CN101015537A - Preparation method of sodium iron chlorophyllin-ethyl cellulose microcapsule - Google Patents

Preparation method of sodium iron chlorophyllin-ethyl cellulose microcapsule Download PDF

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Publication number
CN101015537A
CN101015537A CNA2007100615468A CN200710061546A CN101015537A CN 101015537 A CN101015537 A CN 101015537A CN A2007100615468 A CNA2007100615468 A CN A2007100615468A CN 200710061546 A CN200710061546 A CN 200710061546A CN 101015537 A CN101015537 A CN 101015537A
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China
Prior art keywords
sodium iron
iron chlorophyllin
ethyl cellulose
microcapsule
preparation
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CNA2007100615468A
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CN100462067C (en
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刘淑萍
王丽芸
闫路省
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Hebei University of Science and Technology
Hebei Polytechnic University
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Hebei University of Science and Technology
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Priority to CNB2007100615468A priority Critical patent/CN100462067C/en
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Abstract

A preparation method of sodium iron chlorophyllin-ethyl cellulose microcapsule belongs to preparation field of medicinal and edible pigment. the method with sodium iron chlorophyllin as contents and ethyl cellulose as capsule comprises adding sodium iron chlorophyllin into 2% ethyl cellulose carbon tetrachloride solution, stirring in aqueous thermostat, making into suspensoid solution of sodium iron chlorophyllin, adding to non-solvent of petroleum ether, stirring for 1h, centrifugalizing for 20min, washing with petroleum ether for several time, removing supernatant, paving on the surface of glass plate, and drying in drying oven to obtain the final product. The microcapsule with EC as capsule materials has the advantages of stable property, little toxicity. Microcapsule prepared with auxiliary materials at a certain proportion has slow release, which can maintain effective blood concentration for a long time, and guarantee the therapeutic effect of the drugs.

