient, second of homogeneous 3min under conditions of 2500r/min, cooling is stirred under conditions of 25r/min, is treated in tank
When temperature drops to 30 DEG C, you can discharging.
S5. Full automatic soft pipe conduit loading tail sealing machine is opened, it is no less than 20g/ branch then to adjust loading amount；In pouring process every
Carrying out within 20 minutes a loading quantity inspection, (tare weight is set：Subject to the weight for most weighing one by 5 randomly selected empty aluminum pipes；Often
Secondary 5, sample of extraction, the accurately weighed weight of difference), and record is performed, if loading amount is undesirable, answer hard stop to debug, directly
It can continue to produce to qualification；Complete filling certified products to be sampled, censorship, and certified products are transmitted to outer packing.
Test example
Toxicological study is carried out to emulsifiable paste made from embodiment 4, result of study shows the camphor peppermint willow ester breast of the present invention
Cream is acted on without obvious stimulation and sensitization, without toxic side effect, clinical practice safety.
(1) emulsifiable paste made from is milky, microexamination, and emulsifiable paste emulsion droplet size is respectively less than 9 μm, is dispersed in emulsifiable paste base
In matter, 3000rpm is centrifuged 30 minutes, not stratified, be not demulsified.
(2) skin irritation and sensitization
Using itself androgynous left and right method of comparison, cavy 12.It is divided into two test groups：One blank group, every group of 6 globefish
Mouse, single cage raising.Any material is not smeared after blank group guinea pig back unhairing subregion.On the left of test group cavy unhairing area smear by
Thing cream 0.8g is tried, right side goes to hair-fields to smear bare substrate as control, after giving tested material 24h, removed and remained with warm water
Tested material, remove tested material 1,24,48,72h visually observe, record test block situations such as whetheing there is erythema and oedema, according to such as
Standards of grading shown in table 1 score and judge stimulus intensity and sensitization according to strength criterion.
1 skin irritatin of table and the standards of grading of allergy
2 skin irritatin intensity ratings standard of table
| Integral mean value | Evaluation is horizontal |
| 0-<0.5 | It is nonirritant |
| 0.5-<2 | Subexcite |
| 2-<6 | Moderate stimulation |
| 6-<8 | Strong and stimulating |
Average integral=∑ (erythema integration+oedema integration)/animal number.
Experiment shows, after continuously giving tested material 24h to cavy intact skin, removes remaining tested material with warm water, goes
It it is 0 point except score value is stimulated when tested material 1~72 is small；I.e. brain peppermint willow ester emulsifiable paste has no stimulation cavy intact skin.
Meanwhile through experiment, camphor peppermint willow ester emulsifiable paste group and excipient group are 0% to the sensitization rate of guinea pig skin, nothing
Sensitization.
(3) thermal cycling test
Experimental condition：Each group sample, is first placed in the fresh-keeping chamber of refrigerator made from embodiment 1-4,48 it is small when after take out and put
In 40 DEG C of baking oven 48 it is small when, circulation three times, after the test, sampling investigate, using commercially available camphor peppermint willow ester emulsifiable paste as pair
According to group, thermal cycling test is carried out using above-mentioned identical parameter, microexamination granularity, is investigated under the results are shown in Table 3：
3 result of the test of table
The result shows that the stabilization of each group sample made from embodiment 1-4 is better than commercially available camphor peppermint willow ester emulsifiable paste, embodiment
Each group emulsifiable paste property made from 1-4 is stablized, and crystallite size of the bulk pharmaceutical chemicals in emulsifiable paste is not substantially change, without crystal accumulation
Phenomenon.Control drug is after thermal cycling test, and obvious demulsification, water-oil separating phenomenon occurs in emulsifiable paste, and centrifugation layering is obvious, former
The crystal of material medicine substantially becomes larger, and the phenomenon of crystal accumulation occurs.
(4) accelerated test
Using embodiment 4 and commercially available camphor peppermint willow ester emulsifiable paste, two groups of samples are respectively placed in 30 ± 2 for control group
DEG C, relative humidity test 6 months under the conditions of being 65 ± 5%, respectively at sampling detection in 1,2,3,6 month, emphasis detected emulsifiable paste
Character, layering and microexamination granularity simultaneously measure principal component content.The results are shown in Table 4.
4 experimental result of table
As a result accelerated test 6 months, the character of medicine provided by the invention and microexamination have no significant change, centrifugation
Not stratified, packaging material appearance no abnormality seen, each master divides content without significant change.
At the same time using commercially available QUMIXIN emulsifiable paste as control group, accelerated test is carried out using above-mentioned identical parameter, the results showed that,
The stability of sample made from embodiment 4 is also superior to commercially available QUMIXIN emulsifiable paste.
The stability of embodiment 1-4 is followed successively by 4 ＞ embodiments of embodiment, 3 ＞ embodiments, 1 ＞ embodiments 2.Meanwhile the present invention carries
It is uniform that the camphor peppermint willow ester emulsifiable paste of confession is coated on surface, and fine and smooth, ductility is good, no feeling of grittiness.
To sum up, camphor peppermint willow ester emulsifiable paste provided in an embodiment of the present invention, its stability is high, and main ingredient component divides in emulsifiable paste
Cloth is uniform, stable quality, and skin-penetrating raising, anti-inflammatory, itching-relieving action are rapider.The preparation of above-mentioned camphor peppermint willow ester emulsifiable paste
Method, technique is simple and easy to control, suitable for commercial Application.
Embodiments described above is part of the embodiment of the present invention, instead of all the embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without creative efforts
Every other embodiment, belongs to the scope of protection of the invention.
