CN103893150B - A kind of micro-capsule of potassium v calcium and its preparation method - Google Patents
A kind of micro-capsule of potassium v calcium and its preparation method Download PDFInfo
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- CN103893150B CN103893150B CN201410123276.9A CN201410123276A CN103893150B CN 103893150 B CN103893150 B CN 103893150B CN 201410123276 A CN201410123276 A CN 201410123276A CN 103893150 B CN103893150 B CN 103893150B
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Abstract
The present invention discloses a kind of micro-capsule of potassium v calcium and its preparation method. The micro-capsule of this potassium v calcium is made up of capsule core material potassium v calcium and capsule material ethyl cellulose. Its preparation method is: be dissolved in methylene dichloride to obtain solution a after 1) ethyl cellulose being pulverized; 2) under rotating speed 100��500rpm stirs, the potassium v calcium after pulverizing is dissolved in solution a, obtains solution b, continue stirring 20��30min; 3) control the temperature of water, by surfactant-dispersed in water, obtain solution c; 4) under the speed of 100��500rpm stirs, being added in solution c by solution b, form the micro-capsule of potassium v calcium, continue to be stirred to methylene dichloride and volatilize completely, filtration under diminished pressure, micro-capsule distilled water wash 3 times, is drying to obtain. The present invention adopts intra-liquid desiccation method to prepare micro-capsule, eliminates the unpleasant odor of potassium v calcium, it is to increase patient compliance. This micro-capsule preparation technology's raw material is easy to get, and cheap, production cost is low, and technological operation is simple, easily operates enforcement, and receipts rate is higher.
Description
Technical field
The present invention relates to a kind of micro-capsule of potassium v calcium and its preparation method, belong to technical field of medicine.
Background technology
Potassium v calcium belongs to ��-lactam antibitics, is applicable to light, the grade and moderate infection caused by penicillin-sensitive strains, comprises the tonsillitis caused by suis, pharyngolaryngitis, scarlet fever, erysipelas etc.; Bronchitis caused by streptococcus pneumoniae, otitis media, sinusitis paranasal sinusitis; And the skin soft-tissue infection etc. caused by penicillin-susceptible staphylococcus. Potassium v calcium also can be used as the prophylactic of rheumatic fever recurrence and infective endocarditis, it is possible to for spirochaete infection. Most gram positive organism, the blue negative cocci of leather, indivedual gram negative bacilli (such as hemophilus), spirochete and actinomycetes all there is anti-microbial activity, but most aureus strains (> 90%) comprise streptococcus aureus and coagulase negative staphylococcus can produce beta lactamase and makes the hydrolysis of these product and inactivation, weak compared with penicillin 2��5 times to the activity of most of sensitive strain. To produce penicillinase bacterial strain without anti-microbial effect. The mechanism of action of this medicine is the synthesis of anti-bacteria cell walls, and bacterium is broken rapidly dissolving.
Abundant in content about the correlative study of potassium v calcium solid preparation both at home and abroad.Patent documentation CN101138552A discloses the preparation method of a kind of mould V potassium granular formulation, and this invention adopts dry granulation technique, solves the problem of this product stability difference, and its granule prepared can preserve more than 2 years; Which employs dry granulation technique, save the activity of potassium v calcium better, thus make its invention drug effect more stable, security is better.
The former medicine of potassium v calcium has a kind of than stronger smell, it is not easy to accepted by patient. Patent documentation CN101002767A discloses a kind of dispersion tablets of penicillin V potassium and its preparation method, even makes softwood by former for potassium v calcium powder and supplementary product starch and ethanolic soln being mixed, and then make particle in this invention, and compressing tablet is made. When taking, dispersible tablet disintegration in water forms suspension, it is possible to swallows, chew, containing sucking, greatly convenient for children, old man. Mainly by adding stevioside as correctives in this patent documentation.
Microcapsule technology uses certain technique and apparatus, it may also be useful to the technology that molecule is wrapped in capsule film by macromolecular material that is natural or synthesis, and its particle radius is generally in micrometer range. Material in micro-capsule is owing to being intercepted by capsule material, so external environment is less on the impact of capsule core, thus keeps stable. And have and cover adverse drug smell, improve medicine stability, weaken medicine to features such as the pungencys of gi tract. Meanwhile, under proper condition, capsule core medicine can discharge from capsule material again, by suitable means, it is possible to reach controlled-release effect. Microcapsule technology all has wide application prospects in many-sides such as biological medicines.
Summary of the invention
It is an object of the invention to provide a kind of micro-capsule of potassium v calcium, it is possible to obviously covering the special odor of the former medicine of potassium v calcium, roundness is good.
Another object of the present invention is to provide the preparation method of a kind of micro-capsule of described potassium v calcium, raw material is easy to get, cheap, and production cost is low, and technological operation is simple.
