CN101239052B - Method for preparing sodium alginate/ chitosan sustained-release microcapsule by external gelation - Google Patents
Method for preparing sodium alginate/ chitosan sustained-release microcapsule by external gelation Download PDFInfo
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- CN101239052B CN101239052B CN2008100601120A CN200810060112A CN101239052B CN 101239052 B CN101239052 B CN 101239052B CN 2008100601120 A CN2008100601120 A CN 2008100601120A CN 200810060112 A CN200810060112 A CN 200810060112A CN 101239052 B CN101239052 B CN 101239052B
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Abstract
The invention discloses a method for emulsionizing outer gelation and preparing sodium alginate/chitosan slow release micro-capsule in one step. The current preparation method of calcium alginate gel by internal gelation has defects that small parts of the calcium salt granules cannot be richly reacted with glacial acetic acid and remained in the sodium alginate calcium beads, the encapsulization materials are easily lost and the wrapping rate is low due to the calcium salt is difficult to evenly disperse. The invention uses the sodium alginate liquor as the disperse phase, the edible plant oil as the disperse medium and the sorbitan monooleate as the surfactant to emulsionize small liquid drops wrapped with oil; calcium chloride chitosan liquor is used for initiating the gelation reaction of the sodium alginate so as to generate sodium alginate/chitosan slow release micro-capsule; the oil remained on the surface is eliminated by a oil removing device with precipitation self-drifting method. The invention elevates the micro-capsule medicine contents and the wrapping rate.
Description
Technical field
The invention discloses the method that the outside gelation of one-step method emulsifying prepares the alginate slow-releasing microcapsule.
Background technology
The alginate slow-releasing microcapsule has excellent biological compatibility and mechanical strength, be a good Atrigel, be widely used in various aspects such as medicine controlled release carrier, gene delivery vehicle, immune buffer action and artificial organ, cell culture microreactor, the depollution of environment.The preparation method of alginate slow-releasing microcapsule mainly contains nebulization and emulsion process two big classes at present.Nebulization mainly adopts coaxial air jet system and static titration appratus, the particle diameter of the microcapsule of this method preparation is big, microcapsule ball-type degree and fineness are relatively poor, the slow-releasing microcapsule particle diameter is subjected to the restriction of syringe needle internal diameter and solution viscosity, microcapsule dropwise prepares, and the equipment complexity is difficult to large-scale production.The patent No. is that 01109449.4 Chinese patent discloses the method that a kind of emulsifying/internal gelation prepares calcium alginate gel beads, it adopts with sodium alginate and insoluble calcium salts is decentralized photo, liquid paraffin is a disperse medium, the anhydrous sorbitol Triolein is a surfactant, with the glacial acetic acid is the emulsification system of gel initiator, carries out the emulsifying/internal gelation reaction.This method preparation process complexity because calcium salt is difficult to be uniformly dispersed, has fraction calcium salt granule to fail fully to react with glacial acetic acid and remains in the sodium alginate calcium pearl, and the microencapsulation material easily runs off, and causes envelop rate to reduce.Calcium bead surface liquid paraffin is difficult for removing fully, the inclusion in can a large amount of loss slow-releasing microcapsules in cleaning process, influences the activity of inclusion.In addition, take paraffin for a long time and can cause the human body osteoporosis, the twenties in 20th century, liquid paraffin, once was widely used as filler medically, and lasting many decades, easily caused paraffinoma until generally reporting this material, just stopped using.So use paraffin very improper as disperse medium.Adopting said method will obtain the sodium alginate chitosan particle also needs calcium alginate plastic beads once more with the chitosan solution reaction, makes preparation process further complicated.Therefore, improving entrapment efficiency and preparation stability is problem demanding prompt solution in the sodium alginate chitosan sustained-release preparation research.
In addition, remove the method for slow-releasing microcapsule remained on surface fluid at present and use organic solvent or surfactant mostly, this method is difficult to remove fully slow-releasing microcapsule remained on surface fluid, and the inclusion in can a large amount of loss slow-releasing microcapsules or influence the activity of inclusion.
Summary of the invention
Technical problem to be solved by this invention is to overcome the defective that above-mentioned prior art exists, provide the outside gelation of one-step method emulsifying to prepare the method for alginate slow-releasing microcapsule fast, with raising microcapsule medicament content and envelop rate, and make the microcapsule surface not have fluid substantially.
