CN105147596B - Water-soluble supermolecule salicylic acid gel technology - Google Patents
Water-soluble supermolecule salicylic acid gel technology Download PDFInfo
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Abstract
The invention discloses a kind of new water-soluble supermolecule salicylic acid gels, it is by solution of salicylic acid and alcohol, nanometer starch crystal poloxamer suspension, α cyclodextrin aqueous solutions, after the mixing of low molecule Isin glue collagen aqueous solution, ultrasonic 3min obtains water-soluble supermolecule salicylic acid gel after standing 90min processing.It is made of several active ingredients, and each ingredient plays synergy, not only effectively plays the effect of salicylate treatment acne, also with unexpected transdermal efficient, stable dosage forms, the advantages such as heat-resisting.
Description
Technical field
The invention belongs to the preparing technical fields of supramolecular techniques field water soluble drug inclusion compound.
Background technology
Supramolecular chemistry is the chemistry for studying intermolecular interaction, and two or more molecules pass through intermolecular force knot
It closes and texturizes polymolecular entity so as to fulfill complicated height.Host molecule has special selectivity to guest molecule, and surpasses
The key of molecular chemistry is exactly the synthesis and application of host molecule.Successively there is three generations's oversubscription with the development of supramolecular chemistry
Subsystem, they are the supramolecular system based on crown ether, cyclodextrin and calixarenes respectively.This three generations's supramolecular system respectively has
Feature：First generation supramolecular system is can selectively complexing alkali metal ion, alkaline-earth metal ions using crown ether compound
Grow up with the peculiar property of primary amine salt；Cyclodextrin has interior hydrophobic, outer as second generation supermolecule main block compound
Hydrophilic cavity structure, alternative include most of aromatic compounds and aliphatic compound；The calixarenes of the third generation is
A kind of cyclic oligomer generated by the combined reaction of phenol and formaldehyde.This kind of compound molecule is adjustable hydrophobic with size
Cavity, selectivity is good, and energy and metal ion form super molecule inclusion compound with neutral organic molecule.
And representative of the cyclodextrin (Cyclodextrin, letter be CD) as second generation supermolecule main block molecule, usually by
A kind of cyclic oligosaccharide that 6,7,8 D- glucopyranose units are formed with а-Isosorbide-5-Nitrae bonding, it is cheap since its yield is high,
It is widely used.Cyclodextrin has the hydrophobic cavity of certain size, can selectively include a variety of organic guest molecules, so as to shape
Into super molecular compound.Its cavity structure can effectively include drug molecule and form inclusion compound, simultaneously because more outside cyclodextrin
The hydrophily of hydroxyl makes inclusion compound have good water solubility, so as to achieve the effect that insoluble drug solubilising.
Salicylic acid is a kind of fat-soluble organic acid.Poplar acid starting material includes kind for China and United States Pharmacopeia.At abroad, have
Close that there are many salicylic formulation products, and dosage form has：Gelling agent, ointment, patch, shampoo, lotion, detergent etc., specification (salicylic acid
Concentration) also there are many, be mainly used for treating acne, wart and seborrhea.Research shows its treatment to acne and blackhead
Effect is better than benzoyl peroxide；Salicylic acid Transdermal absorption influences from skin condition, is absorbed in hydrophily alcohol matrix best；1~
4% salicylic acid removal surface horny, more than 5% concentration can be used for going deep layer keratinization.According to《Clinical medicine is complete works of》,
The salicylate treatment acne of 0.5~2% concentration safely and effectively, is mainly used for mild to moderate acne, therefore Salicylic Acid Formulations are in state
It has been widely used outside.
At home, salicylic preparation has unguentum acidi salicylici, performs Ministry of Public Health's ministry standard 1989, to sterilize anti-corrosion
Medicine can dissolve cuticula.With reference to Chinese Pharmacopoeia version two in 2000《Clinical application notice》, salicylic acid is for acne vulgaris, fat
Property of overflowing dermatitis etc..
Salicylic acid and the active ingredient ratio of some other treatment acnes, have the following advantages：(1) high efficiency：Research
Show：The effect of salicylic acid is to acne and blackhead is better than benzoyl hydroperoxide；Salicylate treatment skin aging and remove wrinkle
Curative effect, hence it is evident that better than oxyacetic acid, and side effect is less than oxyacetic acid.(2) security is good：Research shows：It is local using 2% it is hydrophilic
Alcohol water solubility supermolecule salicylic acid gel not only absorbs well, but also no systemic side effect is used continuously.(3) have
Skin-care function：It such as goes to wrinkle and decolourize, for FDA it has been recommended that salicylic acid is used to go to wrinkle as OTC drugs, the salicylic acid of high concentration can
It is used safely in coloured skin：Such as pigmentation, black spot, skin is thick, and oiliness simultaneously has the decoloration of gross porosity and remission treatment.