For achieving the above object, the present invention is by the following technical solutions:
A kind of micro-capsule of potassium v calcium, this micro-capsule is made up of capsule core material potassium v calcium and capsule material ethyl cellulose, is dissolved in methylene dichloride by potassium v calcium and ethyl cellulose, mixed even it is added in the water containing tensio-active agent, it is stirred to methylene dichloride to volatilize completely, takes out filter, be drying to obtain.
Wherein, the mass ratio of described potassium v calcium and ethyl cellulose is 1��3: 1��2.
Described potassium v calcium and ethyl cellulose are crushed to 80��100 orders respectively.
The mass ratio of described tensio-active agent and water is 1��3: 800.
Described tensio-active agent is preferably sodium lauryl sulphate, sodium laurylsulfonate, tween 30, tween 45 or polysorbate60.
Mass ratio between described potassium v calcium, methylene dichloride, water is 1��3: 80��160: 500��800.
In the preparation process of the micro-capsule of this potassium v calcium, temperature dry in water is 20��50 DEG C, is namely stirred to methylene dichloride at 20��50 DEG C and volatilizees completely, and stirring velocity is 100��500rpm.
A preparation method for the described micro-capsule of potassium v calcium, specifically comprises the following steps:
1) it is dissolved in methylene dichloride to obtain solution a after ethyl cellulose being pulverized;
2) under rotating speed 100��500rpm stirs, the potassium v calcium after pulverizing is dissolved in solution a, obtains solution b, continue stirring 20��30min;
3) by surfactant-dispersed in water, the temperature of control water is 20��50 DEG C, and obtaining solution is solution c;
4) under rotating speed 100��500rpm stirs, being added in solution c by solution b, form the micro-capsule of potassium v calcium, continue to be stirred to methylene dichloride and volatilize completely, filtration under diminished pressure, micro-capsule distilled water wash 3 times, is drying to obtain.
A preparation for the described micro-capsule of potassium v calcium, said preparation type is the multiple formulations such as buccal tablet, capsule, tablet, granule, suspensoid or dry suspensoid.
It is an advantage of the current invention that:
The present invention adopts intra-liquid desiccation method to prepare micro-capsule, eliminates the unpleasant odor of potassium v calcium, can be made into suspension solution oral, be particularly suitable for children taking, it is to increase patient compliance. This micro-capsule preparation technology's raw material is easy to get, and cheap, production cost is low, and technological operation is simple, easily operates enforcement, is beneficial to industry test and amplifies, and receipts rate is higher. The method reduces material consumption simultaneously, and methylene chloride can reclaim, and recycles, technique environmental protection.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the embodiment 1 micro-capsule of gained potassium v calcium.
Fig. 2 is the differential calorimetry curve of potassium v calcium in embodiment 1.
Fig. 3 is the differential calorimetry curve of ethyl cellulose in embodiment 1.
Fig. 4 is the differential calorimetry curve of the embodiment 1 micro-capsule of gained potassium v calcium.
Fig. 5 is the X-ray diffractogram of potassium v calcium in embodiment 1.
Fig. 6 is the X-ray diffractogram of ethyl cellulose in embodiment 1.
Fig. 7 is the X-ray diffractogram of the embodiment 1 micro-capsule of gained potassium v calcium.
Embodiment
The invention will be further described by the following examples, but the present invention is not limited to following examples.
Embodiment 1
Ethyl cellulose is crushed to 80 orders, and potassium v calcium is crushed to 80 orders, and precision takes potassium v calcium 1g, ethyl cellulose 1g, under agitation ethyl cellulose is joined in 80mL methylene dichloride and extremely dissolves completely, obtains solution a; Being added to by potassium v calcium at rotating speed is dissolve in the solution a under 400rpm stirs, and obtains solution b, and solution b stirs 20min under rotating speed is 400rpm. By 800mL water as water-bath in beaker, control bath temperature is at 35 DEG C, stir while add tensio-active agent sodium lauryl sulphate 1g, obtain solution c, solution b is added in solution c, it is stirred to methylene dichloride with the rotating speed of 400rpm and volatilizees completely, solid product filtration under diminished pressure, micro-capsule distilled water wash 3 times, is drying to obtain drying solid powder 1.76g. Particle size range 50��700 ��m, median size is 131.9 ��m, and peak value particle diameter is 141.3 ��m.
Potassium v calcium raw material, ethyl cellulose, the micro-capsule of potassium v calcium ethyl cellulose are carried out differential thermal analysis, and analysis condition is: heat-up rate 10 DEG C/min; Temperature range 25-400 DEG C; Nitrogen flow rate 60mL/min. Result is as shown in figs. 2 to 4. The absorption peak that each sample display is not identical, wherein potassium v calcium raw material is 90.7 DEG C, 225.5 DEG C, 258.3 DEG C, (see Fig. 2), ethyl cellulose 137.9 DEG C and 190.7 DEG C respectively due to dehydration with melt and produce absorption peak (see Fig. 3), the micro-capsule of potassium v calcium has absorption peak (see Fig. 4) 68.0 DEG C, 132.5 DEG C, 188.9 DEG C and 223.9 DEG C, and these 4 absorption peaks are different from 3 absorption peak positions of potassium v calcium raw material, prove that micro-capsule is formed.
