CN103893150A - Penicillin V potassium micro-capsule and preparation method thereof - Google Patents
Penicillin V potassium micro-capsule and preparation method thereof Download PDFInfo
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- CN103893150A CN103893150A CN201410123276.9A CN201410123276A CN103893150A CN 103893150 A CN103893150 A CN 103893150A CN 201410123276 A CN201410123276 A CN 201410123276A CN 103893150 A CN103893150 A CN 103893150A
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Abstract
The invention discloses a penicillin V potassium micro-capsule and a preparation method thereof. The penicillin V potassium micro-capsule consists of a core material penicillin V potassium and a capsule wall material ethyecellulose. The preparation method comprises the following steps: 1) smashing and dissolving ethyecellulose in dichloromethane to obtain a solution a; 2) dissolving the smashed penicillin V potassium under stirring at a rotating speed of 100-500rpm in the solution a to obtain a solution b, and continuously stirring for 20-30 minutes; 3) controlling temperature of water and dispersing a surfactant in water to obtain a solution c; and 4) under the condition of stirring at a speed of 100-500rpm, adding the solution b into the solution c to form the penicillin V potassium micro-capsule, continuously stirring till dichloromethane is fully volatilized, filtering under reduced pressure, and washing the micro-capsule three times by using distilled water, and drying to obtain the penicillin V potassium micro-capsule. According to the invention, the micro-capsule is prepared by a drying-in-liquid method to eliminate harmful smell of penicillin V potassium so as to improve the compliance of the patient. The preparation process of the micro-capsule uses easily available and low-price raw materials, is low in production cost, simple in process operation, easy to operate and implement and high in yield.
Description
Technical field
The present invention relates to a kind of potassium v calcium microcapsule and preparation method thereof, belong to technical field of medicine.
Background technology
Potassium v calcium belongs to beta-lactam antibiotic, is applicable to light, grade and moderate infection due to penicillin sensitive strain, comprises tonsillitis due to streptococcus, pharyngolaryngitis, scarlet fever, erysipelas etc.; Bronchitis due to streptococcus pneumoniae, otitis media, sinusitis; And skin soft-tissue infection due to the responsive staphylococcus of penicillin etc.Potassium v calcium also can be used as the prophylactic of rheumatic fever recurrence and infective endocarditis, also can be used for spirochaete infection.Most gram positive bacterias, Grain-negative coccus, indivedual gram negative bacilli (as haemophilus), spirillum and actinomycetes are all had to antibacterial activity, but most aureus strains (>90%) comprise that staphylococcus aureus and coagulase negative staphylococcus can produce beta lactamase and make the hydrolysis of this product and inactivation, to the activity of most of sensitive strains compared with penicillin a little less than 2～5 times.To producing the bacterial strain of penicillinase without antibacterial action.The mechanism of action of this medicine is the synthetic of anti-bacteria cell wall, makes the antibacterial dissolving of breaking rapidly.
Both at home and abroad about the correlational study of potassium v calcium solid preparation is abundant in content.Patent documentation CN101138552A discloses a kind of preparation method of penicillium sp V potassium granular formulation, and this invention adopts dry granulation technique, has solved the problem of this product poor stability, and its granule of preparing can be preserved more than 2 years; It has adopted dry granulation technique, has preserved better the activity of potassium v calcium, thereby makes its invention drug effect more stable, and safety is better.
The former medicine of potassium v calcium has a kind of stronger abnormal smells from the patient, is not easy to be accepted by patient.Patent documentation CN101002767A discloses a kind of dispersion tablets of penicillin V potassium and preparation method thereof, in this invention by former potassium v calcium powder and supplementary product starch and alcoholic solution are mixed and make soft material, and then granulation, tabletting is made.While taking, dispersible tablet disintegrate in water forms suspension, can swallow, chews, contain and suck, greatly convenient for children, old man.In this patent documentation, be mainly by adding stevioside as correctives.
Microcapsule technology is to use certain technology and instrument, uses natural or synthetic macromolecular material that molecule is wrapped in to the technology in cyst membrane, and its particle radius is generally in micrometer range.Material in microcapsule is because tunica material intercepts, so external environment is less on the impact of capsule-core, thereby keeps stable.And there is the adverse drug of covering abnormal smells from the patient, improve medicine stability, weaken medicine to features such as gastrointestinal zests.Meanwhile, under proper condition, capsule-core medicine can discharge from capsule material again, by suitable means, can reach controlled-release effect.Microcapsule technology all has wide application prospects in many-sides such as biological medicines.