Description

The preparation method of sodium iron chlorophyllin-ethyl cellulose microcapsule
Technical field
The present invention relates to a kind of preparation method of sodium iron chlorophyllin-ethyl cellulose microcapsule, 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 chlorophyll iron (II) salt and chlorophyll iron (III) salt), be insoluble in the oils.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 hemopoietic that raw material is made, and is successfully used to the treatment of iron deficiency anemia, and this only is unique iron chlorophyllin sodium salt pharmaceutically dosage form at home.Utilize the characteristic of microcapsule, the further microcapsule 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.Do not see the research report that has the sodium iron chlorophyllin microcapsule especially to prepare the sodium iron chlorophyllin microcapsule up to now as yet with ethyl cellulose.
Summary of the invention
The purpose of this invention is to provide a kind of with ferrum (II) CHLOROPHYLLINE sodium salt core-clad material, EC capsule material, the sodium iron chlorophyllin-ethyl cellulose microcapsule preparation method of solvent-nonsolvent system carbon tetrachloride-petroleum ether.This method has strengthened the stability of sodium iron chlorophyllin, and prepared microcapsule has tangible slow releasing function.
Realize the foregoing invention purpose by the following technical solutions:
A kind of preparation method of sodium iron chlorophyllin-ethyl cellulose microcapsule comprises sodium iron chlorophyllin and ethyl cellulose.Get sodium iron chlorophyllin, join in the carbon tetrachloride solution solvent of 2% ethyl cellulose, put in 39~41 ℃ of waters bath with thermostatic control and stir, make the sodium iron chlorophyllin suspension; It is joined in the petroleum ether non-solvent sodium iron chlorophyllin suspension while stirring, continue to stir 1h, be placed on centrifugal 20min in the centrifuge, use petroleum ether then three times, remove supernatant, be laid on the glass pane surface in the drying baker dryly, promptly get sodium iron chlorophyllin-ethyl cellulose microcapsule.
The core-clad material sodium iron chlorophyllin is soluble in water, and water solution system slightly is alkalescence.Capsule material EC is the water-insoluble cellulose derivative, water insoluble, gastro-intestinal Fluid, glycerol and propylene glycol, but can be dissolved in multiple organic solvents such as ethanol, acetone, isopropyl alcohol, benzene, chloroform, dichloromethane, ethyl chloride, carbon tetrachloride, be one of insoluble framework material of using always.But imbibition also produces certain stickiness, and makes the stripping of medicine and diffusion be subjected to the purpose that certain restriction reaches slow releasing function.Be equipped with sodium iron chlorophyllin-ethyl cellulose microcapsule with the solvent-nonsolvent legal system in the phase separation method.
Medicine is scattered in (being the solvent carbon tetrachloride) in the capsule material solution, add a kind of and the not miscible liquid (being the non-solvent petroleum ether) of capsule material, cause to be separated and medicine is rolled into microcapsule, but core-clad material must all not dissolve yet not interreaction to the solvent and the non-solvent of capsule material in the system.
The significant 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.At first require capsule wood property matter stable as medicament microcapsule, secondly avirulence has slow releasing function behind the encystation.The present invention selects ethyl cellulose (Ethylcellulose for use, EC) as the capsule material, it is the cellulose derivative that the part of hydroxyl in the cellulose chain is replaced by ethyoxyl, it is one of most widely used water-insoluble cellulose derivative, but imbibition also produces certain stickiness, and make the stripping of medicine and diffusion be subjected to certain restriction, reach the purpose of slow releasing function.Thereby be suitable as the release of the capsule material control water soluble drug of microcapsule, and and with its outstanding physical and chemical stability, minimum toxicity and being widely used.EC has different dissolubilities in different preparations, mix with certain proportion with other adjuvants and produce different rate of releasing drug, make medicine form stable and effectively slow control delivery, make the blood drug level that the medicine long period remains valid, make things convenient for the patient, guaranteed the curative effect of medicine.With sem observation microcapsule granule situation, be essentially spherical, between 13~23 μ m, it is the following apertures that reach the drug release function of 2.9 μ m that the microcapsule granule surface distributed closeer maximum gauge behind the capsule wall.Laser particle size analyzer is measured concentrated 100~200 μ m that are distributed in of particle size range.Drug loading is 40.4%, and envelop rate is 85.36%.Strengthened the stability of sodium iron chlorophyllin.Microcapsule has tangible slow releasing function, discharges about 70% in 4 hours.
The specific embodiment
The present invention will be further described below in conjunction with embodiment.
Key instrument: AEL-160 electronic balance; HH-S digital display thermostat water bath; The reinforcement electric blender; Centrifuge; Medicament dissolution instrument; The KYKY2800 scanning electron microscope, resolution 4.5nm; Laser particle size analyzer; F7230 type spectrophotometer.
Reagent and raw material: carbon tetrachloride, petroleum ether, ethyl cellulose; Sodium iron chlorophyllin.
The concrete operations step
Get sodium iron chlorophyllin, join in the carbon tetrachloride solution solvent of 2% ethyl cellulose, place 39~41 ℃ of constant temperature of HH-S digital display thermostat water bath, stir under the 350r/min speed, make the sodium iron chlorophyllin suspension; The sodium iron chlorophyllin suspension is joined it (according to the part by weight adding of selecting) in petroleum ether non-solvent while stirring, the reinforcement electric blender continues to stir 1h, be placed on centrifugal 20min in the centrifuge, use petroleum ether then three times, remove supernatant, be laid on the glass pane surface in the drying baker dryly, promptly get sodium iron chlorophyllin-ethyl cellulose microcapsule.
The preparation process condition of sodium iron chlorophyllin microcapsule
Determine that with orthogonal experiment the best preparation technology of sodium iron chlorophyllin-ethyl cellulose microencapsulation is: the carbon tetrachloride solvent system of 2%EC, the ratio of EC/ sodium iron chlorophyllin are 2: 1, stir 1h under the mixing speed of 350r/min, separate, and are drying to obtain.
Detect performance indications
Performance indications
1. scanning electron microscope (SEM) measurement result is seen Fig. 1,2,3.
With sem observation microcapsule granule situation, be essentially spherical, between 13~23 μ m, it is the following apertures that reach the drug release function of 2.9 μ m that the microcapsule granule surface distributed closeer maximum gauge behind the capsule wall.
2. the drug loading of chemical determination sodium iron chlorophyllin-ethyl cellulose microcapsule is 40.4%, and envelop rate is 85.36%.
3. medicament dissolution instrument is measured: microcapsule has tangible slow releasing function, and 4h discharges about 70%.
4. utilize F7230 type spectrophotometer that the stability that the sodium iron chlorophyllin microcapsule has strengthened sodium iron chlorophyllin is measured, the result: microcapsule Chinese medicine content is constant in 30 days, its particulate dispersibility, mobile fine.