It is contemplated that a kind of new water-soluble supermolecule salicylic acid gel of invention, is made of several active ingredients,
Each ingredient plays synergy, the effect of salicylate treatment acne is not only effectively played, also with unexpected transdermal efficiency
Height, stable dosage forms, the advantages such as heat-resisting.
The content of the invention
Technical problems based on background technology, the present invention for background technology there are the problem of, provide a kind of new
Water-soluble supermolecule salicylic acid gel, be made of several active ingredients, each ingredient plays synergy, not only effectively play
The effect of salicylate treatment acne, also with unexpected transdermal efficient, stable dosage forms, the advantages such as heat-resisting.
The purpose of the present invention is achieved through the following technical solutions：
A kind of new water-soluble supermolecule salicylic acid gel, is prepared by following methods：
Fraction as described below fraction meter by weight；
(1) solution of salicylic acid and alcohol is prepared：
It is molten that 1 part of salicylic acid is added in into alcohol liquid (mixed liquor of 95% ethyl alcohol of 10-12 parts and 25-32 parts of 1,2-PDs) stirring
Solution, obtains solution of salicylic acid and alcohol；
(2) nanometer starch crystal is prepared：
By 3-4 portions of tapiocas, 0.2-0.6 parts of acetate starch, 2-3 parts of cornstarch are scattered in 100 parts of 3.2M sulphur
In acid, then reacted under the conditions of 35 DEG C, 120rpm 3 days, then the Heat thermostability 50s at 60 DEG C, is made suspension；
The suspension is made nanometer starch crystal suspension, is freeze-dried ingredient by washing and centrifuging repeatedly to neutrality
After obtain nanometer starch crystal；
(3) nanometer starch crystal poloxamer suspension is prepared：
4 parts of nanometer starch crystal is taken, it is 13000 to sequentially add 50-80 parts of molecular weight, and the content of polyethylene glycol oxide is 81%
Poloxamer, 120-130 parts of molecular weight are 6200, and the content of polyethylene glycol oxide is 78% poloxamer, deionized water 500
Part simultaneously stirs evenly, and nanometer starch crystal aaerosol solution is made；
(4) the alpha-cyclodextrin aqueous solution of 200mg/mL mass percent concentrations is prepared；
(5) low molecule Isin glue collagen aqueous solution is prepared：
The low molecule Isin glue collagen that molecular weight is taken to be 800-1000, is prepared into saturated aqueous solution；
(6) by solution of salicylic acid and alcohol, the aaerosol solution of nanometer starch crystal and alpha-cyclodextrin aqueous solution, Isin glue collagen are water-soluble
Liquid mixes, at this time salicylic acid, and nanometer starch crystal, mass concentration of the Isin glue collagen in mixed aqueous solution is respectively 2wt%,
0.03wt%, 0.05-0.08wt% ultrasound 3min obtain water-soluble supermolecule salicylic acid gel after standing 90min.
The supersound process refers to：It is 180w in ultrasonic output power, ultrasound is divided in the environment of output frequency is 40kHz
It dissipates.
The technology point of water solubility supermolecule salicylic acid gel of the invention is mainly：1. prepare nanometer starch crystal, optimization
The recipe ingredient of starch, and after mild temperature reaction, heat shock at relatively high temperatures；2. prepare nanometer starch crystal poloxamer
During suspension, two kinds of poloxamers are sequentially added；3. add micro Isin glue collagen etc..The technique totally carries out excellent
Change, after synergistic effect, water solubility supermolecule salicylic acid gel obtained not only good water solubility effectively plays salicylate treatment acne
Effect, also with unexpected transdermal efficient, stable dosage forms, the advantages such as heat-resisting.
The invention has the beneficial effects that：
1. pair skin irritation is extremely low, the therapeutic effect of acne is good.
2. phase transdermal absorption factor is high.
3. performance is stablized, at 40 ± 2 DEG C, under the conditions of RH75% ± 5%, and accelerated test 8 months, water-soluble supermolecule bigcatkin willow
The quality of acid gel does not have significant change.
4. human experimentation proves, the unexpected mass effect for improving acne of the optimization of multifactor lower technique, and
Also there is significant facilitation on transdermal absorption factor.
