CN102120169A - Sodium iron chlorophyllin-chitosan/sodium alginate microcapsules and preparation method thereof - Google Patents
Sodium iron chlorophyllin-chitosan/sodium alginate microcapsules and preparation method thereof Download PDFInfo
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- CN102120169A CN102120169A CN2010106237313A CN201010623731A CN102120169A CN 102120169 A CN102120169 A CN 102120169A CN 2010106237313 A CN2010106237313 A CN 2010106237313A CN 201010623731 A CN201010623731 A CN 201010623731A CN 102120169 A CN102120169 A CN 102120169A
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Abstract
The invention discloses sodium iron chlorophyllin-chitosan/sodium alginate microcapsules and a preparation method thereof. In the method, chitosan/sodium alginate is used as a capsule material, sodium iron chlorophyllin is used as capsule content, and the sodium iron (II) chlorophyllin is microencapsulated by an emulsification-gel method. The preparation method comprises: dissolving sodium iron chlorophyllin in sodium alginate solution at a certain concentration, adding the prepared solution in vegetable oil containing Span-60, and stirring at high steep and emulsifying for 20 minutes; dripping acetic acid aqueous solution containing 2.0-percent chitosan and calcium chloride, continuously stirring for 30 minutes, standing for 2 hours and removing an oil phase; and washing the microcapsules with petroleum ether and isopropanol for three times respectively, performing suction-filtration, and drying at room temperature to obtain the sodium iron chlorophyllin-chitosan/sodium alginate microcapsules. The chitosan which is a natural polysaccharide with high biocompatibility and biodegradability and the sodium alginate serve as sustained and controlled release agent and targeting preparation, the sodium iron chlorophyllin is encapsulated in the center of the microcapsules to be protected from instability caused by change in a light or placing condition, a new formulation is provided in pharmacy, and the microcapsules are suitable to be further developed and used as iron-supplying health-care food and new medicinal preparation for treating iron-deficiency anemia, and have a bright application prospect.
Description
Technical field
The present invention relates to a kind of sodium iron chlorophyllin-shitosan/sodium alginate (CTS/ALG) microcapsules and preparation method, belong to medicinal and preparation method field food coloring.
Background technology
In the soluble in water or Diluted Alcohol solution of sodium iron chlorophyllin (comprising phyllo-iron (II) salt and phyllo-iron (III) salt), be insoluble in the grease class.It is stable to indoor lucifuge to test the iron chlorophyllin sodium solution after deliberation, but not ideal enough to its stability of outdoor natural light.The iron chlorophyllin sodium salt is except being a kind of good food coloring, pharmaceutically can be used as ferrous-fortifier, with the sodium iron chlorophyllin is the peaceful sheet of green blood that raw material is made, and is successfully used to the treatment of hypoferric anemia, and this only is unique iron chlorophyllin sodium salt pharmaceutically dosage form at home.Utilize the characteristic of microcapsules, the further micro-capsule gel of sodium iron chlorophyllin is handled, not only improved medicine stability but also the exploitation of sustained-release preparation is had active operation significance.The inventor has obtained preparation method's patent of invention (patent No. ZL200710061546.8) of sodium iron chlorophyllin-ethyl cellulose microcapsule.Having excellent biological compatibility and biological degradability and the natural polysaccharide that plays sustained-release preparation and targeting preparation effect---shitosan and sodium alginate capsule material relatively will more help improving the drug effect and the bioavilability of medicine with seeing the ethyl cellulose capsule material that can not degrade after light easily decomposes, eats.Do not see as yet that up to now useful chitin-sodium alginate prepares the research report of sodium iron chlorophyllin micro-capsule for the capsule material.
Summary of the invention
The purpose of this invention is to provide a kind of with iron (II) chlorophyllin sodium salt core-clad material, CTS/ALG capsule material, emulsification iron complexing-gelling process sodium iron chlorophyllin-shitosan/sodium alginate micro gel capsule preparation method and product.This method has strengthened the stability of sodium iron chlorophyllin, and prepared micro-capsule has tangible slow releasing function and bioavilability.