For this reason, the present invention adopts following technical scheme: outside gelation prepares the method for alginate slow-releasing microcapsule, it is characterized in that with the sodium alginate soln being decentralized photo, edible vegetable oil is disperse medium, anhydrous sorbitol list olein (span 80) is a surfactant, through being emulsified into water in oil small-sized drop, cause the gelation reaction of sodium alginate soln with the calcium chloride chitosan solution, generate the alginate slow-releasing microcapsule, the residual fluid on its surface adopts precipitation to remove from the drift method by a degreaser.The present invention adopts new dispersion, surfactant, with the method for the outside gelation of emulsifying, prepares that the ball-type degree is good, output is high, surface smoothness is high, the slow-releasing microcapsule of narrow diameter distribution; Adopt degreaser physics to deoil, avoided the use of organic substance, reduced the loss of the loss, particularly contained medicine of microcapsule material in the preparation process, improved microcapsule medicament content and envelop rate.
Above-mentioned outside gelation prepares the method for alginate slow-releasing microcapsule, with mass concentration is that the sodium alginate soln of 0.5%-3% is distributed to meter by volume and contains in the edible vegetable oil of anhydrous sorbitol list olein of 0.5%-2%, and water oil phase volume ratio is 1: 3-1: between 8; Water in oil small-sized drop realizes that by motor stirring system rotating speed of motor is 100r/min-1500r/min, and emulsification times is 10-30 minute.
Above-mentioned degreaser comprises the pond of deoiling that is provided with from inside to outside, sedimentation tank and oil sump, be provided with a Rotational Cylindrical and a lever that is coupling on the pond inwall that deoils in the described pond of deoiling and rock assembly, Rotational Cylindrical is outer to coat the brush that deoils, Rotational Cylindrical is made by light material (as POM polyformaldehyde plastic-steel), lever rocks assembly and comprises and rock an oil-collecting plate and a connecting rod, an end that rocks oil-collecting plate is a power end, the other end is non-power end, the middle part of rocking oil-collecting plate is coupling on the pond inwall that deoils, described non-power end connects the adjustable floater shot of a gravity, the middle part of rocking oil-collecting plate is coupling on the pond inwall that deoils, the outlet of one feed tube is positioned at the top of rocking the oil-collecting plate power end, the outer end of connecting rod is connected on the Rotational Cylindrical, and a waste liquid discharge pipe is housed on the oil sump.The brush that deoils is made by soft coarse material (as through fibers such as the polyamide of processing such as acidic group sulfonic group, phosphate etc. and salt, polyvinyl alcohol, vinylon), can not damage microcapsule.
Above-mentioned degreaser, the exit of feed tube are equipped with the nozzle side by side of adjustable angle, control the direction of current by the angle of adjusting nozzle.
Above-mentioned degreaser; the power end that rocks oil-collecting plate is a semicircle light material plate (as the corrosion-resistant shock-resistant high-strength aluminium alloy plate of acid and alkali-resistance); remainder is network structure; weave with coarse material (as through fibers such as the polyamide of processing such as acidic group sulfonic group, phosphate etc. and salt, polyvinyl alcohol, vinylon) and to form, to alleviate the resistance of water oil-collecting plate.
Above-mentioned degreaser, the pond of deoiling, sedimentation tank and oil sump height reduce step by step, and the outward flange on sedimentation tank top is equipped with filter screen, liquid can pass through smoothly, solid then can not pass through, and is used to stop microcapsule and makes its precipitation, changes filter screen according to the actual needs.
Above-mentioned degreaser, the bottom in the pond of deoiling are equipped with once collects valve, and a main valve of collecting is equipped with in the bottom of sedimentation tank; Deoil and a feed hopper is housed on the pond, the below of this feed hopper is positioned at the place, lateral wall of Rotational Cylindrical.
Above-mentioned degreaser, Rotational Cylindrical are positioned at a side in the pond of deoiling, and the adjustable floater shot of gravity is positioned at the opposite side in the pond of deoiling; Deoil and ultrasonic probe is housed in the pond, the top that it is positioned at Rotational Cylindrical makes more thorough that the fluid on microcapsule surface removes.Rotational Cylindrical is a hollow structure, can reduce friction to rotate more flexibly, can also use external drive power source where necessary.
The present invention simplifies preparation process by the existing emulsification method of improvement, prepares that the ball-type degree is good, output is high, surface smoothness is high, the alginate slow-releasing microcapsule of narrow diameter distribution, is easy to suitability for industrialized production; Avoid the use of organic substance in the process of deoiling, reduced the loss of the loss, particularly contained medicine of microencapsulation material in the preparation process, improved microcapsule medicament content and envelop rate; Thoroughly removed the residual fluid on slow-releasing microcapsule surface, it is easy to deoil; In addition, can also control the size of microcapsule diameter, prepare the alginate slow-releasing microcapsule of different-grain diameter, satisfy actual needs by regulating motor speed.