5. this method also has, preparation process is simple and convenient, and product quality is stablized, and scale industrial production facility etc. is beneficial
Effect.
Specific embodiment
Embodiment 1：
The raw material of the present invention is commercially available is commercially available.
New water-soluble supermolecule salicylic acid gel, is prepared by following methods：
Fraction as described below fraction meter by weight；
(1) solution of salicylic acid and alcohol is prepared：
1 part of salicylic acid is added in into alcohol liquid (mixed liquor of 10 part of 95% ethyl alcohol and 32 parts of 1,2-PDs) stirring and dissolving, is obtained
Solution of salicylic acid and alcohol；
(2) nanometer starch crystal is prepared：
By 3 portions of tapiocas, 0.2 part of acetate starch, 3 parts of cornstarch are scattered in 100 parts of 3.2M sulfuric acid, so
It is reacted under the conditions of 35 DEG C, 120rpm 3 days, then the Heat thermostability 50s at 60 DEG C, is made suspension；
The suspension is made nanometer starch crystal suspension, is freeze-dried ingredient by washing and centrifuging repeatedly to neutrality
After obtain nanometer starch crystal；
(3) nanometer starch crystal poloxamer suspension is prepared：
4 parts of nanometer starch crystal is taken, it is 13000 to sequentially add 50 parts of molecular weight, and the content of polyethylene glycol oxide is 81% pool
Luo Shamu, 130 parts of molecular weight is 6200, and the content of polyethylene glycol oxide is 78% poloxamer, and 500 parts of deionized water is simultaneously stirred
It mixes uniformly, nanometer starch crystal aaerosol solution is made；
(4) the alpha-cyclodextrin aqueous solution of 200mg/mL mass percent concentrations is prepared；
(5) low molecule Isin glue collagen aqueous solution is prepared：
The low molecule Isin glue collagen that molecular weight is taken to be 800, is prepared into saturated aqueous solution；
(6) by solution of salicylic acid and alcohol, the aaerosol solution of nanometer starch crystal and alpha-cyclodextrin aqueous solution, Isin glue collagen are water-soluble
Liquid mixes, at this time salicylic acid, and nanometer starch crystal, mass concentration of the Isin glue collagen in mixed aqueous solution is respectively 2wt%,
0.03wt%, 0.08wt% ultrasound 3min obtain water-soluble supermolecule salicylic acid gel after standing 90min.
The supersound process refers to：It is 180w in ultrasonic output power, ultrasound is divided in the environment of output frequency is 40kHz
It dissipates.
Embodiment 2：
New water-soluble supermolecule salicylic acid gel, is prepared by following methods：
Fraction as described below fraction meter by weight；
(1) solution of salicylic acid and alcohol is prepared：
1 part of salicylic acid is added in into alcohol liquid (mixed liquor of 12 part of 95% ethyl alcohol and 25 parts of 1,2-PDs) stirring and dissolving, is obtained
Solution of salicylic acid and alcohol；
(2) nanometer starch crystal is prepared：
By 4 portions of tapiocas, 0.6 part of acetate starch, 2 parts of cornstarch are scattered in 100 parts of 3.2M sulfuric acid, so
It is reacted under the conditions of 35 DEG C, 120rpm 3 days, then the Heat thermostability 50s at 60 DEG C, is made suspension；
The suspension is made nanometer starch crystal suspension, is freeze-dried ingredient by washing and centrifuging repeatedly to neutrality
After obtain nanometer starch crystal；
(3) nanometer starch crystal poloxamer suspension is prepared：
4 parts of nanometer starch crystal is taken, it is 13000 to sequentially add 80 parts of molecular weight, and the content of polyethylene glycol oxide is 81% pool
Luo Shamu, 120 parts of molecular weight is 6200, and the content of polyethylene glycol oxide is 78% poloxamer, and 500 parts of deionized water is simultaneously stirred
It mixes uniformly, nanometer starch crystal aaerosol solution is made；
(4) the alpha-cyclodextrin aqueous solution of 200mg/mL mass percent concentrations is prepared；
(5) low molecule Isin glue collagen aqueous solution is prepared：
The low molecule Isin glue collagen that molecular weight is taken to be 1000, is prepared into saturated aqueous solution；
(6) by solution of salicylic acid and alcohol, the aaerosol solution of nanometer starch crystal and alpha-cyclodextrin aqueous solution, Isin glue collagen are water-soluble
Liquid mixes, at this time salicylic acid, and nanometer starch crystal, mass concentration of the Isin glue collagen in mixed aqueous solution is respectively 2wt%,
0.03wt%, 0.05wt% ultrasound 3min obtain water-soluble supermolecule salicylic acid gel after standing 90min.
