CN102935071A - Venlafaxine hydrochloride controlled-release pellet and preparation method thereof - Google Patents
Venlafaxine hydrochloride controlled-release pellet and preparation method thereof Download PDFInfo
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Abstract
The invention provides a venlafaxine hydrochloride controlled-release pellet and a preparation method thereof. The venlafaxine hydrochloride controlled-release pellet comprises a blank pellet core, a venlafaxine hydrochloride-containing layer and a controlled-release film, wherein the venlafaxine hydrochloride-containing layer comprises active components including venlafaxine hydrochloride and talcum powder which are in a weight ratio of 12:1-8:1, and the weight ratio of the venlafaxine hydrochloride to the blank pellet core is 4:10-8:10. The venlafaxine hydrochloride controlled-release pellet is prepared by adopting a fluidized bed bottom-spraying venlafaxine hydrochloride applying mode; by using 75 percent alcohol as a solvent, the viscosity of the venlafaxine hydrochloride in a water solution is remarkably lowered, the venlafaxine hydrochloride applying speed is increased; and the prepared venlafaxine hydrochloride containing pellet adopts a bottom-spraying coating process, thus the problem of static electricity generated because of the adoption of the pure organic solvent is overcome; the application process and the wrapping process can be continuously operated in the same device, thus the production efficiency is increased and the production cost is lowered; and no toxic organic solvent is adopted in the whole process, thus the venlafaxine hydrochloride controlled-release pellet is environmental-friendly and is good in stability, and almost no broken pellets or dust is produced.
Description
Technical field
The invention belongs to field of medicaments, be specifically related to a kind of venlafaxine hydrochloride sustained-release pellet preparations and preparation method thereof.
Background technology
Depression is a kind of common mood disorders, can be caused by a variety of causes, and is low as main clinical characteristics take remarkable and lasting mental state, and mental state is low unbecoming with its situation, and suicidal thought and behavior can appear in severe patient.Majority of cases has the repeatedly tendency of outbreak, and the great majority that at every turn show effect can be alleviated, and part can have residual symptoms or transfer to chronic.
Venlafaxine is a kind of brand-new antidepressants.Chemical name is (R/S)-1-[2-(dimethylamine)-1-(4-anisyl) ethyl] Hexalin, venlafaxine is to strengthen its neurotransmitter activity in the central nervous system to the antidepressant mechanism of human body.Preclinical study shows that venlafaxine and major metabolite O-DMV (ODV) thereof are the potent inhibitors of 5-hydroxy tryptamine and norepinephrine reuptake.Venlafaxine also has slight inhibitory action to the picked-up of dopamine.The zooscopy demonstration only after giving tricyclic antidepressant for a long time, can reduce beta-adrenergic reactivity.Yet behind single or the long-term taking venlafaxine, venlafaxine and O-DMV can both reduce beta-adrenergic reactivity.Venlafaxine is similar to the inhibitory action of neurotransmitter re-uptake with O-DMV.
VENLAFAXINE HCL is a kind of novel antidepressant, has instant effect, better tolerance, the all good distinguishing features of short-term and long-term treatment effect, but there be short (about 5 ± 2 hours), client need frequent drug administration (2-3 times/day) of half-life in the venlafaxine of ordinary preparation, and the problem such as side effect is larger.After taking the venlafaxine conventional tablet of therapeutic dose, medicine is dissolving rapidly, causing after the administration soon, the blood drug level of active component venlafaxine raises rapidly, reactive compound is by metabolism or drain after several hours, blood drug level descends rapidly, after the administration about 12 hours, blood drug level has dropped to the level that is not enough to play therapeutical effect, therefore need multiple dosing, behind the every day multiple dosing, the most common side effect is exactly to feel sick, experimental results show that, with the patient that venlafaxine is treated, about 45% the patient symptom that occurs to feel sick, about 17% patient even vomit.
Summary of the invention
For the defects that exists in the prior art, the invention provides a kind of venlafaxine hydrochloride sustained-release pellet preparations and preparation method thereof, VENLAFAXINE HCL preparation of the present invention can the 24h sustained release, prolonged the time of drug action, make things convenient for patient's medication, therefore reduced patient's adverse reaction rate.