Summary of the invention
The object of the present invention is to provide a kind of potassium v calcium microcapsule, can obviously cover the special odor of the former medicine of potassium v calcium, roundness is good.
The preparation method that another object of the present invention is to provide a kind of described potassium v calcium microcapsule, 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 potassium v calcium microcapsule, this microcapsule is made up of capsule core material potassium v calcium and capsule material ethyl cellulose, and potassium v calcium and ethyl cellulose are dissolved in dichloromethane, mix and be added in the water that contains surfactant, be stirred to dichloromethane and volatilize completely, sucking filtration, is 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 respectively 80～100 orders.
The mass ratio of described surfactant and water is 1～3: 800.
Described surfactant is preferably sodium lauryl sulphate, dodecyl sodium sulfate, tween 30, tween 45 or polysorbate60.
Mass ratio between described potassium v calcium, dichloromethane, water is 1～3: 80～160: 500～800.
In the preparation process of this potassium v calcium microcapsule, in water, dry temperature is 20～50 DEG C, is stirred to dichloromethane at 20～50 DEG C and volatilizees completely, and mixing speed is 100～500rpm.
A preparation method for described potassium v calcium microcapsule, specifically comprises the following steps:
1) be dissolved in after ethyl cellulose is pulverized and in dichloromethane, obtain solution a;
2) under rotating speed 100～500rpm stirs, the potassium v calcium after pulverizing is dissolved in solution a, obtains solution b, continue to stir 20～30min;
3) by surfactant-dispersed in water, controlling the temperature of water is 20～50 DEG C, obtaining solution is solution c;
4) under rotating speed 100～500rpm stirs, solution b is added in solution c, forms potassium v calcium microcapsule, continue to be stirred to dichloromethane and volatilize completely, filtration under diminished pressure, microcapsule distilled water wash 3 times, are drying to obtain.
A preparation for described potassium v calcium microcapsule, said preparation type is the multiple dosage forms such as buccal tablet, capsule, tablet, granule, suspensoid or dry suspension.
The invention has the advantages that:
The present invention adopts intra-liquid desiccation method to prepare microcapsule, eliminates the bad smell of potassium v calcium, can be made into suspension solution oral, is particularly suitable for children taking, improves patient compliance.This microcapsule preparation technology raw material is easy to get, and cheap, production cost is low, and technological operation is simple, and enforcement easy to operate be beneficial to industry test and amplify, and yield is higher.The method reduces material consumption simultaneously, and methylene chloride can reclaim, and recycles technique environmental protection.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of embodiment 1 gained potassium v calcium microcapsule.
Fig. 2 is the differential scanning calorimetry curve of potassium v calcium in embodiment 1.
Fig. 3 is the differential scanning calorimetry curve of ethyl cellulose in embodiment 1.
Fig. 4 is the differential scanning calorimetry curve of embodiment 1 gained potassium v calcium microcapsule.
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 embodiment 1 gained potassium v calcium microcapsule.
Detailed description of the invention
The invention will be further described by the following examples, but the present invention is not limited to following examples.
Ethyl cellulose is crushed to 80 orders, and potassium v calcium is crushed to 80 orders, and precision takes potassium v calcium 1g, and ethyl cellulose 1g under agitation joins ethyl cellulose in 80mL dichloromethane and extremely dissolves completely, obtains solution a; It is to dissolve in the solution a under 400rpm stirs that potassium v calcium is added at rotating speed, obtains solution b, and solution b is to stir 20min under 400rpm at rotating speed.By 800mL water as for water-bath in beaker, control bath temperature at 35 DEG C, add Surfactant SDS 1g while stirring, obtain solution c, solution b is added in solution c, be stirred to dichloromethane with the rotating speed of 400rpm and volatilize completely, solid product filtration under diminished pressure, microcapsule distilled water wash 3 times, are drying to obtain drying solid powder 1.76g.Particle size range 50～700 μ m, mean diameter is 131.9 μ m, peak value particle diameter is 141.3 μ m.
Potassium v calcium raw material, ethyl cellulose, potassium v calcium ethyl cellulose microcapsule are carried out to differential thermal analysis, and analysis condition is: 10 DEG C/min of programming rate; Temperature range 25-400 DEG C; Nitrogen flow rate 60mL/min.Result is as shown in Fig. 2～4.Each sample shows not identical absworption peak, wherein potassium v calcium raw material is 90.7 DEG C, 225.5 DEG C, 258.3 DEG C, (seeing Fig. 2), ethyl cellulose 137.9 DEG C and 190.7 DEG C respectively due to dehydration with melt and produce absworption peak (seeing Fig. 3), potassium v calcium microcapsule has absworption peak (seeing Fig. 4) at 68.0 DEG C, 132.5 DEG C, 188.9 DEG C and 223.9 DEG C, and these 4 absworption peaks are different from 3 absworption peak positions of potassium v calcium raw material, prove that microcapsule forms.