The supersound process refers to：It is 180w in ultrasonic output power, ultrasound is divided in the environment of output frequency is 40kHz
It dissipates.
Embodiment 3：
New water-soluble supermolecule salicylic acid gel, is prepared by following methods：
Fraction as described below fraction meter by weight；
(1) solution of salicylic acid and alcohol is prepared：
1 part of salicylic acid is added in into alcohol liquid (mixed liquor of 11 part of 95% ethyl alcohol and 30 parts of 1,2-PDs) stirring and dissolving, is obtained
Solution of salicylic acid and alcohol；
(2) nanometer starch crystal is prepared：
By 3 portions of tapiocas, 0.3 part of acetate starch, 3 parts of cornstarch are scattered in 100 parts of 3.2M sulfuric acid, so
It is reacted under the conditions of 35 DEG C, 120rpm 3 days, then the Heat thermostability 50s at 60 DEG C, is made suspension；
The suspension is made nanometer starch crystal suspension, is freeze-dried ingredient by washing and centrifuging repeatedly to neutrality
After obtain nanometer starch crystal；
(3) nanometer starch crystal poloxamer suspension is prepared：
4 parts of nanometer starch crystal is taken, it is 13000 to sequentially add 60 parts of molecular weight, and the content of polyethylene glycol oxide is 81% pool
Luo Shamu, 125 parts of molecular weight is 6200, and the content of polyethylene glycol oxide is 78% poloxamer, and 500 parts of deionized water is simultaneously stirred
It mixes uniformly, nanometer starch crystal aaerosol solution is made；
(4) the alpha-cyclodextrin aqueous solution of 200mg/mL mass percent concentrations is prepared；
(5) low molecule Isin glue collagen aqueous solution is prepared：
The low molecule Isin glue collagen that molecular weight is taken to be 900, is prepared into saturated aqueous solution；
(6) by solution of salicylic acid and alcohol, the aaerosol solution of nanometer starch crystal and alpha-cyclodextrin aqueous solution, Isin glue collagen are water-soluble
Liquid mixes, at this time salicylic acid, and nanometer starch crystal, mass concentration of the Isin glue collagen in mixed aqueous solution is respectively 2wt%,
0.03wt%, 0.07wt% ultrasound 3min obtain water-soluble supermolecule salicylic acid gel after standing 90min.
The supersound process refers to：It is 180w in ultrasonic output power, ultrasound is divided in the environment of output frequency is 40kHz
It dissipates.
Embodiment 4：
New water-soluble supermolecule salicylic acid gel, is prepared by following methods：
Fraction as described below fraction meter by weight；
(1) solution of salicylic acid and alcohol is prepared：
1 part of salicylic acid is added in into alcohol liquid (mixed liquor of 10 part of 95% ethyl alcohol and 27 parts of 1,2-PDs) stirring and dissolving, is obtained
Solution of salicylic acid and alcohol；
(2) nanometer starch crystal is prepared：
By 4 portions of tapiocas, 0.5 part of acetate starch, 2 parts of cornstarch are scattered in 100 parts of 3.2M sulfuric acid, so
It is reacted under the conditions of 35 DEG C, 120rpm 3 days, then the Heat thermostability 50s at 60 DEG C, is made suspension；
The suspension is made nanometer starch crystal suspension, is freeze-dried ingredient by washing and centrifuging repeatedly to neutrality
After obtain nanometer starch crystal；
(3) nanometer starch crystal poloxamer suspension is prepared：
4 parts of nanometer starch crystal is taken, it is 13000 to sequentially add 70 parts of molecular weight, and the content of polyethylene glycol oxide is 81% pool
Luo Shamu, 121 parts of molecular weight is 6200, and the content of polyethylene glycol oxide is 78% poloxamer, and 500 parts of deionized water is simultaneously stirred
It mixes uniformly, nanometer starch crystal aaerosol solution is made；
(4) the alpha-cyclodextrin aqueous solution of 200mg/mL mass percent concentrations is prepared；
(5) low molecule Isin glue collagen aqueous solution is prepared：
The low molecule Isin glue collagen that molecular weight is taken to be 800, is prepared into saturated aqueous solution；
(6) by solution of salicylic acid and alcohol, the aaerosol solution of nanometer starch crystal and alpha-cyclodextrin aqueous solution, Isin glue collagen are water-soluble
Liquid mixes, at this time salicylic acid, and nanometer starch crystal, mass concentration of the Isin glue collagen in mixed aqueous solution is respectively 2wt%,
0.03wt%, 0.06wt% ultrasound 3min obtain water-soluble supermolecule salicylic acid gel after standing 90min.