For achieving the above object, the present invention adopts following technical proposals to be achieved:
A kind of venlafaxine hydrochloride sustained-release pellet preparations, it comprises that celphere, uniform fold are in the VENLAFAXINE HCL medicated layer on celphere surface, the uniform fold release membranes on the medicated layer surface, described medicated layer comprises active ingredient hydrochloric acid venlafaxine and Pulvis Talci, VENLAFAXINE HCL and talcous weight ratio are 12:1-8:1, VENLAFAXINE HCL and celphere weight ratio are 4:10-8:10, celphere and VENLAFAXINE HCL medicated layer form and contain pill, described release membranes comprises slow-release material, and release membranes is 4%-12% to containing the pill weightening finish.
To further improvement in the technical proposal: described celphere is selected from sucrose ball, microcrystalline Cellulose ball, starch ball or lactose ball, and particle size distribution is preferably 710-850 μ m between 500-1000 μ m.
To further improvement in the technical proposal: VENLAFAXINE HCL and talcous weight ratio are preferably 10:1.
To further improvement in the technical proposal: contain that VENLAFAXINE HCL and celphere weight ratio are preferably 6:10 in the pill, release membranes is preferably 5%-8% to containing the pill weightening finish.
To further improvement in the technical proposal: described release membranes also comprises plasticizer and/or porogen.
To further improvement in the technical proposal: described slow-release material is selected from any one or more than one mixture in cellulose acetate, ethyl cellulose, cellulose propionate, Merlon, polyethylene, polyvinyl alcohol, the vinylacetate, preferred, ethyl.
To further improvement in the technical proposal: described plasticizer is selected from any one or more than one the mixture in phthalate, polyethylene glycols, glyceride, Oleum Ricini, succinate, ethanedioic acid ester, the tartrate, preferred Oleum Ricini; The weight ratio of slow-release material and plasticizer is selected from 8:1-13:1, preferred 10:1.
To further improvement in the technical proposal: described porogen is selected from the mixture of polyethylene glycols, hypromellose, methylcellulose, polyacrylic resin class, citrate apoplexy due to endogenous wind any one or more than one, preferably especially strange s100 and HPMC E5; The weight ratio of slow-release material and porogen is selected from 5:1-18:1, preferred 10:1.
The present invention also provides the preparation method of described venlafaxine hydrochloride sustained-release pellet preparations, may further comprise the steps: a, be saturated solution or the supersaturation suspension of the ethanol-water solution preparation VENLAFAXINE HCL of 50%-95% with concentration, and in this solution, add Pulvis Talci, under stirring state with the pastille solution spray to celphere, make and contain pill, contain drug solns and comprise VENLAFAXINE HCL, Pulvis Talci and ethanol water, concrete spray parameters is: inlet temperature is 50-65 ℃, temperature of charge is 40-50 ℃, the feed flow rotating speed is 50rpm, the blower fan frequency is 25Hz, and atomizing pressure is 0.14Mpa; B, with described ethanol-water solution preparation sustained release coating liquid, it is sprayed to makes sustained-release pellet preparation on the pill containing that step a makes, design parameter is: inlet temperature is 45-55 ℃, temperature of charge is 35-45 ℃, the feed flow rotating speed is 65rpm, and the blower fan frequency is 25Hz, and atomizing pressure is 0.12Mpa.
To further improvement in the technical proposal: the ethanol-water solution among described step a, the b is preferably 75% alcoholic solution.
Compared with prior art, advantage of the present invention and good effect are: the venlafaxine hydrochloride sustained-release pellet preparations that the objective of the invention is to prepare Stable Release, the present invention adopts and sprays the prescription formula at the bottom of the fluid bed and be prepared for this reason, VENLAFAXINE HCL and Pulvis Talci are added in 75% alcoholic solution, significantly reduce the viscosity that VENLAFAXINE HCL exists in aqueous solution, improved medicine-feeding speed; The pill that contains that makes is still adopted end spray art for coating, and adopt 75% alcoholic solution as the coating material solvent, overcome and adopted simple organic solvent coating electrostatic problem; And medicine-feeding and art for coating can same equipment in continued operation, do not interrupt during production, obviously improved production efficiency, improve at least 85% productive rate, preferred productive rate is higher than 95%, and has reduced production cost; Do not adopt virose organic reagent in the whole technique, environmental protection, and good stability, broken ball and dust are few.