The present invention is further illustrated below in conjunction with specification drawings and specific embodiments.
Description of drawings
Fig. 1-2 is the structural representation of degreaser of the present invention.
Fig. 3 is for rocking the structural representation of oil-collecting plate among Fig. 1-2.
Among the figure, the 1～pond of deoiling, 2～sedimentation tank, 3～oil sump, 4～Rotational Cylindrical, the 5～brush that deoils, 6～rock oil-collecting plate, 7～connecting rod, 8～turning cylinder, 9～non-power end, the adjustable floater shot of 10～gravity, 11～feed tube, 12～nozzle, 13～power end arranged more, 14～waste liquid discharge pipe, 15～filter screen, 16～inferior collection valve, 17～main valve, 18～feed hopper, the 19～ultrasonic probe collected.
The specific embodiment
Amycin (mass concentration is 1.5%) sodium alginate (mass concentration is 1.5%) normal saline solution 100ml is distributed among the edible vegetable oil 500ml that contains 0.5% span 80, regulates motor speed and stirred 15 minutes to 400r/min.Chitosan (deacetylation is 95.3%) the solution 500ml of the calcium chloride 0.5% of adding 1% causes the sodium alginate gel reaction, continues to stir after 30 minutes, adopts to precipitate by degreaser and thoroughly removes the fluid on slow-releasing microcapsule surface from the drift method.Collect, natural drying obtains amycin sodium alginate chitosan sustained-release microcapsule.According to 2005 editions appendix VA of the Pharmacopoeia of the People's Republic of China (appendix 28) UV-VIS spectrophotometry, measure the drug loading of amycin in the amycin alginate slow-releasing microcapsule in the 481nm place, the content that records amycin in the amycin alginate slow-releasing microcapsule is 31.2%-35.7%, envelop rate is 66.3%-70.4%, observe for 15 * 10 times at ordinary optical microscope, residual fluid is not seen on the slow-releasing microcapsule surface.
The comparative example 1
Adopt the described preparation method of Chinese patent No. 01109449.4,, add calcium carbonate granule 1.5g and mix into uniform suspension amycin (mass concentration is 1.5%) sodium alginate (mass concentration is 1.5%) normal saline solution 100ml.This suspension is distributed among the liquid paraffin 500ml that contains 0.5% span 85, regulates motor speed and stirred 15 minutes to 400r/min.Add glacial acetic acid 10ml, reduction system pH value dissociates calcium carbonate and discharges calcium ion, initiated gel reaction.Continue to stir after 30 minutes, add 1% calcium chloride solution 500ml and make the sedimentation of glue pearl, clean prepared amycin calcium alginate gel beads with screen filtration and with the 1%Tween80 aqueous solution.The amycin calcium alginate gel beads was put into 0.5% chitosan (deacetylation is 95.3%) solution reaction 5 minutes.Collect, natural drying obtains amycin alginate slow-releasing microcapsule.According to 2005 editions appendix VA of the Pharmacopoeia of the People's Republic of China (appendix 28) UV-VIS spectrophotometry, measure the drug loading of amycin in the amycin sodium alginate chitosan sustained-release microcapsule in the 481nm place, the content that records amycin in the amycin alginate slow-releasing microcapsule is 17.1%-22.4%, envelop rate is 34.5%-39.9%, observe the visible obvious residual fluid in slow-releasing microcapsule surface for 15 * 10 times at ordinary optical microscope.
With mass fraction is that 3% sodium alginate normal saline solution 10ml is distributed among the edible vegetable oil 80ml that contains 0.5% span80, regulates motor speed and stirs 20 minutes to 1000r/min.Add mass concentration and be respectively 10% calcium chloride, 1% chitosan (deacetylation is 85.7%) solution 50ml initiation sodium alginate gel reaction, continue to stir after 60 minutes, collect slow-releasing microcapsule, adopt precipitation thoroughly to remove the fluid on slow-releasing microcapsule surface by degreaser from the drift method, collect, natural drying obtains slow-releasing microcapsule.
With mass fraction is that 1% sodium alginate normal saline solution 10ml is distributed among the edible vegetable oil 30ml that contains 1% span 80, regulates motor speed and stirs 15 minutes to 500r/min.Add mass concentration and be respectively 3% calcium chloride, 0.5% chitosan (deacetylation is 98.2%) solution 50ml initiation sodium alginate gel reaction, continue to stir after 20 minutes, collect slow-releasing microcapsule, adopt precipitation thoroughly to remove the fluid on slow-releasing microcapsule surface by degreaser from the drift method, collect, natural drying obtains slow-releasing microcapsule.