The supersound process refers to：It is 180w in ultrasonic output power, ultrasound is divided in the environment of output frequency is 40kHz
It dissipates.
Embodiment 5：
New water-soluble supermolecule salicylic acid gel, is prepared by following methods：
Fraction as described below fraction meter by weight；
(1) solution of salicylic acid and alcohol is prepared：
1 part of salicylic acid is added in into alcohol liquid (mixed liquor of 12 part of 95% ethyl alcohol and 31 parts of 1,2-PDs) stirring and dissolving, is obtained
Solution of salicylic acid and alcohol；
(2) nanometer starch crystal is prepared：
By 3 portions of tapiocas, 0.4 part of acetate starch, 3 parts of cornstarch are scattered in 100 parts of 3.2M sulfuric acid, so
It is reacted under the conditions of 35 DEG C, 120rpm 3 days, then the Heat thermostability 50s at 60 DEG C, is made suspension；
The suspension is made nanometer starch crystal suspension, is freeze-dried ingredient by washing and centrifuging repeatedly to neutrality
After obtain nanometer starch crystal；
(3) nanometer starch crystal poloxamer suspension is prepared：
4 parts of nanometer starch crystal is taken, it is 13000 to sequentially add 53 parts of molecular weight, and the content of polyethylene glycol oxide is 81% pool
Luo Shamu, 129 parts of molecular weight is 6200, and the content of polyethylene glycol oxide is 78% poloxamer, and 500 parts of deionized water is simultaneously stirred
It mixes uniformly, nanometer starch crystal aaerosol solution is made；
(4) the alpha-cyclodextrin aqueous solution of 200mg/mL mass percent concentrations is prepared；
(5) low molecule Isin glue collagen aqueous solution is prepared：
The low molecule Isin glue collagen that molecular weight is taken to be 900, is prepared into saturated aqueous solution；
(6) by solution of salicylic acid and alcohol, the aaerosol solution of nanometer starch crystal and alpha-cyclodextrin aqueous solution, Isin glue collagen are water-soluble
Liquid mixes, at this time salicylic acid, and nanometer starch crystal, mass concentration of the Isin glue collagen in mixed aqueous solution is respectively 2wt%,
0.03wt%, 0.08wt% ultrasound 3min obtain water-soluble supermolecule salicylic acid gel after standing 90min.
The supersound process refers to：It is 180w in ultrasonic output power, ultrasound is divided in the environment of output frequency is 40kHz
It dissipates.
Embodiment 6：
Comparative example of the present invention be it is exemplary enumerate, in fact, from the time of heat shock, the formula of starch, poloxamer
Property, many factors such as the source of collagen and molecular weight selection are all most important, and slight change is all difficult to reach the present invention
Effect.
Comparative example 1：Without Heat thermostability：
New water-soluble supermolecule salicylic acid gel, is prepared by following methods：
Fraction as described below fraction meter by weight；
(1) solution of salicylic acid and alcohol is prepared：
1 part of salicylic acid is added in into alcohol liquid (mixed liquor of 11 part of 95% ethyl alcohol and 26 parts of 1,2-PDs) stirring and dissolving, is obtained
Solution of salicylic acid and alcohol；
(2) nanometer starch crystal is prepared：
By 3 portions of tapiocas, 0.2 part of acetate starch, 2 parts of cornstarch are scattered in 100 parts of 3.2M sulfuric acid, so
3 days obtained suspension is reacted under the conditions of 35 DEG C, 120rpm；
The suspension is made nanometer starch crystal suspension, is freeze-dried ingredient by washing and centrifuging repeatedly to neutrality
After obtain nanometer starch crystal；
(3) nanometer starch crystal poloxamer suspension is prepared：
4 parts of nanometer starch crystal is taken, it is 13000 to sequentially add 77 parts of molecular weight, and the content of polyethylene glycol oxide is 81% pool
Luo Shamu, 123 parts of molecular weight is 6200, and the content of polyethylene glycol oxide is 78% poloxamer, and 500 parts of deionized water is simultaneously stirred
It mixes uniformly, nanometer starch crystal aaerosol solution is made；
(4) the alpha-cyclodextrin aqueous solution of 200mg/mL mass percent concentrations is prepared；
(5) low molecule Isin glue collagen aqueous solution is prepared：
The low molecule Isin glue collagen that molecular weight is taken to be 888, is prepared into saturated aqueous solution；
(6) by solution of salicylic acid and alcohol, the aaerosol solution of nanometer starch crystal and alpha-cyclodextrin aqueous solution, Isin glue collagen are water-soluble
Liquid mixes, at this time salicylic acid, and nanometer starch crystal, mass concentration of the Isin glue collagen in mixed aqueous solution is respectively 2wt%,
0.03wt%, 0.05wt% ultrasound 3min obtain water-soluble supermolecule salicylic acid gel after standing 90min.