The present invention is prepared into once-a-day slow releasing capsule with VENLAFAXINE HCL, can greatly facilitate patient's medication, significantly reduces the incidence rate of untoward reaction, reduce gastrointestinal side effect, make blood drug level steady, effectively the persistent period is lasting, the individual variation impact is little, and safety is good, and patient compliance is good.
After reading the specific embodiment of the present invention by reference to the accompanying drawings, other characteristics of the present invention and advantage will become clearer.
Description of drawings
Fig. 1 is sustained-release pellet preparation and the release comparison diagram of Efexor XR in the pH1.0 medium that the embodiment of the invention makes.
Fig. 2 is sustained-release pellet preparation and the release comparison diagram of Efexor XR in the pH4.5 medium that the embodiment of the invention makes.
Fig. 3 is sustained-release pellet preparation and the release comparison diagram of Efexor XR in the pH6.8 medium that the embodiment of the invention makes.
Fig. 4 is sustained-release pellet preparation and the release comparison diagram of Efexor XR in water that the embodiment of the invention makes.
The specific embodiment
Below in conjunction with the drawings and specific embodiments technical scheme of the present invention is described in further detail.
Embodiment 1
Venlafaxine hydrochloride sustained-release micropill provided by the present invention is comprised of three parts: celphere, uniform fold are in the VENLAFAXINE HCL medicated layer on celphere surface and the uniform fold release membranes on the medicated layer surface.
1, the selection of the blank pill heart
Celphere can be selected from the acceptable ball cores of pharmacy such as sucrose ball, microcrystalline Cellulose ball, starch ball, lactose ball, particle size distribution all can be prepared qualified samples between 500-1000 μ m the time, the present invention finds that by great many of experiments working as celphere is the sucrose ball, and particle diameter is optimal choice at 710-850 μ m.By the RSD contrast test of release, optimum with proof 710-850 μ m particle diameter.
Table 1: particle diameter is on the impact of the release of sustained-release pellet preparation among the present invention
Can be known by table 1 and to find out that when celphere particle size distribution during at 710-850 μ m, sample is minimum at the RSD of each point of release, the homogeneity of sample room is better, and difference is less, and is more approaching with Efexor XR.
2, contain the preparation of pill
Spray drug layering at the bottom of the stable fluid bed is adopted in the preparation that contains pill.Contain drug solns and comprise active ingredient hydrochloric acid venlafaxine, Pulvis Talci and ethanol-water solution.VENLAFAXINE HCL and talcous weight ratio are 12:1-8:1, preferred 10:1.VENLAFAXINE HCL and celphere weight ratio are selected from 4:10-8:10, preferred 6:10.Ethanol-water solution is selected from the 95%-50% alcoholic solution, preferred 75% alcoholic solution, and the consumption of ethanol water is for can dissolve the minimum dosage of VENLAFAXINE HCL.The present invention finds that by great many of experiments the concrete technology parameter is: inlet temperature is 50-65 ℃, and temperature of charge is 40-50 ℃, and the feed flow rotating speed is 50rpm, and the blower fan frequency is 25Hz, and atomizing pressure is 0.14Mpa.Whole drug layering stability is high, and medicine-feeding speed is fast, and broken ball and dust are few, and it is high to contain the pill yield.
3, the preparation of slow release ball
The preparation of slow release ball is sprayed art for coating at the bottom of adopting stable fluid bed.Release membranes is comprised of slow-release material, plasticizer, porogen.Wherein slow-release material can be selected from any one or more than one mixture in cellulose acetate, ethyl cellulose, cellulose propionate, Merlon, polyethylene, polyvinyl alcohol, the vinylacetate, preferred, ethyl; Plasticizer can be selected from any one or more than one the mixture in phthalate, polyethylene glycols, glyceride, Oleum Ricini, succinate, ethanedioic acid ester, the tartrate, preferred Oleum Ricini; Porogen can be selected from the mixture of glycols, hypromellose, methylcellulose, polyacrylic resin class, citrate apoplexy due to endogenous wind any one or more than one, optimization polypropylene acid resin III or especially strange s100 or HPMC E5.Release membranes can be selected from 4%-12%, preferred 5%-8% to containing the pill weightening finish.The present invention finds that by great many of experiments the concrete technology parameter is: inlet temperature is 45-55 ℃, and temperature of charge is 35-45 ℃, and the feed flow rotating speed is 65rpm, and the blower fan frequency is 25Hz, and atomizing pressure is 0.12Mpa.Do not adopt virose organic reagent in the whole art for coating, environmental protection, and stability is high, and coating speed is fast, and broken ball and dust are few, and slow release pill yield is high.