Claims (10)
- A kind of 1. camphor peppermint willow ester emulsifiable paste, it is characterised in that including：The gaultherolin of 9-12 parts by weight, the menthol of 9-12 parts by weight, the camphor of 9-12 parts by weight, 13.5-17 parts by weight Water base auxiliary material, the oil base auxiliary material of 14.5-18 parts by weight, the carbomer of 0.6-1 parts by weight, and the water of 136-140 parts by weight.
- 2. camphor peppermint willow ester emulsifiable paste according to claim 1, it is characterised in that the water base auxiliary material include weight ratio according to Secondary is 0.015-0.025：0.015-0.025：13-15：The disodium ethylene diamine tetraacetate of 0.5-2, ethyl hydroxy benzoate, sorbierite and Triethanolamine.
- 3. camphor peppermint willow ester emulsifiable paste according to claim 1, it is characterised in that the oil base auxiliary material include weight ratio according to Secondary is 6-8：1-3：1.5-3：1.5-3：Stearic acid, tristerin and the polyethylene glycol stearate of 1.5-3, peregal, Octadecyl alcolol and hexadecanol.
- 4. camphor peppermint willow ester emulsifiable paste according to claim 3, it is characterised in that the oil base auxiliary material further includes 2.6- bis- Butylated Hydroxytoluene, the 2.6- di-tert-butyl p-cresol and the stearic weight ratio are 0.01-0.03：6-8.
- 5. according to claim 1-4 any one of them camphor peppermint willow ester emulsifiable pastes, it is characterised in that the camphor peppermint willow ester Emulsifiable paste further includes the dimethyl sulfoxide (DMSO) of 1-3 parts by weight, and the natrium adetate of 0.1-0.6 parts by weight.
- A kind of 6. preparation method of camphor peppermint willow ester emulsifiable paste as claimed in claim 1, it is characterised in that including：The water base auxiliary material, the carbomer and the water are stirred in 20-30r/min, obtain water phase；By the oil base auxiliary material in 70-80 DEG C of mixing, 25-45min is kept the temperature, obtains oil phase；By the gaultherolin, the menthol and the camphor in 56-64 DEG C of mixing, main ingredient is obtained；The water phase, the oil phase are mixed in 68-75 DEG C, after first time homogeneous, mixed in 58-63 DEG C with the main ingredient, the Second homogenate, stirring cooling.
- 7. preparation method according to claim 6, it is characterised in that the blend step of the water phase is as follows：First water, disodium ethylene diamine tetraacetate, ethyl hydroxy benzoate are mixed, the carbomer is added under stirring, overnight, filtering Afterwards, sorbierite, triethanolamine are added under conditions of stir speed (S.S.) is 20-30r/min in filtrate, continue stirring after five minutes, It is heated to 65-75 DEG C.
- 8. preparation method according to claim 7, it is characterised in that be 20- in stir speed (S.S.) after being heated to 65-75 DEG C Under conditions of 25r/min, mixed with dimethyl sulfoxide (DMSO) and natrium adetate.
- 9. preparation method according to claim 6, it is characterised in that after oil phase is filtered in decompression suction emulsion tank, with The water mutually under conditions of the 28-35r/min under conditions of mix, the first time homogeneous 4- under conditions of 2300-2800r/min 7min。
- 10. preparation method according to claim 6, it is characterised in that bar of second of homogeneous in 2300-2800r/min 2-4min is carried out under part.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110101709A (en) * | 2019-04-25 | 2019-08-09 | 广东人人康药业有限公司 | A kind of compound camphor emulsifiable paste and preparation method thereof |
| CN114392300A (en) * | 2022-03-04 | 2022-04-26 | 安徽华馨生物科技有限公司 | Traditional Chinese medicine extract composition for preparing analgesic ointment, preparation method and application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR930010580B1 (en) * | 1989-04-19 | 1993-10-30 | 주식회사 유한양행 | Creame preparations having a lange quantity of volatile components |
| CN103142697A (en) * | 2013-03-01 | 2013-06-12 | 福建美菰林生物科技有限公司 | Pharmaceutical composition for relieving muscular soreness and preparation method thereof |
| CN104042652A (en) * | 2014-06-21 | 2014-09-17 | 刘丰 | Special-effect heart tonic ointment |
-
2017
- 2017-12-26 CN CN201711430972.4A patent/CN107998114A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR930010580B1 (en) * | 1989-04-19 | 1993-10-30 | 주식회사 유한양행 | Creame preparations having a lange quantity of volatile components |
| CN103142697A (en) * | 2013-03-01 | 2013-06-12 | 福建美菰林生物科技有限公司 | Pharmaceutical composition for relieving muscular soreness and preparation method thereof |
| CN104042652A (en) * | 2014-06-21 | 2014-09-17 | 刘丰 | Special-effect heart tonic ointment |
Non-Patent Citations (2)
| Title |
|---|
| 孙涛 主编: "《家庭常用药物合理使用指南》", 31 October 2016, 吉林科学技术出版社 * |
| 宋小平 等: "《香料与食品添加剂制造技术》", 31 March 2000, 科学技术文献出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110101709A (en) * | 2019-04-25 | 2019-08-09 | 广东人人康药业有限公司 | A kind of compound camphor emulsifiable paste and preparation method thereof |
| CN110101709B (en) * | 2019-04-25 | 2022-05-17 | 广东人人康药业有限公司 | Compound camphor emulsifiable paste and preparation method thereof |
| CN114392300A (en) * | 2022-03-04 | 2022-04-26 | 安徽华馨生物科技有限公司 | Traditional Chinese medicine extract composition for preparing analgesic ointment, preparation method and application |
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Application publication date: 20180508 |