The X-ray diffractogram of potassium v calcium raw material, ethyl cellulose, potassium v calcium-ethyl cellulose microcapsule is as shown in Fig. 5～7, adopt the German Brooker axs d8advance of company X-ray diffractometer, analysis condition is 40kv voltage in copper target, and scanning speed is 0.1sec/step.From X-ray diffractogram: potassium v calcium raw material has obvious crystal diffraction peak (seeing Fig. 5), ethyl cellulose does not have obvious crystal diffraction peak (seeing Fig. 6), potassium v calcium-ethyl cellulose microcapsule does not have obvious crystal diffraction peak (seeing Fig. 7), illustrate that potassium v calcium crystal disappears, potassium v calcium exists with the unformed form of one.
Ethyl cellulose is crushed to 80 orders, and potassium v calcium is crushed to 80 orders, and precision takes potassium v calcium 2g, and ethyl cellulose 1g under agitation joins ethyl cellulose in 80mL dichloromethane and extremely dissolves completely, obtains solution a; It is to dissolve in the solution a under 400rpm stirs that potassium v calcium is added at rotating speed, obtains solution b, and solution b is to stir 20min under 400rpm at rotating speed.By 500mL water as for water-bath in beaker, control bath temperature at 35 DEG C, add Surfactant SDS 1g while stirring, obtain solution c, solution b is added in solution c, be stirred to dichloromethane with the rotating speed of 400rpm and volatilize completely, solid product filtration under diminished pressure, microcapsule distilled water wash 3 times, are drying to obtain drying solid powder 1.82g.
Ethyl cellulose is crushed to 80 orders, and potassium v calcium is crushed to 80 orders, and precision takes potassium v calcium 2g, and ethyl cellulose 2g under agitation joins ethyl cellulose in 150mL dichloromethane and extremely dissolves completely, obtains solution a; It is to dissolve in the solution a under 400rpm stirs that potassium v calcium is added at rotating speed, obtains solution b, and solution b is to stir 20min under 400rpm at rotating speed.By 800mL water as for water-bath in beaker, control bath temperature at 35 DEG C, add Surfactant SDS 1g while stirring, obtain solution c, solution b is added in solution c, be stirred to dichloromethane with the rotating speed of 400rpm and volatilize completely, solid product filtration under diminished pressure, microcapsule distilled water wash 3 times, are 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, and ethyl cellulose 1g under agitation joins ethyl cellulose in 80mL dichloromethane and extremely dissolves completely, obtains solution a; It is to dissolve in the solution a under 400rpm stirs that potassium v calcium is added at rotating speed, obtains solution b, and solution b is to stir 20min under 400rpm at rotating speed.By 800mL water as for water-bath in beaker, control bath temperature at 35 DEG C, add Surfactant SDS 1.5g while stirring, obtain solution c, solution b is added in solution c, be stirred to dichloromethane with the rotating speed of 400rpm and volatilize completely, solid product filtration under diminished pressure, microcapsule distilled water wash 3 times, are 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, and ethyl cellulose 1g under agitation joins ethyl cellulose in 80mL dichloromethane and extremely dissolves completely, obtains solution a; It is to dissolve in the solution a under 400rpm stirs that potassium v calcium is added at rotating speed, obtains solution b, and solution b is to stir 30min under 400rpm at rotating speed.By 800mL water as for water-bath in beaker, control bath temperature at 40 DEG C, add Surfactant SDS 1g while stirring, obtain solution c, solution b is added in solution c, be stirred to dichloromethane with the rotating speed of 400rpm and volatilize completely, solid product filtration under diminished pressure, microcapsule distilled water wash 3 times, are 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, and ethyl cellulose 1g under agitation joins ethyl cellulose in 160mL dichloromethane and extremely dissolves completely, obtains solution a; It is to dissolve in the solution a under 400rpm stirs that potassium v calcium is added at rotating speed, obtains solution b, and solution b is to stir 30min under 400rpm at rotating speed.By 800mL water as for water-bath in beaker, control bath temperature at 35 DEG C, add Surfactant SDS 1g while stirring, obtain solution c, solution b is added in solution c, be stirred to dichloromethane with the rotating speed of 400rpm and volatilize completely, solid product filtration under diminished pressure, microcapsule distilled water wash 3 times, are drying to obtain drying solid powder 1.71g.