The preparation technology of venlafaxine hydrochloride sustained-release micropill disclosed in this invention can produce in same fluid bed continuously, all need not interrupt between same process and the different process, and ultimate yield is no less than 85%, and preferred productive rate is higher than 95%.This technique has greatly improved production efficiency, has reduced production cost.
Embodiment 2
Present embodiment is described, and to contain the preparation process of pill specific as follows: the celphere of 3.1kg particle size distribution in 710-850 μ m added in the fluid bed, and 1.9kg VENLAFAXINE HCL, 190g Pulvis Talci be suspended in the 3.8kg75% alcoholic solution, adopt end pressure spray process with this suspension even spraying at the ball wicking surface.Fluid bed medicine-feeding major parameter record is as follows:
| Parameter | Numerical value |
| Inlet temperature | 55℃ |
| Temperature of charge | 45℃ |
| The feed flow rotating speed | 50rpm |
| The blower fan frequency | 25Hz |
| Atomizing pressure | 0.14Mpa |
In prescription, added an amount of Pulvis Talci, and adopted 75% alcoholic solution to replace distilled water as solvent, greatly reduced solution viscosity, make the medicine-feeding process continuously, fast, piller is without adhesion, is applicable to commercial production.Following table is the phenomenon contrast in the medicine-feeding process.
| Prescription | Pulvis Talci+75% ethanol | Pulvis Talci+distilled water | Distilled water |
| Phenomenon | Continuously, fast, without adhesion | Continuously, the utmost point at a slow speed, adhesion arranged | Be interrupted, the utmost point at a slow speed, adhesion is serious |
The preparation process of the described slow release ball of present embodiment is specific as follows: with 250g EC (45 centipoise), 25g especially strange s100,25g Oleum Ricini be dissolved in the 6.25kg75% alcoholic solution, and by pressure spray process at the bottom of the fluid bed coating solution is sprayed to the described 5kg that is prepared into and contains the pill surface and make described sustained-release pellet preparation.Fluidized bed coating major parameter record is as follows:
| Parameter | Numerical value |
| Inlet temperature | 50℃ |
| Temperature of charge | 40℃ |
| The feed flow rotating speed | 65rpm |
| The blower fan frequency | 25Hz |
| Atomizing pressure | 0.12Mpa |
Embodiment 3
Contain the preparation of pill with embodiment 2.
The preparation process of the described slow release ball of present embodiment is specific as follows: 250g EC (45 centipoise), 12.5g polyacrylic resin III, 12.5g HPMC E5,25g Oleum Ricini are dissolved in the 6.25kg75% alcoholic solution, and by pressure spray process at the bottom of the fluid bed coating solution are sprayed to 5kg that embodiment 1 is prepared into and contain the pill surface and make described sustained-release pellet preparation.Fluidized bed coating major parameter record is as follows:
| Parameter | Numerical value |
| Inlet temperature | 50℃ |
| Temperature of charge | 40℃ |
| The feed flow rotating speed | 65rpm |
| The blower fan frequency | 25Hz |
| Atomizing pressure | 0.12Mpa |
Embodiment 4
Contain the preparation of pill with embodiment 2.
The preparation process of the described slow release ball of present embodiment is specific as follows: 250g EC (45 centipoise), 25gHPMCE5,25g Oleum Ricini are dissolved in the 6.25kg75% alcoholic solution, and by pressure spray process at the bottom of the fluid bed coating solution are sprayed to 5kg that embodiment 1 is prepared into and contain the pill surface and make described sustained-release pellet preparation.Fluidized bed coating major parameter record is as follows:
| Parameter | Numerical value |
| Inlet temperature | 50℃ |
| Temperature of charge | 40℃ |
| The feed flow rotating speed | 65rpm |
| The blower fan frequency | 25Hz |
| Atomizing pressure | 0.12Mpa |
Embodiment 5
In the 1# capsule shells, the release in pH1.0, pH4.5, pH6.8 and water and formerly grind the medicine Efexor XR relatively is shown in result following Fig. 1-4 with example 2,3,4 prepared slow-release micro-pill fills.
