CN1554330A - Konjaku gluocomannan-calcium alginate microball for carrying medicine and preparing method - Google Patents
Konjaku gluocomannan-calcium alginate microball for carrying medicine and preparing method Download PDFInfo
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- CN1554330A CN1554330A CNA2003101178380A CN200310117838A CN1554330A CN 1554330 A CN1554330 A CN 1554330A CN A2003101178380 A CNA2003101178380 A CN A2003101178380A CN 200310117838 A CN200310117838 A CN 200310117838A CN 1554330 A CN1554330 A CN 1554330A
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Abstract
The said microballoon is in single nuclear structure or in core-shell structure. The core material is composite of konjaku glucomannan and calcium alginate; and the shell material is chitosan-calcium alginate polyelectrolyte film. The preparation process includes dropping the mixed hydrosol of konjaku glucomannan-calcium alginate into the water solution of CaCl2 or chitosan-CaCl2; water washing and drying the microspherical matter to obtain konjaku glucomannan-calcium alginate or konjaku glucomannan-calcium alginate-chitosan microballoon. The present invention has the advantages of raised medicine slow releasing performance, easy control of medicine release, simple technological process, low production cost and easy scale production.
Description
Technical field
The present invention relates to a kind of Rhizoma amorphophalli glucomannan-calcium alginate microsphere and preparation method, belong to the microsphere preparation technology that is used for medicine carrying.
Background technology
Natural polysaccharide has characteristics such as biocompatibility is good as the medicament slow release material, has obtained extensive studies and application.Alginic acid is a kind of acidic polysaccharose that extracts from Brown algae, links the linear block copolymers that form in three kinds of modes (being MM section, GG section and MG section) by α (1-4) glycosidic bond by two kinds of construction units of guluronic acid (being designated as the G section) and its stereoisomer mannuronic acid (being designated as the M section).It can form hydrogel in the bivalent metal ion aqueous solution, the preparation condition gentleness is suitable for embedding protein, enzyme and cell isoreactivity material.In addition, it has excellent biological compatibility and bioadhesive, makes it have certain advantage as the mucosa delivery carrier.In addition, alginic acid is a kind of polyanion polyelectrolyte, and formed gel has loose structure, by regulating preparation condition, can improve the medicament slow release performance easily, as adopts different gel ions, adds other material or overlay film etc.
Alginic acid at pH=5 to stable chemical performance between the pH=10.In low pH value medium, the alginic acid molecular weight can reduce, and it is placed in the neutral medium once more can discharges the embedding thing rapidly.Therefore when alginic acid gel during as the oral drugs slow-release material, in acidic gastric juice, though because acid precipitation phenomenon, the swellbility of alginic acid gel is less, the release of medicine is lower, but after entering neutral intestinal juice, because the hydrolysis of acid, alginic acid will lose the gel ion release medicine of degrading rapidly, might cause the burst release of medicine.
At present, improving the alginic acid gel is to cover poly-L-Lysine (PLL) or chitosan film in the alginic acid gel surface to the main method of drug release characteristics, this will form the comparatively fine and close polyelectrolyte film of one deck in gel surface, can reduce release aperture, raising gel strength and the acid-resisting of medicine.In the recent period, the researcher report is arranged, use alginic acid and pectin as the core macromolecular material, the PLL overlay film prepares microcapsule, has obtained effect preferably.Pectin helps to form the better capsule of intensity, and can resist acid solution, and can be in control drug release under the alkali condition.Pectin is a kind of dietary fiber, and it can not be decomposed by digestive enzyme etc. in vivo and utilizes, only in large intestine as the substrate of part thalline, be different from alginic acid in gastric acid, to degrade, this may be its reason that can resist acid solution.Change the ratio and the gel speed of alginic acid and methoxy group pectin, will influence particulate size, stability, pH response, drug loading and rate of release.In addition, alginic acid is being made in the process of tablet, added carrageenin, pectin, sodium carboxymethyl cellulose, tragacanth gum and hydroxypropyl emthylcellulose as additive, tablet will have good physical property and can control the release of diclofenac sodium preferably.Therefore utilizing the interaction of alginic acid and other polysaccharide, will be the effective ways that improve alginic acid gel rubber sustained-release performance.