The X-ray diffractogram of potassium v calcium raw material, ethyl cellulose, the micro-capsule of potassium v calcium-ethyl cellulose is as shown in Fig. 5��7, adopt Bu Luke axs company of Germany d8advanceX x ray diffractometer x, analysis condition is 40kv voltage in copper target, and sweep velocity is 0.1sec/step.From X-ray diffractogram: potassium v calcium raw material has obvious crystalline diffraction peak (see Fig. 5), ethyl cellulose does not have obvious crystalline diffraction peak (see Fig. 6), the micro-capsule of potassium v calcium-ethyl cellulose does not have obvious crystalline diffraction peak (see Fig. 7), illustrating that potassium v calcium crystal disappears, potassium v calcium exists with a kind of form without sizing.
Embodiment 2
Ethyl cellulose is crushed to 80 orders, and potassium v calcium is crushed to 80 orders, and precision takes potassium v calcium 2g, ethyl cellulose 1g, under agitation ethyl cellulose is joined in 80mL methylene dichloride and extremely dissolves completely, obtains solution a; Being added to by potassium v calcium at rotating speed is dissolve in the solution a under 400rpm stirs, and obtains solution b, and solution b stirs 20min under rotating speed is 400rpm. By 500mL water as water-bath in beaker, control bath temperature is at 35 DEG C, stir while add tensio-active agent sodium lauryl sulphate 1g, obtain solution c, solution b is added in solution c, it is stirred to methylene dichloride with the rotating speed of 400rpm and volatilizees completely, solid product filtration under diminished pressure, micro-capsule distilled water wash 3 times, is drying to obtain drying solid powder 1.82g.
Embodiment 3
Ethyl cellulose is crushed to 80 orders, and potassium v calcium is crushed to 80 orders, and precision takes potassium v calcium 2g, ethyl cellulose 2g, under agitation ethyl cellulose is joined in 150mL methylene dichloride and extremely dissolves completely, obtains solution a; Being added to by potassium v calcium at rotating speed is dissolve in the solution a under 400rpm stirs, and obtains solution b, and solution b stirs 20min under rotating speed is 400rpm. By 800mL water as water-bath in beaker, control bath temperature is at 35 DEG C, stir while add tensio-active agent sodium lauryl sulphate 1g, obtain solution c, solution b is added in solution c, it is stirred to methylene dichloride with the rotating speed of 400rpm and volatilizees completely, solid product filtration under diminished pressure, micro-capsule distilled water wash 3 times, is drying to obtain drying solid powder 1.6g.
Embodiment 4
Ethyl cellulose is crushed to 80 orders, and potassium v calcium is crushed to 80 orders, and precision takes potassium v calcium 1g, ethyl cellulose 1g, under agitation ethyl cellulose is joined in 80mL methylene dichloride and extremely dissolves completely, obtains solution a; Being added to by potassium v calcium at rotating speed is dissolve in the solution a under 400rpm stirs, and obtains solution b, and solution b stirs 20min under rotating speed is 400rpm. By 800mL water as water-bath in beaker, control bath temperature is at 35 DEG C, stir while add tensio-active agent sodium lauryl sulphate 1.5g, obtain solution c, solution b is added in solution c, it is stirred to methylene dichloride with the rotating speed of 400rpm and volatilizees completely, solid product filtration under diminished pressure, micro-capsule distilled water wash 3 times, is drying to obtain drying solid powder 1.53g.
Embodiment 5
Ethyl cellulose is crushed to 80 orders, and potassium v calcium is crushed to 80 orders, and precision takes potassium v calcium 1g, ethyl cellulose 1g, under agitation ethyl cellulose is joined in 80mL methylene dichloride and extremely dissolves completely, obtains solution a; Being added to by potassium v calcium at rotating speed is dissolve in the solution a under 400rpm stirs, and obtains solution b, and solution b stirs 30min under rotating speed is 400rpm. By 800mL water as water-bath in beaker, control bath temperature is at 40 DEG C, stir while add tensio-active agent sodium lauryl sulphate 1g, obtain solution c, solution b is added in solution c, it is stirred to methylene dichloride with the rotating speed of 400rpm and volatilizees completely, solid product filtration under diminished pressure, micro-capsule distilled water wash 3 times, is drying to obtain drying solid powder 1.6g.