The supersound process refers to：It is 180w in ultrasonic output power, ultrasound is divided in the environment of output frequency is 40kHz
It dissipates.
Comparative example 2：Active ingredient is not added with Isin glue collagen：
New water-soluble supermolecule salicylic acid gel, is prepared by following methods：
Fraction as described below fraction meter by weight；
(1) solution of salicylic acid and alcohol is prepared：
1 part of salicylic acid is added in into alcohol liquid (mixed liquor of 10 part of 95% ethyl alcohol and 28 parts of 1,2-PDs) stirring and dissolving, is obtained
Solution of salicylic acid and alcohol；
(2) nanometer starch crystal is prepared：
By 4 portions of tapiocas, 0.6 part of acetate starch, 3 parts of cornstarch are scattered in 100 parts of 3.2M sulfuric acid, so
It is reacted under the conditions of 35 DEG C, 120rpm 3 days, then the Heat thermostability 50s at 60 DEG C, is made suspension；
The suspension is made nanometer starch crystal suspension, is freeze-dried ingredient by washing and centrifuging repeatedly to neutrality
After obtain nanometer starch crystal；
(3) nanometer starch crystal poloxamer suspension is prepared：
4 parts of nanometer starch crystal is taken, it is 13000 to sequentially add 66 parts of molecular weight, and the content of polyethylene glycol oxide is 81% pool
Luo Shamu, 127 parts of molecular weight is 6200, and the content of polyethylene glycol oxide is 78% poloxamer, and 500 parts of deionized water is simultaneously stirred
It mixes uniformly, nanometer starch crystal aaerosol solution is made；
(4) the alpha-cyclodextrin aqueous solution of 200mg/mL mass percent concentrations is prepared；
(5) by solution of salicylic acid and alcohol, the aaerosol solution of nanometer starch crystal and alpha-cyclodextrin aqueous solution, Isin glue collagen are water-soluble
Liquid mixes, at this time salicylic acid, and nanometer starch crystal, mass concentration of the Isin glue collagen in mixed aqueous solution is respectively 2wt%,
0.03wt%, 0.07wt% ultrasound 3min obtain water-soluble supermolecule salicylic acid gel after standing 90min.
The supersound process refers to：It is 180w in ultrasonic output power, ultrasound is divided in the environment of output frequency is 40kHz
It dissipates.
(1) transdermal absorption factor：
Water-soluble supermolecule salicylic acid gel prepared by the present invention carries out mouse percutaneous penetration, experiment instrument used
Device is the vertical Transdermal diffusion cells of Franz, and the structure of vertical Transdermal diffusion cell includes supply chamber, delivery system, receiving chamber and sampling
Mouthful.Wherein, supply chamber is for placing laboratory sample, and receiving chamber is equipped with receiving liquid, and receiving liquid is water, and receiving chamber bottom is provided with magnetic
Power blender.
Carry out mouse percutaneous penetration before, first by mouse break neck put to death, immediately after with electric hair cutter remove mouse back
Hair, clip mouse back skin, and remove the subcutaneus adipose tissue of mouse back skin, and after being rinsed well with clear water,
The mouse back skin for removing subcutaneus adipose tissue is placed in physiological saline, refrigeration is spare.
Mouse percutaneous penetration is carried out to above-mentioned 7 kinds water-soluble supermolecule salicylic acid gels respectively, through calculating after experiment,
In 7 kinds of water-soluble supermolecule salicylic acid gels, the salicylic acid Transdermal absorption amount of embodiment 5 is significantly higher than comparative example, respectively
It is 1.3 times and 2.1 times of comparative example 1 and comparative example 2.