Rhizoma amorphophalli glucomannan is a kind of macromole heteropolysaccharide that is coupled together with β-1,4 glycosidic bond by D-glucose and D-mannose that extracts from the natural product Rhizoma amorphophalli.The Rhizoma amorphophalli glucomannan neutral, water absorption is strong, absorbs water inflatable 80～100 times.After water-soluble, form thickness colloidal sol, have unique gelling, good rheological characteristic and thickening property.Rhizoma amorphophalli glucomannan is low grade fever, a low fat soluble polysaccharide representative in the dietary fiber, in gastrointestinal, can not decompose be utilized by the human consumption enzyme, and only part digestion in large intestine, it is cheap to compare wide material sources such as pectin.Modern medicine study shows that Rhizoma amorphophalli glucomannan and oligosaccharide thereof have prevention and effects such as treatment diabetes and cardiovascular disease to human body.Mainly Rhizoma amorphophalli glucomannan and oligosaccharide thereof are used as food primary raw materials or health promoting product both at home and abroad at present, Rhizoma amorphophalli glucomannan is also less as slow releasing carrier of medication.
Summary of the invention
The object of the present invention is to provide a kind of Rhizoma amorphophalli glucomannan-calcium alginate microsphere and preparation method.The microsphere of this technology preparation is used for medicine carrying, has the advantages that to improve controlled drug release and drug effect power, and its preparation process is simple.
The present invention is realized by following technical proposals, Rhizoma amorphophalli glucomannan-the calcium alginate microsphere that is used for medicine carrying, it is characterized in that, microspherulite diameter is less than 3mm, this microsphere is single nuclear structure, its material is the complex that Rhizoma amorphophalli glucomannan and calcium alginate are formed, and the weight ratio of Rhizoma amorphophalli glucomannan and calcium alginate is 1: 2-1: 9; Perhaps this microsphere is hud typed, its nuclear material is the complex that Rhizoma amorphophalli glucomannan and calcium alginate are formed, the weight ratio of Rhizoma amorphophalli glucomannan and calcium alginate is 1: 2-1: 9, and its shell material is chitin-alginic acid calcium polyelectrolyte film, wherein chitosan molecule amount 20-150 ten thousand.
The preparation method of above-mentioned microsphere is characterized in that comprising following process:
(1) configuration Rhizoma amorphophalli glucomannan-sodium alginate mixing water colloidal sol, the weight ratio of Rhizoma amorphophalli glucomannan and sodium alginate is 1: 2-1: 8, sodium alginate content is 1-4%, this mixed sols pH=5-6;
(2), add 0.1-0.4MCaCl with the fine droplet form with above-mentioned Rhizoma amorphophalli glucomannan-sodium alginate mixing water colloidal sol
2In the aqueous solution, behind the gentle agitation 15-60min, filter, after the washing of gained round, 25-50 ℃ of drying obtains Rhizoma amorphophalli glucomannan-calcium alginate microsphere; Perhaps, add chitosan-CaCl with the fine droplet form with Rhizoma amorphophalli glucomannan-sodium alginate mixing water colloidal sol
2In the aqueous solution, chitosan molecular weight 20-150 ten thousand in the solution, CaCl
2Concentration is 0.1-0.4M, filters, and after the washing of gained round, 25-50 ℃ of drying obtains Rhizoma amorphophalli glucomannan-calcium alginate-chitosan microball.