In order to realize the foregoing invention purpose, the present invention has adopted following technical scheme:
The preparation method of a kind of sodium iron chlorophyllin-shitosan/sodium alginate micro-capsule, comprise sodium iron chlorophyllin and shitosan/sodium alginate, it is characterized in that, get in the sodium alginate soln that sodium iron chlorophyllin is dissolved in 1.5 times, the solution that generates places the vegetable oil that contains 1.0gSpan-60, (more than the 600r/min) stirs at a high speed, emulsification 20min.Splash into the acetic acid aqueous solution that contains 2.0% shitosan and calcium chloride, continue to stir 30min, leave standstill 2h, remove oil phase.Micro-capsule is given a baby a bath on the third day after its birth inferior respectively with benzinum, isopropyl alcohol, suction filtration, and drying at room temperature promptly gets sodium iron chlorophyllin-shitosan/sodium alginate micro gel capsule.
The core-clad material sodium iron chlorophyllin is soluble in water, and water solution system slightly is alkalescence.(Chitosan CTS) is the chitin deacetylase based products to shitosan, and the source is abundant, and preparation is simple.Have anti-inflammation, promote wound healing, pharmacologically actives such as antiacid, antiulcer, lipopenicillinase and reduction cholesterol.Be alkaline polysaccharide unique in the natural polysaccharide, the stability of utilizing micro-capsule that shitosan makes or microballoon can increase protein, polypeptide drug reduces medicine side effect in vivo, the prolong drug curative effect.Shitosan is as novel auxiliary material extensive use.
(Sodium alginate ALG) is the sodium salt of a kind of polyanionic polysaccharide that extracts (alginic acid) to sodium alginate from natural brown alga.Because of its unique physical and chemical properties and excellent biological compatibility, be widely used in fields such as pharmaceutical preparation, organizational project, clinical treatment, cell cultivation, food processing.Contain carboxyl and hydroxyl freely in the ALG molecule, can form gel with multiple metal ion; As the natural polysaccharide of polyanion type can with multiple polycation compound of polysaccharide such as synergies such as shitosan and polylysine, make micro-capsule by adopting dropping preparation method, emulsion process, spray-on process etc., both improved micro-capsule stability and medicine embedding rate, can strengthen under different pH values discharging the controllability of medicine again.Because can better sticking to mucomembranous surface, anion ratio polycation or uncharged macromolecular material make it have certain advantage as the mucosa delivery carrier.Sodium alginate micro-capsule will help improving drug effect and the bioavilability of medicine in mucosal sites such as stomach and intestine or nasopharynxs.
CTS its with to have the sodium alginate of negative electrical charge compatible, form compound capsule material by electrostatic interaction, become the research focus of newtype drug delivery system.Emulsification iron complexing-gelling process with complex coacervation prepares sodium iron chlorophyllin-shitosan/sodium alginate micro gel capsule.
Particularly, preparation sodium iron chlorophyllin-shitosan of the present invention/sodium alginate micro-capsule method may further comprise the steps:
1, gets in the ALG solution that sodium iron chlorophyllin is dissolved in 1.5 times, generate solution;
2, generate solution and place the vegetable oil that contains 1.0gSpan-60, (more than the 600r/min) stirs at a high speed, emulsification 20min;
3, splash into the acetic acid aqueous solution that contains 2.0% shitosan and calcium chloride, continue to stir 30min, leave standstill 2h, supernatant liquid gets micro-capsule in the removal;
4, micro-capsule is given a baby a bath on the third day after its birth respectively time with benzinum, isopropyl alcohol, suction filtration, and drying at room temperature promptly gets sodium iron chlorophyllin-shitosan/sodium alginate micro gel capsule.
