CN102373110A - Microcapsule sustained release agent and preparation method and application thereof - Google Patents
Microcapsule sustained release agent and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a microcapsule sustained release agent and a preparation method and application thereof. The microcapsule sustained release agent is prepared by embedding essence with gelatin and Arabic gum, and is applied to sanitary towels or sanitary cushions or panty-shape diapers or pet cushions. The microcapsule sustained release agent consists of a core material and a wall material, wherein the wall material consists of natural high molecular gelatin, Arabic gum and a curing agent; the core material consists of essence and essential oil; the curing agent consists of tannic acid and glutaraldehyde; and microencapsulation is performed on the core material and the wall material in the ratio 1:2. The invention further provides a preparation method of the microcapsule sustained release agent. The preparation method comprises the following steps of: adding an emulsifier into Arabic gum for mixing; adding essence or essential oil into an emulsion for homogenizing and emulsifying; adding a gelatin solution into the emulsified emulsion; agglomerating into a capsule; curing with a curing agent; and drying to obtain a high-dispersity microcapsule sustained release agent. By adding the microcapsule sustained release agent into the space between a skin contact layer and a water-absorbing layer of a sanitary towel or sanitary cushion or panty-shape diaper or pet cushion, the effect of keeping fragrance for a long time can be achieved.
Description
Technical field
The present invention relates to controlled release formulation of capsule, especially have the controlled release formulation of capsule that can be used for sanitary towel or sanitary pad or paper diaper or pet pads of fragrance.
Background technology
Along with expanding economy and growth in the living standard, very big variation has taken place to the requirement of sanitary product in people, transforms to enjoyment, health from the practical of past, and the sanitary towel perfuming has been complied with this trend.Because the fragrance sanitary towel has antibacterial expelling parasite, covering smell, makes effects such as body and mind is comfortable, thereby has obtained generally liking of people.
The sanitary towel perfuming is of long duration, and generally is with after the essence dilution but give the sanitary towel perfuming in the market, is sprayed directly on the sanitary towel surface; Because the volatility of essence is very strong, solvent also has certain volatility, causes the fragrance RT short; Wherein solvent can cause allergy to skin, stimulates.
Number of patent application is to mention the absorbing component that comprises spices in 200480043300.2 the one Chinese patent application, is that the spices district is set on sanitary towel, can select as required then whether spices discharges fragrance, but does not solve the problem that fragrance slowly discharges.
Wo93/09818 also discloses the absorbing component like dressings or sanitary towel and so on, and this absorbing component has the perfume layer that can be activated through the separate protection layer of dismantling.This application also is can select whether to discharge fragrance the solution people, but does not solve the short problem of essence fragrance remaining time.
Summary of the invention
The purpose of this invention is to provide controlled release formulation of capsule that a kind of gelatin and gum arabic wrap up essence or essential oil and preparation method thereof.
Another object of the present invention is with being used on sanitary towel or sanitary pad or paper diaper or the pet pads with controlled release formulation of capsule, making a kind of fragrance that has, and is antibacterial, and long sanitary towel or sanitary pad or paper diaper or the pet pads of fragrance remaining time.
The present invention presses mass ratio with core and wall material, and its component concentration is a core: the wall material is 1: 2.
Described core is essence or essential oil.
Described wall material is gelatin and gum arabic, and the amount ratio of gelatin and gum arabic is 1: 1.