In above-mentioned microsphere preparation process, in Rhizoma amorphophalli glucomannan-sodium alginate mixing water colloidal sol, according to dosage add medicine, just can obtain the medicament slow-release microsphere of Rhizoma amorphophalli glucomannan-calcium alginate, or obtain the medicament slow-release microsphere of Rhizoma amorphophalli glucomannan-calcium alginate-chitosan.
Advantage of the present invention, compare with existing calcium alginate-chitosan microball, its medicament slow release performance obviously improves, as carrying insulin microsphere, in simulated gastric fluid, to handle after 4 hours, microsphere is placed in the simulated intestinal fluid once more, insulin discharges from existing calcium alginate-chitosan microball, be 1 hour release time, and discharge from Rhizoma amorphophalli glucomannan-calcium alginate of the present invention-chitosan microball, is increased to 3 hours release time; In addition, can be by changing preparation conditions such as content of konjak glucomannan, gel ion concentration, chitosan molecule amount and chitosan concentration, can regulate the slow release effect of microsphere easily and in gastrointestinal controlled release ability; Microsphere cost of the present invention is low, and preparation technology is simple, and mild condition all is fit to the embedding controlled release from the protide active medicine to the hydrophobicity synthetic drug, is suitable for large-scale production.
Description of drawings
Fig. 1 is the hygrometric state Rhizoma amorphophalli glucomannan-calcium alginate microsphere photo of the present invention's preparation.
Fig. 2 is the infrared spectrum of five kinds of unlike material microspheres.Among the figure: a is the infrared curve of calcium alginate microsphere; B is the infrared curve of calcium alginate-chitosan microball; C is the infrared curve of Rhizoma amorphophalli glucomannan-calcium alginate microsphere; D is the infrared curve of Rhizoma amorphophalli glucomannan-calcium alginate-chitosan microball; E is the infrared curve of Rhizoma amorphophalli glucomannan.
Fig. 3 is a section electromicroscopic photograph after calcium alginate-chitosan microball lyophilization.
Fig. 4 for the Rhizoma amorphophalli glucomannan-calcium alginate-chitosan microball lyophilization of the present invention preparation after the section electromicroscopic photograph.
Fig. 5 does not cover chitosan film for two kinds and carries the bovine serum albumin microsphere, in simulated gastric fluid, handles after 4 hours, and the releasing curve diagram of bovine serum albumin in simulated intestinal fluid, among the figure: ■ is that bovine serum albumin is from the calcium alginate microsphere release profiles; ● for bovine serum albumin from calcium alginate-Rhizoma amorphophalli glucomannan microsphere release profiles.
Fig. 6 covers chitosan film for two kinds and carries insulin microsphere, in simulated gastric fluid, handles after 4 hours, and the releasing curve diagram of insulin in simulated intestinal fluid, among the figure: ■ is that insulin is from calcium alginate-chitosan microball release profiles; ● for insulin from calcium alginate-Rhizoma amorphophalli glucomannan-chitosan microball release profiles.
The specific embodiment
Example 1
The 2g sodium alginate is dissolved in the 100ml deionized water or 2g sodium alginate and 0.5g Rhizoma amorphophalli glucomannan are dissolved in the 100ml deionized water, sodium alginate colloidal sol or mixed sols are splashed in the calcium chloride solution that concentration is 0.2M with the fine droplet form, gel 30 minutes, filtration washing can obtain calcium alginate microsphere or smooth surface, particle diameter evenly and the good Rhizoma amorphophalli glucomannan-calcium alginate microsphere (Fig. 1) of sphericity.By Rhizoma amorphophalli glucomannan-calcium alginate microsphere infrared absorption curve, can find that owing to faint hydrogen bond and electrostatic interaction between alginic acid and Rhizoma amorphophalli glucomannan, some absworption peaks disappear or some new absworption peaks (Fig. 2) occurred in Rhizoma amorphophalli glucomannan-calcium alginate microsphere external curve.