Claims (1)

1, a kind of preparation method of sodium iron chlorophyllin-ethyl cellulose microcapsule, it is core-clad material with the sodium iron chlorophyllin, ethyl cellulose is the capsule material, it is characterized in that, as follows preparation:
A, get sodium iron chlorophyllin, join in the carbon tetrachloride solution solvent of 2% ethyl cellulose, put in 39~41 ℃ of waters bath with thermostatic control and stir, make the sodium iron chlorophyllin suspension;
B, it is joined in the petroleum ether non-solvent sodium iron chlorophyllin suspension while stirring, continue to stir 1h, be placed on centrifugal 20min in the centrifuge, then for several times with petroleum ether, remove supernatant, be laid on the glass pane surface in the drying baker dryly, promptly get sodium iron chlorophyllin-ethyl cellulose microcapsule.
CNB2007100615468A 2007-02-15 2007-02-15 Preparation method of sodium iron chlorophyllin-ethyl cellulose microcapsule Expired - Fee Related CN100462067C (en)

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CN100462067C CN100462067C (en) 2009-02-18

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102114400A (en) * 2010-12-30 2011-07-06 唐山师范学院 Method for preparing sodium alginate-iron chlorophyllin sodium microcapsule
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
CN104855375A (en) * 2015-05-11 2015-08-26 张国财 Ragweed plant source microcapsule preparation
CN108083451A (en) * 2017-12-12 2018-05-29 武汉沃田生态科技有限公司 A kind of compound bacteria microcapsule water purification agent of slow-release and preparation method thereof
CN111359553A (en) * 2020-03-12 2020-07-03 蚌埠学院 Preparation method of biodegradable edible pigment microcapsule

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU2800000A (en) * 1999-02-15 2000-09-04 Bernard, Laurence M. C. Encapsulation
JP2002035571A (en) * 2000-07-26 2002-02-05 Dai Ichi Kogyo Seiyaku Co Ltd Microcapsule including associable chlorophyllous coloring matter and method for manufacturing the same
CN1195068C (en) * 2001-01-02 2005-03-30 蒋佃水 Small peptide heme and its prepn

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN102114400A (en) * 2010-12-30 2011-07-06 唐山师范学院 Method for preparing sodium alginate-iron chlorophyllin sodium microcapsule
CN102114400B (en) * 2010-12-30 2012-12-26 唐山师范学院 Method for preparing sodium alginate-iron chlorophyllin sodium microcapsule
CN104855375A (en) * 2015-05-11 2015-08-26 张国财 Ragweed plant source microcapsule preparation
CN108083451A (en) * 2017-12-12 2018-05-29 武汉沃田生态科技有限公司 A kind of compound bacteria microcapsule water purification agent of slow-release and preparation method thereof
CN111359553A (en) * 2020-03-12 2020-07-03 蚌埠学院 Preparation method of biodegradable edible pigment microcapsule

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