Further, ALG concentration is 1.5%-2.0% in the preparation process, calcium chloride concentration 3.0%, acetate concentration 2.0%.Mixing speed 600r/min-900r/min.
Wherein, the arbitrary data control of mixing speed between 600r/min-900r/min all with micro-capsule not broken wall be the best.
Remarkable advantage of the present invention is that the character of core-clad material and the purpose of microencapsulation have determined the character of used capsule material.The present invention selects for use CTS/ALG as the capsule material, stable in properties, nontoxic, have the trophism and the property of medicine concurrently.CTS its with to have the ALG of negative electrical charge compatible, form compound capsule material by electrostatic interaction, be newtype drug delivery system quality material.Preparing sodium iron chlorophyllin-shitosan/sodium alginate micro gel capsule with emulsification iron complexing-gelling process sticks to mucomembranous surface and makes it as the mucosa delivery carrier, make the stripping and the diffusion of medicine be subjected to certain restriction, reach the purpose of slow releasing function, improved drug effect and the bioavilability of medicine in mucosal sites.Safe preparation process, convenience, simple to operate.With sem observation microcapsule granule situation, be essentially elliposoidal, see accompanying drawing 1.The microscopically of laser particle size analyzer and order micrometer is observed and is measured the concentrated 75 μ m～100 μ m that are distributed in of particle size range.The medicine carrying amount is 50.41%, and envelop rate is 88.52%.Strengthened the stability of sodium iron chlorophyllin.Micro-capsule has tangible slow releasing function, discharges accumulation and is lower than 60% in external 4 hours.The nontoxic operation of this technology is fit to suitability for industrialized production.
Description of drawings
Fig. 1 is the microcapsules picture (amplifying 800 times) of microscopically.
The specific embodiment
The present invention will be further described below in conjunction with specific embodiment.
The key instrument that the present invention uses comprises: the AEL-160 electronic balance; HH-S digital display thermostat water bath (Jintan); The reinforcement electric blender; Medicament dissolution instrument; Miillpore filter; The KYKY2800 SEM, resolution ratio 4.5nm; Laser particle size analyzer; F7230 type spectrophotometer (Xiamen);
The main medicine that the present invention uses: sodium iron chlorophyllin.Shitosan (molecular weight 200,000, deacetylation＞85%), the biological Co., Ltd of Zhejiang Yuhuan gold shell; Sodium alginate (viscosity is 600cps), Qingdao Jin Ying Co., Ltd; Calcium chloride; Acetic acid.
Embodiment 1
Get in 1.5% sodium alginate soln that sodium iron chlorophyllin is dissolved in 1.5 times, the solution that generates places the vegetable oil that contains 1.0gSpan-60, stirs emulsification 20min with 600r/min.Splash into the acetic acid aqueous solution that contains 2.0% shitosan and calcium chloride, continue to stir 30min, leave standstill 2h, remove oil phase.Micro-capsule is given a baby a bath on the third day after its birth inferior respectively with benzinum, isopropyl alcohol, suction filtration, and drying at room temperature promptly gets sodium iron chlorophyllin-shitosan/sodium alginate micro gel capsule.
Carry out the micro-capsule evaluation: its outward appearance becomes uniform spheroid shape to see Fig. 1, is uniformly dispersed; Particle diameter is distributed in 75 μ m～100 mu m ranges and reaches 70%; External 4 hours releases 50% of micro-capsule.
Embodiment 2
Get in 1.8% sodium alginate soln that sodium iron chlorophyllin is dissolved in 1.5 times, the solution that generates places the vegetable oil that contains 1.0gSpan-60, stirs emulsification 20min with 700r/min.Splash into the acetic acid aqueous solution that contains 2.0% shitosan and calcium chloride, continue to stir 30min, leave standstill 2h, remove oil phase.Micro-capsule is given a baby a bath on the third day after its birth inferior respectively with benzinum, isopropyl alcohol, suction filtration, and drying at room temperature promptly gets sodium iron chlorophyllin-shitosan/sodium alginate micro gel capsule.