Described gelatin is the natural polymer gelatin
A kind of preparation method of controlled release formulation of capsule comprises the preparation of wall material solution, the emulsification of core, and microcapsule liquid forms, the curing of microcapsule, five steps of the drying of microcapsule, wherein:
(a) preparation of wall material solution: it is the 1%-5% gelatin solution that gelatin is dissolved in the hot water preparation weight percent concentration, with the gumwater that gum arabic preparation weight percent concentration soluble in water is 1%-5%, subsequent use;
(b) emulsification of core: the adding emulsifier for mixing is even in gumwater, adds essence or essential oil again, and the mass ratio of essence or sesame oil and gum arabic is 1: 1, then mixed solution is become homogeneous latex emulsion with homogeneous machinery homogeneous;
(c) microcapsule liquid forms: will wait the gelatin of quality to join in the good emulsion of step (b) homogeneous, and under 20 ℃ of-60 ℃ of temperature, condense, and drip acetum and regulate pH value to 4-5; Reaction 0.5h-3h; Stop heating, make system temperature reduce to room temperature, microcapsule liquid forms;
(d) curing of microcapsule: add solidifying agent in the microcapsule liquid and solidify 0.5h-3h, regulating pH value is that 7-10 continues to stir 0.5h-3h, leaves standstill then and treats the microcapsule sedimentation;
(e) drying of microcapsule: the solution normal temperature of gained left standstill centrifugally obtain throw out or extraction filters filter cake, filter cake is immersed in the tannic acid solution 12 hours, suction filtration is washed with ethanol again, obtains controlled release formulation of capsule after the drying.
Described emulsifying agent is THIXCIN Soxylat A 25-7 or polyoxyethylene 20 sorbitan monolaurate.THIXCIN Soxylat A 25-7 name of product is CO40, and the polyoxyethylene 20 sorbitan monolaurate name of product is a polysorbas20.
Described solidifying agent is LUTARALDEHYDE or Weibull.
The essence of described controlled release formulation of capsule or the embedding rate of essential oil are 50%-90%, and drug loading is 10%-25%.
Controlled release formulation of capsule can be used for sanitary towel or sanitary pad or paper diaper or pet pads, at sanitary towel or sanitary pad or paper diaper or pet pads Time of Fluff Slurry sandwich layer position, adds according to the amount of every of 0.1-0.3g.Mix with polymer water-absorbent at sanitary towel or sanitary pad or paper diaper or pet pads top layer, add according to the amount of every of 0.1-0.3g.
The invention has the advantages that: the controlled release formulation of capsule that the present invention makes essence or essential oil embedding, selecting natural polymer gelatin, gum arabic for use is compound wall materials.The microcapsule wall material composition all is a natural polymer, does not contain harmful composition, and the operational path that is designed is simple, and mild condition is easy to realize.
It is solid-state that micro encapsulation not only makes essence be converted into from liquid state, improved the stability of essence, makes it be easy to store, transport and use.
It is applied on sanitary towel or sanitary pad or paper diaper or the pet pads has the following advantages: 1) natural polymer gelatin, gum arabic are non-stimulated to skin safe; 2) prevent the volatilization of essence behind the micro encapsulation, avoided essence to contact the influence of avoiding envrionment conditions during storage with the external world, improved the essence stability in storage.
Embodiment
Below in conjunction with specific embodiment the present invention is further specified.
Embodiment 1
Under the normal temperature 5g gelatin is dissolved in and is mixed with 2% solution in the hot water of 245ml; The 5g gum arabic is dissolved in is mixed with 4% the gum arabic aqueous solution in the 120ml water, in gumwater, add 2ml CO40 stirring and dissolving, add 5g essence; 3000rpm homogenizing emulsifying 15min adds the above-mentioned gelatin solution for preparing, 50 ℃ of cohesions in the good emulsion of emulsification; Dripping acetic acid accent pH value is 4.0, stirs 30min, stops heating; Make temperature reduce to room temperature, add 25% LUTARALDEHYDE 4ml and solidify 1h; Accent system pH value to 7 continue to stir 30min, stops then stirring, and sedimentation, suction filtration gets filter cake, filter cake is immersed in the tannic acid solution of 1% concentration 12 hours, and suction filtration is washed with ethanol again, obtains controlled release formulation of capsule after the drying.The embedding rate of essence is 80%, and drug loading is 20%.
Getting the controlled release formulation of capsule of instance 1 preparation verifies and the related check index as follows
1. the mensuration of embedding rate
In microcapsule embedded rate=microcapsule volatile oil content/volatile oil feed intake measure * 100%
Volatile oil content in microcapsule drug loading=microcapsule/microcapsule quality * 100%
1) pre-treatment of microcapsule
Take by weighing the 0.5g microcapsule, place the 500mL flask, add 85mL zero(ppm) water, add thermal distillation, receiving tube inserts and fills in the 100mL volumetric flask of 20mL50% (volume(tric)fraction) ethanol-water solution, distillation 3h.Be diluted to scale with ethanol-water solution, with its light absorption value of spectrophotometric determination, according to the oleaginousness of the typical curve calculation sample of having measured.