Degreaser described in the foregoing description 1-3 as Figure 1-3, it is made up of the pond 1 of deoiling, sedimentation tank 2 and oil sump 3, it is provided with highly from inside to outside from high to low, have a Rotational Cylindrical 4 and a lever that is coupling on the pond inwall that deoils to rock assembly in the described pond 1 of deoiling, Rotational Cylindrical 4 is made by light material, and is cylindrical, airtight hollow, the outer brush 5 that deoils that coats of Rotational Cylindrical 4, this brush 5 of deoiling is made by soft coarse material, can not damage microcapsule; Lever rocks assembly by rocking oil-collecting plate 6 and connecting rod 7 constitutes, the non-power end 9 that rocks oil-collecting plate 6 connects the adjustable floater shot 10 of gravity, the middle part of rocking oil-collecting plate 6 is coupling on the pond inwall that deoils, the nozzle side by side 12 of adjustable angle is equipped with in the exit of feed tube 11, it is positioned at the top of the power end 13 that rocks oil-collecting plate 6, the outer end of connecting rod 7 is connected on the Rotational Cylindrical 4, and the inner of connecting rod is connected by turning cylinder 8 with power end, and waste liquid discharge pipe 14 is housed on the oil sump 3.Rotational Cylindrical 4 is positioned at a side in the pond 1 of deoiling, the opposite side in gravity is adjustable floater shot 10 the is positioned at pond 1 of deoiling.
The power end 13 that rocks oil-collecting plate is a light material plate, and remainder is network structure, forms with the braiding of coarse material, to alleviate the resistance of water to oil-collecting plate.The outward flange on sedimentation tank 2 tops is equipped with filter screen 15 (can change filter screen as required), is used to block microcapsule and makes its precipitation.Time collection valve 16 is equipped with in the deoil bottom in pond 1, and the main valve 17 of collecting is equipped with in the bottom of sedimentation tank 2; Deoil and a feed hopper 18 is housed on the pond 1, the below of this feed hopper 18 is positioned at the place, lateral wall of Rotational Cylindrical 4, in the pond 1 of deoiling ultrasonic probe 19 is housed, and it is positioned at the top of Rotational Cylindrical 4.
The work process of above-mentioned degreaser is as follows: open feed tube, regulate the angle of nozzle side by side, make under the water flow impact pressure effect and rock oil-collecting plate and do not stop to rock, rotate thereby drive Rotational Cylindrical; After the alginate slow-releasing microcapsule adds from feed hopper, rotation by Rotational Cylindrical, the brush brush that deoils on it is from surperficial fluid, fluid rock oil-collecting plate and the effect of the brush that deoils under assemble come-up, oil content in the water is further reduced, fluid constantly come-up overflows, enter poly-oil sump, discharge by the waste liquid discharge pipe, microcapsule is filtered screen cloth and blocks gradually, and the microcapsule major part is in sedimentation tank, and small part is in the pond of deoiling, after treating the fluid removal totally on microcapsule surface, open primary and secondary and collect valve collection microcapsule.In addition, can also open Ultrasound Instrument when needed, further remove the fluid on microcapsule surface.
The above only is preferred embodiment of the present invention, is not structure of the present invention is done any pro forma restriction.Every foundation technical spirit of the present invention all falls within the scope of protection of the present invention any simple modification, equivalent variations and modification that above embodiment did.
Claims (8)
1. outside gelation prepares the method for alginate slow-releasing microcapsule, it is characterized in that with the sodium alginate soln being decentralized photo, edible vegetable oil is disperse medium, anhydrous sorbitol list olein is a surfactant, form water in oil small-sized drop through emulsifying, gelation reaction with calcium chloride chitosan solution initiation sodium alginate soln generates the alginate slow-releasing microcapsule, and the residual fluid on its surface adopts precipitation to remove from the drift method by a degreaser;
Described degreaser comprises the pond of deoiling that is provided with from inside to outside, sedimentation tank and oil sump, be provided with a Rotational Cylindrical and a lever that is coupling on the pond inwall that deoils in the described pond of deoiling and rock assembly, Rotational Cylindrical is outer to coat the brush that deoils, lever rocks assembly and comprises and rock an oil-collecting plate and a connecting rod, an end that rocks oil-collecting plate is a power end, the other end is non-power end, the middle part of rocking oil-collecting plate is coupling on the pond inwall that deoils, described non-power end connects the adjustable floater shot of a gravity, the outlet of one feed tube is positioned at the top of the power end that rocks oil-collecting plate, the outer end of connecting rod is connected on the Rotational Cylindrical, the inner of connecting rod is connected by a turning cylinder with power end, one waste liquid discharge pipe is housed on the oil sump, the exit of feed tube is provided with the nozzle side by side of adjustable angle, deoil and a feed hopper is housed on the pond, the below of this feed hopper is positioned at the top of the brush that deoils;
Described precipitation is as follows from the step of method of drifting about: open feed tube, regulate the angle of nozzle side by side, make under the water flow impact pressure effect and rock oil-collecting plate and do not stop to rock, rotate thereby drive Rotational Cylindrical; After the alginate slow-releasing microcapsule adds from feed hopper, rotation by Rotational Cylindrical, the brush brush that deoils on it is from surperficial fluid, fluid rock oil-collecting plate and the effect of the brush that deoils under assemble come-up, oil content in the water is further reduced, fluid constantly come-up overflows, and enters oil sump, discharges by the waste liquid discharge pipe.