Carry out the micro-capsule evaluation: its outward appearance becomes uniform spheroid shape to see Fig. 1; Particle diameter is distributed in 100 ± 0.65 mu m ranges and reaches 60%; External 4 hours releases 40% of micro-capsule.
Embodiment 3
Get in 2.0% sodium alginate soln that sodium iron chlorophyllin is dissolved in 1.5 times, the solution that generates places the vegetable oil that contains 1.0gSpan-60, stirs emulsification 20min with 900r/min.Splash into the acetic acid aqueous solution that contains 2.0% shitosan and calcium chloride, continue to stir 30min, leave standstill 2h, remove oil phase.Micro-capsule is given a baby a bath on the third day after its birth inferior respectively with benzinum, isopropyl alcohol, suction filtration, and drying at room temperature promptly gets sodium iron chlorophyllin-shitosan/sodium alginate micro gel capsule.
Carry out the micro-capsule evaluation: its outward appearance becomes uniform spheroid shape and broken capsule, causes scrotiform irregular; Particle diameter reaches 70% in 75 ± 0.74 mu m ranges; External 4 hours releases 60% of micro-capsule.
Although above the specific embodiment of the present invention has been given to describe in detail and explanation; but what should indicate is; we can carry out various equivalences to above-mentioned embodiment according to conception of the present invention and change and modification; when the function that it produced does not exceed spiritual that specification and accompanying drawing contain yet, all should be within protection scope of the present invention.
The preparation optimum process condition of sodium iron chlorophyllin microcapsules
Determine the best preparation process condition of sodium iron chlorophyllin-CTS/ALG microencapsulation with orthogonal experiment: ALG/ sodium iron chlorophyllin (g/g) is 2: 1, and 2%ALG liquor ratio 2%CTS liquid (v/v) is 1: 1.600r/min stirs.
Claims (9)
1. sodium iron chlorophyllin-shitosan/sodium alginate micro gel capsule product
2. the preparation method of sodium iron chlorophyllin-shitosan/sodium alginate micro gel capsule is characterized in that, prepares sodium iron chlorophyllin-shitosan/sodium alginate micro gel capsule by emulsification iron complexing-gelling process.
3. method as claimed in claim 2 is characterized in that: being capsule core material with the sodium iron chlorophyllin, is the capsule material with shitosan/sodium alginate, is prepared.
4. as claim 2 or 3 described methods, may further comprise the steps:
1) gets in the ALG solution that sodium iron chlorophyllin is dissolved in 1.5 times, generate solution;
2) generate solution and place the vegetable oil that contains 1.0gSpan-60, (more than the 600r/min) stirs at a high speed, emulsification 20min;
3) splash into the acetic acid aqueous solution that contains 2.0% shitosan and calcium chloride, continue to stir 30min, leave standstill 2h, remove oil phase;
4) micro-capsule is given a baby a bath on the third day after its birth respectively time with benzinum, isopropyl alcohol, suction filtration, and drying at room temperature promptly gets sodium iron chlorophyllin-shitosan/sodium alginate micro gel capsule.
5. method as claimed in claim 4, wherein, ALG/ sodium iron chlorophyllin (g/g) is 2: 1.
6. method as claimed in claim 4, wherein, vegetable oil is edible.
7. method as claimed in claim 4, wherein, the arbitrary data control of mixing speed between 600r/min-900r/min all with micro-capsule not broken wall be optimised quantity.
8. method as claimed in claim 4, wherein, ALG liquor ratio CTS liquid (v/v) is 1: 1, ALG concentration is 1.5%, 1.8%, 2.0%, calcium chloride concentration 3.0%, acetate concentration 2.0%.