2) detection of microcapsule
The preparation of working curve
Reference liquid preparation: accurately take by weighing the 2.2g core; With after the small amount of ethanol dissolving, pour in the volumetric flask of 200ml, with 1/1 amass ratio aqueous ethanolic solution be diluted to scale; Shake up. get 4,2,1,0.5 and 0.25ml solution to 50ml, in the volumetric flask with the aqueous ethanolic solution constant volume of 1/1 volume ratio.
Preparation than toner: measure 85ml zero(ppm) water to the 1000ml beaker; Measure again that the 136ml vitriol oil is slow to add (1.6 volume concentrated acids/1 water by volume) in the entry; Constantly stir, ice bath cooling in case of necessity, accurately take by weighing again 1.00g right-dimethylaminobenzaldehyde adds in the brown volumetric flask of 200ml; With the sulphuric acid soln constant volume for preparing, it is subsequent use to shake up the dissolving back.
Normal concentration core solution is put into the 10ml test tube, adds 5ml and compares toner; Accurately heat 2min in the boiling water through shaking up to be placed on; Cool off 2min in the tap water then, being reference than toner+alcohol-water mixture, in 15min with the absorbancy of each reference liquid of spectrophotometric determination at the 550nm place; To the mapping of corresponding standard strength of solution, promptly get working curve by the absorbance of measuring.
Get the linear regression line equation of essence according to working curve: C=0.1579+0.0016 (correlation coefficient r
2=0.99)
Microcapsule essence content (mg.g
-1)=cv/w
C is a sample mass by the TV W that regression equation gets concentration V-extraction liquid in the formula
Sample core Determination on content
The pre-treatment of microcapsule
Take by weighing the 0.5g microcapsule, place the 500mL flask, add 85mL zero(ppm) water, add thermal distillation, receiving tube inserts and fills in the 100mL volumetric flask of 20mL 50% (volume(tric)fraction) ethanol-water solution, distillation 3h.Be diluted to scale with ethanol-water solution, get the 1ml distillate and put into the 10ml test tube, add 5ml, with its 550nm place light absorption value of spectrophotometric determination (by above-mentioned steps), according to the oleaginousness of the typical curve calculation sample of having measured than toner.
The data of measuring are following:
Sample | Absorbancy |
1# | 5.68 |
2# | 5.64 |
3# | 5.65 |
2. controlled release formulation of capsule makes an addition to long lasting quality that sanitary towel and essence directly is sprayed on sanitary towel relatively
The sanitary towel that has added controlled release formulation of capsule is placed indoor environmental condition (about 25 degree of temperature; Humidity 60%-85%) under; Measure essence content in the microcapsule at a distance from for some time, confirm that according to mensuration result after storing beginning and for some time microcapsule keep the ability of essence.(detection method is the same, uses ultraviolet spectrophotometer)
Table 1 microcapsule essence fragrance RT is measured
The sanitary towel that has sprayed essence is placed same environment, record following data with identical method
Table 2 essence fragrance RT is measured
Can find out through table 1, table 2; The essence rate of decay of the sanitary towel that the pure essence of process sprayed is very high; After 28 days placement naturally, essence is evaporated completely basically, and the sanitary towel of interpolation controlled release formulation of capsule is after placing for 24 weeks; Still have part essence to retain, explain and add the fragrance keeping period that controlled release formulation of capsule can prolong sanitary towel greatly.
3. acute skin irritation test
By the third party of Tianjin Center for Disease Control and Prevention authentication, and to carry out skin irritation reaction scoring by 2-11 in " detoxicating technical specifications " (version in 2002) skin irritation test and table 2-12 be non-stimulated with stimulus intensity judgement controlled release formulation of capsule to Japan large rabbit skin.