Example 2
2g sodium alginate and 0.5g Rhizoma amorphophalli glucomannan are dissolved in the 100ml deionized water, and mixed sols is splashed into 0.2M CaCl with the fine droplet form
2In the aqueous solution or CaCl
2Concentration is that 0.2M, chitosan concentration are that 0.5% (w/v), chitosan molecule amount are 8.55 * 10
6The chitosan calcium chloride solution in, gel 30 minutes, filtration washing can obtain calcium alginate-chitosan microball or have the Rhizoma amorphophalli glucomannan-calcium alginate-chitosan microball of higher-strength and good controlled release properties.From the infrared absorption curve (Fig. 2) of Rhizoma amorphophalli glucomannan-calcium alginate-chitosan microball, a little less than most absworption peak all became, this mainly was because the multiple interaction between alginic acid, Rhizoma amorphophalli glucomannan and chitosan causes.Do not add Rhizoma amorphophalli glucomannan and the microsphere gel structure obviously different (Fig. 3, Fig. 4) of adding Rhizoma amorphophalli glucomannan in addition, this mainly is because the filling of Rhizoma amorphophalli glucomannan, and the multiple interaction between alginic acid, Rhizoma amorphophalli glucomannan and chitosan causes.
Example 3
2g sodium alginate and 0.5g Rhizoma amorphophalli glucomannan are dissolved in the 100ml deionized water, mixed sols is splashed into CaCl with the fine droplet form
2Concentration is that 0.2M, chitosan concentration are that 0.25% (w/v), molecular weight are 5.87 * 10
6The chitosan calcium chloride solution in, gel 30 minutes, filtration washing can obtain covering the less Rhizoma amorphophalli glucomannan-calcium alginate of chitosan molecule amount-chitosan microball.
Example 4
Preparation process according to microsphere in the example 1, in sodium alginate colloidal sol and Rhizoma amorphophalli glucomannan-sodium alginate mixed sols, add bovine serum albumin (bovine serum albumin content is 3mg/ml) preparation microsphere respectively, 25 ℃ of dryings can be carried the calcium alginate microsphere and the Rhizoma amorphophalli glucomannan-calcium alginate microsphere of bovine serum albumin.In simulated gastric fluid, handle 4h, the release rate of bovine serum albumin is respectively 21.7% and 9.6% in calcium alginate microsphere and the Rhizoma amorphophalli glucomannan-calcium alginate microsphere, shows that the interpolation Rhizoma amorphophalli glucomannan gets microsphere and can effectively reduce leakage and the inactivation of bovine serum albumin in simulated gastric fluid.Microsphere is placed in the simulated intestinal fluid once more, and Fig. 5 is seen in the release of bovine serum albumin.The system slow release effect that adds Rhizoma amorphophalli glucomannan as seen from the figure obviously strengthens, and bovine serum albumin was increased to 1 hour by 40 minutes release time.
Example 5
Preparation process according to microsphere in the example 2, in sodium alginate colloidal sol and Rhizoma amorphophalli glucomannan-sodium alginate mixed sols, add insulin (insulin content is 3mg/ml) preparation microsphere respectively, 25 ℃ of dryings can be carried the calcium alginate-chitosan microball and the Rhizoma amorphophalli glucomannan-calcium alginate-chitosan microball of insulin.In simulated gastric fluid, handle 4h, the release rate of insulin is respectively 6.2% and 14.6% in calcium alginate-chitosan microball and Rhizoma amorphophalli glucomannan-calcium alginate-chitosan microball, shows that covering chitosan can effectively reduce leakage and the inactivation of insulin in simulated gastric fluid.Microsphere is placed in the simulated intestinal fluid once more, and Fig. 6 is seen in the release of insulin.The system slow release effect that adds Rhizoma amorphophalli glucomannan as seen from the figure obviously strengthens, and insulin was increased to 3 hours by 1 hour release time.