2. outside gelation according to claim 1 prepares the method for alginate slow-releasing microcapsule, it is characterized in that with mass concentration being that the sodium alginate soln of 0.5%-3% is distributed to meter by volume and contains in the edible vegetable oil of anhydrous sorbitol list olein of 0.5%-2%, water oil phase volume ratio is 1: 3-1: between 8.
3. outside gelation according to claim 1 prepares the method for alginate slow-releasing microcapsule, it is characterized in that water in oil small-sized drop realizes by motor stirring system, rotating speed of motor is 100r/min-1500r/min, and emulsification times is 10-30 minute.
4. outside gelation according to claim 1 prepares the method for alginate slow-releasing microcapsule, it is characterized in that the calcium chloride chitosan solution is that the calcium chloride solution of 1%-10% and chitosan solution that mass concentration is 0.4%-1% are formed by mass concentration, the deacetylation of chitosan is more than 85%.
5. outside gelation according to claim 1 prepares the method for alginate slow-releasing microcapsule, and the power end that it is characterized in that rocking oil-collecting plate is the light material plate of a semicircle, and remainder is network structure.
6. outside gelation according to claim 1 prepares the method for alginate slow-releasing microcapsule, it is characterized in that the height of the described pond of deoiling, sedimentation tank and oil sump reduces step by step, and the outward flange on sedimentation tank top is equipped with filter screen.
7. outside gelation according to claim 1 prepares the method for alginate slow-releasing microcapsule, and the bottom in the pond that it is characterized in that deoiling is equipped with and is once collected valve, and a main valve of collecting is equipped with in the bottom of sedimentation tank.
8. outside gelation according to claim 1 prepares the method for alginate slow-releasing microcapsule, it is characterized in that described Rotational Cylindrical is positioned at a side in the pond of deoiling, and the adjustable floater shot of gravity is positioned at the opposite side in the pond of deoiling; Deoil and ultrasonic probe is housed in the pond, it is positioned at the top of Rotational Cylindrical, and described Rotational Cylindrical is a hollow structure.
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| CN102120169A (en) * | 2010-12-27 | 2011-07-13 | 河北联合大学 | Sodium iron chlorophyllin-chitosan/sodium alginate microcapsules and preparation method thereof |
| CN102266308B (en) * | 2011-07-27 | 2012-10-24 | 淮阴工学院 | Method for preparing odor masking sustained-release garlicin composite micro-capsules |
| CN103099798B (en) * | 2013-01-29 | 2014-12-17 | 浙江中医药大学 | Preparation method of soybean isoflavone-chitosan slow-release microcapsules |
| CN105311630B (en) * | 2014-06-20 | 2019-07-09 | 普莱柯生物工程股份有限公司 | A kind of mammalian cell suspension culture prepares the method and application of vaccine |
| CN104645306B (en) * | 2015-01-27 | 2017-10-20 | 李建民 | The preparation technology of oral placenta peptide chitosan sodium alginate slow-releasing microcapsule |
| CN105724429A (en) * | 2016-04-15 | 2016-07-06 | 佛山市聚成生化技术研发有限公司 | Preparing method for degradable modified chitosan bactericide and prepared degradable modified chitosan bactericide |
| CN111358711B (en) * | 2018-12-25 | 2023-08-11 | 万华化学集团股份有限公司 | Photosensitive material/calcium alginate core-shell nanocapsule dispersoid and preparation method thereof |
| CN112515981B (en) * | 2020-11-24 | 2021-07-30 | 湖南御家化妆品制造有限公司 | Light absorption core-shell structure particle and preparation method and application thereof |
| CN116531275B (en) * | 2023-07-04 | 2023-10-13 | 北京青颜博识健康管理有限公司 | Microcapsule for relieving high-concentration vitamin C ethyl ether stimulation and preparation method and application thereof |
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