Embodiment 2
Under the normal temperature 5g natural polymer gelatin is dissolved in and is mixed with 4% solution in the hot water of 120ml; The 5g gum arabic is dissolved in is mixed with 2% the gum arabic aqueous solution in the 245ml water, in gumwater, add 2ml tween 20 stirring and dissolving, add 5g essence; 3000rpm homogenizing emulsifying 15min adds the above-mentioned natural polymer gelatin solution for preparing, 50 ℃ of cohesions in the good emulsion of emulsification; Transferring pH value is 4.0, stirs 30min, stops heating; Make temperature reduce to room temperature, add 25% LUTARALDEHYDE 4ml and solidify 1h; Accent system pH value to 7 continue to stir 30min, stops then stirring, and sedimentation, suction filtration gets filter cake, filter cake is immersed in the tannic acid solution of 1% concentration 12 hours, and suction filtration is washed with ethanol again, obtains microscapsule powder after the drying.The embedding rate of essence is 90%, and drug loading is 25%.
Embodiment 3
Under the normal temperature 5g gelatin is dissolved in and is mixed with 4% solution in the hot water of 120ml; The 5g gum arabic is dissolved in is mixed with 2% the gum arabic aqueous solution in the 245ml water, in gumwater, add 2ml CO40 stirring and dissolving, add 5g essence; 3000rpm homogenizing emulsifying 15min adds the above-mentioned gelatin solution for preparing, 50 ℃ of cohesions in the good emulsion of emulsification; Transferring pH value is 4.0, stirs 30min, stops heating; Make temperature reduce to room temperature, add 25% LUTARALDEHYDE 4ml and solidify 1h; Accent system pH value to 7 continue to stir 30min, stops then stirring, and sedimentation, suction filtration gets filter cake, filter cake is immersed in the tannic acid solution of 1% concentration 12 hours, and suction filtration is washed with ethanol again, obtains microscapsule powder after the drying.The embedding rate of essence is 50%, and drug loading is 10%.
Embodiment 4
Under the normal temperature 5g gelatin is dissolved in and is mixed with 5% solution in the hot water of 95ml; The 5g gum arabic is dissolved in is mixed with 1% the gum arabic aqueous solution in the 495ml water, in gumwater, add 2ml tween 20 stirring and dissolving, add 5g essence; 3000rpm homogenizing emulsifying 15min adds the above-mentioned gelatin solution for preparing, 50 ℃ of cohesions in the good emulsion of emulsification; Transferring pH value is 4.0, stirs 30min, stops heating; Make temperature reduce to room temperature, add 25% LUTARALDEHYDE 4ml and solidify 1h; Accent system pH value to 7 continue to stir 30min, stops then stirring, and sedimentation, suction filtration gets filter cake, filter cake is immersed in the tannic acid solution of 1% concentration 12 hours, and suction filtration is washed with ethanol again, obtains microscapsule powder after the drying.The embedding rate of essence is 50%, and drug loading is 10%.
Embodiment 5
Under the normal temperature 5g gelatin is dissolved in and is mixed with 1% solution in the hot water of 495ml; The 5g gum arabic is dissolved in is mixed with 5% the gum arabic aqueous solution in the 95ml water, in gumwater, add 2ml tween 20 stirring and dissolving, add 5g essence; 3000rpm homogenizing emulsifying 15min adds the above-mentioned gelatin solution for preparing, 50 ℃ of cohesions in the good emulsion of emulsification; Transferring pH value is 4.0, stirs 30min, stops heating; Make temperature reduce to room temperature, add 25% LUTARALDEHYDE 4ml and solidify 1h; Accent system pH value to 7 continue to stir 30min, stops then stirring, and sedimentation, suction filtration gets filter cake, filter cake is immersed in the tannic acid solution of 1% concentration 12 hours, and suction filtration is washed with ethanol again, obtains microscapsule powder after the drying.The embedding rate of essence is 50%, and drug loading is 10%.