9. method as claimed in claim 4, wherein, sodium iron chlorophyllin-shitosan/sodium alginate micro gel capsule product appearance becomes smooth spheroid shape, and particle size range is concentrated and is distributed in 75 μ m～100 μ m.The medicine carrying amount is 50.41%, and envelop rate is 88.52%.Release accumulation in 4 hours is lower than 60%.
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Cited By (8)
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| CN102578110A (en) * | 2011-12-23 | 2012-07-18 | 河海大学 | Preparation method of artemisinin slow-release body |
| CN103006617A (en) * | 2012-12-31 | 2013-04-03 | 青岛农业大学 | Decoquinate oral micro-capsule preparation and preparation process thereof |
| CN103157413A (en) * | 2013-03-28 | 2013-06-19 | 湖南农业大学 | Method for preparing sodium alginate microcapsule-supported nanoscale zero-valent iron particles |
| CN103271424A (en) * | 2013-05-28 | 2013-09-04 | 上海交通大学 | Preparing method of fragrant microcapsule |
| CN104087020A (en) * | 2014-07-01 | 2014-10-08 | 常州大学 | Preparation method and application of chitosan-natural plant pigment macromolecular dye solution |
| CN105477014A (en) * | 2015-12-15 | 2016-04-13 | 中国疾病预防控制中心营养与健康所 | Nano-level ferrous sulfate nutritional supplement micro-capsule product and preparation process thereof |
| CN114948911A (en) * | 2022-06-17 | 2022-08-30 | 佛山市中医院 | A kind of traumatic oil sustained-release microcapsule and preparation method thereof |
| CN115606811A (en) * | 2022-04-19 | 2023-01-17 | 中国科学院烟台海岸带研究所 | Preparation method of stichopus japonicus visceral oligopeptide microcapsules and microcapsules |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102578110A (en) * | 2011-12-23 | 2012-07-18 | 河海大学 | Preparation method of artemisinin slow-release body |
| CN103006617A (en) * | 2012-12-31 | 2013-04-03 | 青岛农业大学 | Decoquinate oral micro-capsule preparation and preparation process thereof |
| CN103157413A (en) * | 2013-03-28 | 2013-06-19 | 湖南农业大学 | Method for preparing sodium alginate microcapsule-supported nanoscale zero-valent iron particles |
| CN103271424A (en) * | 2013-05-28 | 2013-09-04 | 上海交通大学 | Preparing method of fragrant microcapsule |
| CN103271424B (en) * | 2013-05-28 | 2015-08-12 | 上海交通大学 | A kind of preparation method of essence microcapsule |
| CN104087020A (en) * | 2014-07-01 | 2014-10-08 | 常州大学 | Preparation method and application of chitosan-natural plant pigment macromolecular dye solution |
| CN104087020B (en) * | 2014-07-01 | 2016-01-06 | 常州大学 | The preparation method of a kind of chitosan-natural plant pigment macromole dye liquor and application |
| CN105477014A (en) * | 2015-12-15 | 2016-04-13 | 中国疾病预防控制中心营养与健康所 | Nano-level ferrous sulfate nutritional supplement micro-capsule product and preparation process thereof |
| CN105477014B (en) * | 2015-12-15 | 2018-04-13 | 中国疾病预防控制中心营养与健康所 | A kind of nanometer grade ferrous sulfate nutritional supplement microencapsulation product and its preparation process |
| CN115606811A (en) * | 2022-04-19 | 2023-01-17 | 中国科学院烟台海岸带研究所 | Preparation method of stichopus japonicus visceral oligopeptide microcapsules and microcapsules |
| CN114948911A (en) * | 2022-06-17 | 2022-08-30 | 佛山市中医院 | A kind of traumatic oil sustained-release microcapsule and preparation method thereof |
| CN114948911B (en) * | 2022-06-17 | 2024-02-09 | 佛山市中医院 | A kind of Shangke oil sustained-release microcapsule and its preparation method |
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Application publication date: 20110713 |