Embodiment 6
Ethyl cellulose is crushed to 80 orders, and potassium v calcium is crushed to 80 orders, and precision takes potassium v calcium 2g, ethyl cellulose 1g, under agitation ethyl cellulose is joined in 160mL methylene dichloride and extremely dissolves completely, obtains solution a; Being added to by potassium v calcium at rotating speed is dissolve in the solution a under 400rpm stirs, and obtains solution b, and solution b stirs 30min under rotating speed is 400rpm. By 800mL water as water-bath in beaker, control bath temperature is at 35 DEG C, stir while add tensio-active agent sodium lauryl sulphate 1g, obtain solution c, solution b is added in solution c, it is stirred to methylene dichloride with the rotating speed of 400rpm and volatilizees completely, solid product filtration under diminished pressure, micro-capsule distilled water wash 3 times, is drying to obtain drying solid powder 1.71g.
Claims (8)
1. the micro-capsule of potassium v calcium, it is characterised in that, it is made up of capsule core material potassium v calcium and capsule material ethyl cellulose, potassium v calcium and ethyl cellulose are dissolved in methylene dichloride, mixed even are added in the water containing tensio-active agent, be stirred to methylene dichloride and volatilize completely, take out filter, it is drying to obtain; The mass ratio of described potassium v calcium and ethyl cellulose is 1��3:1��2; Mass ratio between described potassium v calcium, methylene dichloride, water is 1��3:80��160:500��800; The mass ratio of described tensio-active agent and water is 1��3:800.
2. the micro-capsule of potassium v calcium according to claim 1, it is characterised in that, described potassium v calcium and ethyl cellulose are crushed to 80��100 orders respectively.
3. the micro-capsule of potassium v calcium according to claim 1, it is characterised in that, described tensio-active agent is sodium lauryl sulphate, sodium laurylsulfonate, tween 30, tween 45 or polysorbate60.
4. the micro-capsule of potassium v calcium according to claim 1, it is characterised in that, it is stirred to methylene dichloride at 20��50 DEG C and volatilizees completely.
5. the micro-capsule of potassium v calcium according to claim 4, it is characterised in that, stirring velocity is 100��500rpm.
6. the preparation method of the micro-capsule of potassium v calcium according to claim 1, it is characterised in that, specifically comprise the following steps:
1) it is dissolved in methylene dichloride to obtain solution a after ethyl cellulose being pulverized;
2) under rotating speed 100��500rpm stirs, the potassium v calcium after pulverizing is dissolved in solution a, obtains solution b, continue stirring 20��30min;
3) by surfactant-dispersed in water, the temperature of control water is 20��50 DEG C, and obtaining solution is solution c;
4) under rotating speed 100��500rpm stirs, being added in solution c by solution b, form the micro-capsule of potassium v calcium, continue to be stirred to methylene dichloride and volatilize completely, filtration under diminished pressure, micro-capsule distilled water wash 3 times, is drying to obtain.
7. the preparation of the micro-capsule of potassium v calcium according to any one of a claim 1��6, it is characterised in that, said preparation type is capsule, tablet, granule or suspensoid.
8. preparation according to claim 7, it is characterised in that, described tablet is buccal tablet, and described suspensoid is dry suspensoid.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4443497A (en) * | 1981-01-19 | 1984-04-17 | Tanabe Seiyaku Co., Ltd. | Method of preparing microcapsules |
| CN1961870A (en) * | 2006-12-01 | 2007-05-16 | 北京联合大学生物化学工程学院 | Method for preparing sustained releasing microcapsule of phenoxybenzamine hydrochloride and ethyl cellulose |
| CN102579401A (en) * | 2012-03-27 | 2012-07-18 | 山东省中医药研究院 | Gromwell pigment micro-capsules and preparation method thereof |
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| JPH0955820A (en) * | 1995-08-10 | 1997-02-25 | Konica Corp | Image formation device |
| EP1534251A1 (en) * | 2002-07-17 | 2005-06-01 | Eurand Pharmaceuticals Ltd. | Process for the preparation of pharmaceutical microcapsules with enhanced taste-masking and high dissolution rate |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4443497A (en) * | 1981-01-19 | 1984-04-17 | Tanabe Seiyaku Co., Ltd. | Method of preparing microcapsules |
| CN1961870A (en) * | 2006-12-01 | 2007-05-16 | 北京联合大学生物化学工程学院 | Method for preparing sustained releasing microcapsule of phenoxybenzamine hydrochloride and ethyl cellulose |
| CN102579401A (en) * | 2012-03-27 | 2012-07-18 | 山东省中医药研究院 | Gromwell pigment micro-capsules and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| The prolongation of the in vitro dissolution of a soluble drug (phenethicillin potassium) by microencapsulation with ethyl cellulose;H. OYA ALPAR et al.;《I. Pharm. Pharmacol.》;19811231;第33卷;第419-422页，尤其第419页摘要 * |
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