Controlled release formulation of capsule of the present invention can be used to prepare the sanitary towel with champignon effect, sanitary pad, paper diaper, pet pads.Be added in process of production between skin-friendly layer and the water accepting layer, add, can mix interpolation, also can be added on the Time of Fluff Slurry sandwich layer separately with polymer water-absorbent according to the amount of every of 0.1-0.3g.Its characteristics are: at first, the inside that makes an addition to sanitary towel with form of powder is direct contacting skin, has avoided the stimulation of surface sprinkling to skin; Secondly in use, owing under the temperature and moisture of human body, particularly under the effect of menses, can make essence slowly continue to have guaranteed the homogeneous of use fragrance, and prolong fragrance remaining time to discharging.
The finished product of getting controlled release formulation of capsule carries out chromatogram ration analysis, and the 3-4 when proving common liq essence lasting doubly carries out the toxicity analytical test with the sanitary towel finished product that adds controlled release formulation of capsule, proves that human body is definitely had no stimulation.
Claims (10)
1. controlled release formulation of capsule, it is characterized in that: comprise core and wall material, press mass ratio, its component concentration is a core: the wall material is 1: 2.
2. a kind of controlled release formulation of capsule according to claim 1 is characterized in that: described core is essence or essential oil.
3. a kind of controlled release formulation of capsule according to claim 1 is characterized in that: described wall material is gelatin and gum arabic, and the amount ratio of gelatin and gum arabic is 1: 1.
4. gelatin according to claim 3 is the natural polymer gelatin.
5. the preparation method of a kind of controlled release formulation of capsule according to claim 1 is characterized in that: comprise the preparation of wall material solution, and the emulsification of core, microcapsule liquid forms, the curing of microcapsule, five steps of the drying of microcapsule, wherein:
(a) preparation of wall material solution: it is the 1%-5% gelatin solution that gelatin is dissolved in the hot water preparation weight percent concentration, with the gumwater that gum arabic preparation weight percent concentration soluble in water is 1%-5%, subsequent use;
(b) emulsification of core: the adding emulsifier for mixing is even in gumwater, adds essence or essential oil again, and the mass ratio of essence or sesame oil and gum arabic is 1: 1, then mixed solution is become homogeneous latex emulsion with homogeneous machinery homogeneous;
(c) microcapsule liquid forms: will wait the gelatin of quality to join in the good emulsion of step (b) homogeneous, and under 20 ℃ of-60 ℃ of temperature, condense, and drip acetum and regulate pH value to 4-5; Reaction 0.5h-3h; Stop heating, make system temperature reduce to room temperature, microcapsule liquid forms;
(d) curing of microcapsule: add solidifying agent in the microcapsule liquid and solidify 0.5h-3h, regulating pH value is that 7-10 continues to stir 0.5h-3h, leaves standstill then and treats the microcapsule sedimentation;
(e) drying of microcapsule: the solution normal temperature of gained left standstill centrifugally obtain throw out or extract filtrating obtaining filter cake, filter cake is immersed in the tannic acid solution 12 hours, suction filtration is washed with ethanol again, obtains controlled release formulation of capsule after the drying.
6. the preparation method of a kind of controlled release formulation of capsule according to claim 5, it is characterized in that: described emulsifying agent is THIXCIN Soxylat A 25-7 or polyoxyethylene 20 sorbitan monolaurate.
7. the preparation method of a kind of controlled release formulation of capsule according to claim 5, it is characterized in that: described solidifying agent is LUTARALDEHYDE or Weibull.
8. the preparation method of a kind of controlled release formulation of capsule according to claim 5, it is characterized in that: the essence of described controlled release formulation of capsule or the embedding rate of essential oil are 50%-90%, drug loading is 10%-25%.
9. a kind of controlled release formulation of capsule according to claim 1 is in the application of preparation sanitary towel or sanitary pad or paper diaper or pet pads.
10. a kind of controlled release formulation of capsule according to claim 8 is in the application of preparation sanitary towel or sanitary pad or paper diaper or pet pads; It is characterized in that: between sanitary towel or sanitary pad or paper diaper or pet pads skin-friendly layer and the water accepting layer, add according to the amount of every of 0.1-0.3g.
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