Claims (3)
1. Rhizoma amorphophalli glucomannan-calcium alginate microsphere that is used for medicine carrying, it is characterized in that: microspherulite diameter is less than 3mm, this microsphere is single nuclear structure, and its material is the complex that Rhizoma amorphophalli glucomannan and calcium alginate are formed, and the weight ratio of Rhizoma amorphophalli glucomannan and calcium alginate is 1: 2-1: 9; Perhaps this microsphere is hud typed, its nuclear material is the complex that Rhizoma amorphophalli glucomannan and calcium alginate are formed, the weight ratio of Rhizoma amorphophalli glucomannan and calcium alginate is 1: 2-1: 9, and its shell material is chitin-alginic acid calcium polyelectrolyte film, wherein chitosan molecule amount 20-150 ten thousand.
2. method for preparing by the described microsphere of claim 1 is characterized in that comprising following process:
(1) configuration Rhizoma amorphophalli glucomannan-sodium alginate mixing water colloidal sol, the weight ratio of Rhizoma amorphophalli glucomannan and sodium alginate is 1: 2-1: 8, sodium alginate content is 1-4%, this mixed sols pH=5-6;
(2), add 0.1-0.4MCaCl with the fine droplet form with above-mentioned Rhizoma amorphophalli glucomannan-sodium alginate mixing water colloidal sol
2In the aqueous solution, behind the gentle agitation 15-60min, filter, after the washing of gained round, 25-50 ℃ of drying obtains Rhizoma amorphophalli glucomannan-calcium alginate microsphere; Perhaps, add chitosan-CaCl with the fine droplet form with Rhizoma amorphophalli glucomannan-sodium alginate mixing water colloidal sol
2In the aqueous solution, chitosan molecular weight 20-150 ten thousand in the solution, CaCl
2Concentration is 0.1-0.4M, filters, and after the washing of gained round, 25-50 ℃ of drying obtains Rhizoma amorphophalli glucomannan-calcium alginate-chitosan microball.
3. by claim 1 or by described microsphere of claim 2 or preparation method, it is characterized in that, in preparation process, to according to dosage add medicine in Rhizoma amorphophalli glucomannan-sodium alginate mixing water colloidal sol, just can obtain the medicament slow-release microsphere of Rhizoma amorphophalli glucomannan-calcium alginate, or obtain the medicament slow-release microsphere of Rhizoma amorphophalli glucomannan-calcium alginate-chitosan.
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| CN101889985A (en) * | 2010-07-08 | 2010-11-24 | 东华大学 | Medicament-carrying nano microspheres and preparation method thereof |
| CN102492178A (en) * | 2011-11-29 | 2012-06-13 | 中国科学院过程工程研究所 | Konjac glucomannan microballoon with uniform dimension and preparation method thereof |
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| CN101889985B (en) * | 2010-07-08 | 2011-11-23 | 东华大学 | Medicament-carrying nano microspheres and preparation method thereof |
| CN101889985A (en) * | 2010-07-08 | 2010-11-24 | 东华大学 | Medicament-carrying nano microspheres and preparation method thereof |
| CN102492178A (en) * | 2011-11-29 | 2012-06-13 | 中国科学院过程工程研究所 | Konjac glucomannan microballoon with uniform dimension and preparation method thereof |
| CN102492178B (en) * | 2011-11-29 | 2014-12-24 | 中国科学院过程工程研究所 | Konjac glucomannan microballoon with uniform dimension and preparation method thereof |
| CN102627779A (en) * | 2012-02-23 | 2012-08-08 | 宁波争光树脂有限公司 | Preparation method of konjac glucomannan gel microspheres |
| CN102627779B (en) * | 2012-02-23 | 2014-12-10 | 宁波争光树脂有限公司 | Preparation method of konjac glucomannan gel microspheres |
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| CN104758395B (en) * | 2015-03-09 | 2017-11-28 | 西北农林科技大学 | A kind of apple polyphenol capsule and preparation method thereof |
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