(2) stability test：
It is tested through influence factor, preliminary proof water solubility supermolecule salicylic acid gel is to light and high temperature (60 DEG C) and low temperature base
This stabilization；Accelerated experiment investigation, water-soluble supermolecule salicylic acid gel is at 40 ± 2 DEG C, under the conditions of RH75% ± 5%, accelerates
Experiment 8 months, the quality of water-soluble supermolecule salicylic acid gel does not have significant change；Water-soluble supermolecule salicylic acid gel is upper
Under city's terms of packing, long term test is investigated 24 months, and product quality is stablized.If it is packed with composite soft tube, and at 40 ± 2 DEG C,
Accelerated test is done under the conditions of RH75% ± 5% and investigates 8 months, the investigation of long-term stable experiment, water-soluble supermolecule salicylic acid
The quality of gel does not change significantly.
According to every stability test as a result, and the characteristics of dosage form, prescription, determining that preservation condition is：Sealing, in cool place
Place preserves；The term of validity is fixed tentatively 3 years.
And the stability of comparative example 1 and 2 is significantly worse than the embodiment of the present invention, and at 40 ± 2 DEG C, ± 5% conditions of RH75%
Under, it is preserved under accelerated test, started to be layered respectively at 1 month and 3 months.
(3) Journal of Sex Research is stimulated：
Experiment tests the irritation of guinea pig skin with regard to water-soluble supermolecule salicylic acid gel, the results showed that：Globefish
Mouse normal skin and damaged skin were once applied with continuous 7 days with after water-soluble supermolecule salicylic acid gel, had no skin irritation
Reaction shows that water-soluble supermolecule salicylic acid gel reacts skin without obvious irritation.
Experiment has carried out allergic reaction on guinea pigs to water-soluble supermolecule salicylic acid gel, the results showed that：Cavy is local
Repeated multiple times apply of skin has no allergic reaction with after water-soluble supermolecule salicylic acid gel.
(4) Clinical practice effect：
The effect of 2% water-soluble supermolecule salicylic acid gel treatment acne vulgaris prepared to embodiment 3 and security into
Clinical test is gone.Each embodiment selects 100 satisfactory subjects to participate in this experiment.Treat each experimental group
The equal no difference of science of statistics of severity at age, gender and the state of an illness, shown in the following form of result of the test：
Conclusion：The 2% salicylic acid supermolecular gel of the present invention treats light, moderate acne based on acne safely, effectively,
The probability that especially furfur occurs is substantially less than control group.The especially formula of embodiment 1, quick, high efficiency are bad anti-
It should lack.
Above-mentioned description of test, new water-soluble supermolecule salicylic acid gel of the invention, by several active ingredients group
Into each ingredient plays synergy, the effect of salicylate treatment acne is not only effectively played, also with unexpected transdermal effect
Rate is high, the advantages such as stable dosage forms are heat-resisting, and adverse reaction rate is low.It also found in the experiment in later stage, compared with comparative example 1-
2, the formula of embodiment 2 also has the unexpected significantly higher effect lightened the stain.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (3)
1. a kind of new water-soluble supermolecule salicylic acid gel, is prepared by following methods：
Number as described below is counted in parts by weight；
(1) solution of salicylic acid and alcohol is prepared：
1 part of salicylic acid is added in into alcohol liquid stirring and dissolving, obtains solution of salicylic acid and alcohol；The alcohol liquid is 95% ethyl alcohol of 10-12 parts and 25-
The mixed liquor of 32 parts of 1,2-PDs；
(2) nanometer starch crystal is prepared：
By 3-4 portions of tapiocas, 0.2-0.6 parts of acetate starch, 2-3 parts of cornstarch are scattered in 100 parts of 3.2M sulfuric acid
In, it is then reacted under the conditions of 35 DEG C, 120rpm 3 days, then the Heat thermostability 50s at 60 DEG C, is made suspension；
The suspension is made nanometer starch crystal suspension, is obtained after being freeze-dried ingredient by washing and centrifuging repeatedly to neutrality
To nanometer starch crystal；
(3) nanometer starch crystal poloxamer suspension is prepared：
4 parts of nanometer starch crystal is taken, it is 13000 to sequentially add 50-80 parts of molecular weight, and the pool Lip river that polyoxyethylated content is 81% is husky
Nurse, 120-130 parts of molecular weight is 6200, and polyoxyethylated content is 78% poloxamer, and 500 parts of deionized water simultaneously stirs
Uniformly, nanometer starch crystal poloxamer suspension is made；
(4) the alpha-cyclodextrin aqueous solution of 200mg/mL mass percent concentrations is prepared；
(5) low molecule Isin glue collagen aqueous solution is prepared：
The low molecule Isin glue collagen that molecular weight is taken to be 800-1000, is prepared into saturated aqueous solution；
(6) by solution of salicylic acid and alcohol, nanometer starch crystal poloxamer suspension and alpha-cyclodextrin aqueous solution, Isin glue collagen are water-soluble
Liquid mixes, at this time salicylic acid, and nanometer starch crystal, mass concentration of the Isin glue collagen in mixed aqueous solution is respectively 2wt%,
0.03wt%, 0.05-0.08wt%, ultrasonic 3min obtain water-soluble supermolecule salicylic acid gel after standing 90min.