Claims (10)
1. a potassium v calcium microcapsule, is characterized in that, is made up of capsule core material potassium v calcium and capsule material ethyl cellulose, potassium v calcium and ethyl cellulose are dissolved in dichloromethane, mix and be added in the water that contains surfactant, be stirred to dichloromethane and volatilize completely, sucking filtration, is drying to obtain.
2. potassium v calcium microcapsule according to claim 1, is characterized in that, the mass ratio of described potassium v calcium and ethyl cellulose is 1～3: 1～2.
3. potassium v calcium microcapsule according to claim 1, is characterized in that, described potassium v calcium and ethyl cellulose are crushed to respectively 80～100 orders.
4. potassium v calcium microcapsule according to claim 1, is characterized in that, the mass ratio of described surfactant and water is 1～3: 800.
5. potassium v calcium microcapsule according to claim 1, is characterized in that, described surfactant is sodium lauryl sulphate, dodecyl sodium sulfate, tween 30, tween 45 or polysorbate60.
6. potassium v calcium microcapsule according to claim 1, is characterized in that, the mass ratio between described potassium v calcium, dichloromethane, water is 1～3: 80～160: 500～800.
7. potassium v calcium microcapsule according to claim 1, is characterized in that, is stirred to dichloromethane volatilizees completely at 20～50 DEG C.
8. potassium v calcium microcapsule according to claim 7, is characterized in that, mixing speed is 100～500rpm.
9. a preparation method for potassium v calcium microcapsule claimed in claim 1, is characterized in that, specifically comprises the following steps:
1) be dissolved in after ethyl cellulose is pulverized and in dichloromethane, obtain solution a;
2) under rotating speed 100～500rpm stirs, the potassium v calcium after pulverizing is dissolved in solution a, obtains solution b, continue to stir 20～30min;
3) by surfactant-dispersed in water, controlling the temperature of water is 20～50 DEG C, obtaining solution is solution c;
4) under rotating speed 100～500rpm stirs, solution b is added in solution c, forms potassium v calcium microcapsule, continue to be stirred to dichloromethane and volatilize completely, filtration under diminished pressure, microcapsule distilled water wash 3 times, are drying to obtain.
10. a preparation for the potassium v calcium microcapsule described in claim 1～8, is characterized in that, said preparation type is buccal tablet, capsule, tablet, granule, suspensoid or dry suspension.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104983715A (en) * | 2015-05-19 | 2015-10-21 | 北京联合大学 | Preparation method for berberine hydrochloride micro-capsules |
Citations (5)
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|---|---|---|---|---|
| US4443497A (en) * | 1981-01-19 | 1984-04-17 | Tanabe Seiyaku Co., Ltd. | Method of preparing microcapsules |
| JPH0955820A (en) * | 1995-08-10 | 1997-02-25 | Konica Corp | Image formation device |
| WO2004009058A1 (en) * | 2002-07-17 | 2004-01-29 | Eurand Pharmaceuticals Ltd | Process for the preparation of pharmaceutical microcapsules with enhanced taste-masking and high dissolution rate |
| 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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2014
- 2014-03-28 CN CN201410123276.9A patent/CN103893150B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4443497A (en) * | 1981-01-19 | 1984-04-17 | Tanabe Seiyaku Co., Ltd. | Method of preparing microcapsules |
| JPH0955820A (en) * | 1995-08-10 | 1997-02-25 | Konica Corp | Image formation device |
| WO2004009058A1 (en) * | 2002-07-17 | 2004-01-29 | Eurand Pharmaceuticals Ltd | Process for the preparation of pharmaceutical microcapsules with enhanced taste-masking and high dissolution rate |
| 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 |
|---|
| H. OYA ALPAR ET AL.: "The prolongation of the in vitro dissolution of a soluble drug (phenethicillin potassium) by microencapsulation with ethyl cellulose", 《I. PHARM. PHARMACOL.》, vol. 33, 31 December 1981 (1981-12-31) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104983715A (en) * | 2015-05-19 | 2015-10-21 | 北京联合大学 | Preparation method for berberine hydrochloride micro-capsules |
| CN104983715B (en) * | 2015-05-19 | 2017-11-17 | 北京联合大学 | A kind of preparation method of Berberine Hydrochloride Microcapsules |
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| CN103893150B (en) | 2016-06-08 |
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