2. water solubility supermolecule salicylic acid gel as described in claim 1, it is characterised in that：
The supersound process refers to：It is 180w in ultrasonic output power, output frequency is ultrasonic disperse in the environment of 40kHz.
3. water solubility supermolecule salicylic acid gel as claimed in claim 1 or 2, it is characterised in that：
(1) solution of salicylic acid and alcohol is prepared：
1 part of salicylic acid is added in into alcohol liquid (mixed liquor of 10 part of 95% ethyl alcohol and 32 parts of 1,2-PDs) stirring and dissolving, obtains bigcatkin willow
Acid alcohol solution；The alcohol liquid is 10 part of 95% ethyl alcohol and the mixed liquor of 32 parts of 1,2-PDs；
(2) nanometer starch crystal is prepared：
By 3 portions of tapiocas, 0.2 part of acetate starch, 3 parts of cornstarch are scattered in 100 parts of 3.2M sulfuric acid, Ran Houyu
35 DEG C, react under the conditions of 120rpm 3 days, then the Heat thermostability 50s at 60 DEG C, is made suspension；
The suspension is made nanometer starch crystal suspension, is obtained after being freeze-dried ingredient by washing and centrifuging repeatedly to neutrality
To nanometer starch crystal；
(3) nanometer starch crystal poloxamer suspension is prepared：
4 parts of nanometer starch crystal is taken, it is 13000 to sequentially add 50 parts of molecular weight, and polyoxyethylated content is 81% poloxamer,
130 parts of molecular weight is 6200, and polyoxyethylated content is 78% poloxamer, and 500 parts of deionized water simultaneously stirs evenly, and is made
Into nanometer starch crystal poloxamer suspension；
(4) the alpha-cyclodextrin aqueous solution of 200mg/mL mass percent concentrations is prepared；
(5) low molecule Isin glue collagen aqueous solution is prepared：
The low molecule Isin glue collagen that molecular weight is taken to be 800, is prepared into saturated aqueous solution；
(6) by solution of salicylic acid and alcohol, nanometer starch crystal poloxamer suspension and alpha-cyclodextrin aqueous solution, Isin glue collagen are water-soluble
Liquid mixes, at this time salicylic acid, and nanometer starch crystal, mass concentration of the Isin glue collagen in mixed aqueous solution is respectively 2wt%,
0.03wt%, 0.08wt% ultrasound 3min obtain water-soluble supermolecule salicylic acid gel after standing 90min.
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| CN1502677A (en) * | 2002-11-27 | 2004-06-09 | 西北工业大学 | Beta-cyclodextrin supermolecular complex electro-rheological fluid and its preparation process |
| WO2009145982A1 (en) * | 2008-04-01 | 2009-12-03 | Antipodean Pharmaceuticals, Inc. | Compositions and methods for skin care |
| CN101608029A (en) * | 2009-07-09 | 2009-12-23 | 上海纳米技术及应用国家工程研究中心有限公司 | Polysaccharide nanoparticle composite supramolecular aquagel and preparation method |
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| CN1502677A (en) * | 2002-11-27 | 2004-06-09 | 西北工业大学 | Beta-cyclodextrin supermolecular complex electro-rheological fluid and its preparation process |
| WO2009145982A1 (en) * | 2008-04-01 | 2009-12-03 | Antipodean Pharmaceuticals, Inc. | Compositions and methods for skin care |
| CN101608029A (en) * | 2009-07-09 | 2009-12-23 | 上海纳米技术及应用国家工程研究中心有限公司 | Polysaccharide nanoparticle composite supramolecular aquagel and preparation method |
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| α-环糊精/水杨酸等包络物的NMR 自扩散研究;彭敏等;《波谱学杂志》;20050630;第22卷(第2期);141-147页 * |
| 正交设计法优选水杨酸β-环糊精的包合工艺;徐勤等;《实用药物与临床》;20101231;第13卷(第4期);第264-265页 * |
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