Can be found out that by Fig. 1-4 by the release behavior of sustained-release micro-pill capsules in 4 kinds of different dissolution mediums quite similar to Efexor XR (national regulation f2 can judge similar greater than 50) of embodiment 2-4 method preparation, f2 is all greater than 85; Release behavior is consistent with Efexor XR in water, and f2 is greater than 92.
In embodiment 2,3,4, adopt 75% ethanol of asepsis environment-protecting as the solvent of slow-release material, to replace poisonous organic reagent such as acetone, dichloromethane etc.And 25% moisture is arranged in 75% ethanol, can significantly regulate humidity in the fluid bed, greatly reduce a large amount of static that slow-release pill produces in the fluidisation friction process, solved the problem that normally to produce because of electrostatic interaction.
The organic solvent residual data see the following form:
| Residual organic solvent title | Ethanol (unique) |
| Determination of Residual Organic Solvents % | 0.0012-0.0023 |
| Residual ethanol standard % | ≤0.5 |
Following table is the phenomenon contrast in the coating process:
Above embodiment is only in order to illustrating technical scheme of the present invention, but not limits it; Although with reference to previous embodiment the present invention is had been described in detail, for the person of ordinary skill of the art, still can make amendment to the technical scheme that previous embodiment is put down in writing, perhaps part technical characterictic wherein is equal to replacement; And these modifications or replacement do not make the essence of appropriate technical solution break away from the spirit and scope of the present invention's technical scheme required for protection.
Claims (10)
1. venlafaxine hydrochloride sustained-release pellet preparations, it is characterized in that it comprises that celphere, uniform fold are in the VENLAFAXINE HCL medicated layer on celphere surface, the uniform fold release membranes on the medicated layer surface, described medicated layer comprises active ingredient hydrochloric acid venlafaxine and Pulvis Talci, VENLAFAXINE HCL and talcous weight ratio are 12:1-8:1, VENLAFAXINE HCL and celphere weight ratio are 4:10-8:10, celphere and VENLAFAXINE HCL medicated layer form and contain pill, described release membranes comprises slow-release material, and release membranes is 4%-12% to containing the pill weightening finish.
2. a kind of venlafaxine hydrochloride sustained-release pellet preparations according to claim 1, it is characterized in that: described celphere is selected from sucrose ball, microcrystalline Cellulose ball, starch ball or lactose ball, and particle size distribution is preferably 710-850 μ m between 500-1000 μ m.
3. a kind of venlafaxine hydrochloride sustained-release pellet preparations according to claim 1, it is characterized in that: VENLAFAXINE HCL and talcous weight ratio are preferably 10:1.
4. a kind of venlafaxine hydrochloride sustained-release pellet preparations according to claim 3 is characterized in that: contain that VENLAFAXINE HCL and celphere weight ratio are preferably 6:10 in the pill, release membranes is preferably 5%-8% to containing the pill weightening finish.
5. a kind of venlafaxine hydrochloride sustained-release pellet preparations according to claim 1, it is characterized in that: described release membranes also comprises plasticizer and/or porogen.
6. a kind of venlafaxine hydrochloride sustained-release pellet preparations according to claim 1, it is characterized in that: described slow-release material is selected from any one or more than one mixture in cellulose acetate, ethyl cellulose, cellulose propionate, Merlon, polyethylene, polyvinyl alcohol, the vinylacetate, preferred, ethyl.
7. a kind of venlafaxine hydrochloride sustained-release pellet preparations according to claim 5, it is characterized in that: described plasticizer is selected from any one or more than one the mixture in phthalate, polyethylene glycols, glyceride, Oleum Ricini, succinate, ethanedioic acid ester, the tartrate, preferred Oleum Ricini; The weight ratio of slow-release material and plasticizer is selected from 8:1-13:1, preferred 10:1.
8. a kind of venlafaxine hydrochloride sustained-release pellet preparations according to claim 5, it is characterized in that: described porogen is selected from the mixture of polyethylene glycols, hypromellose, methylcellulose, polyacrylic resin class, citrate apoplexy due to endogenous wind any one or more than one, preferably especially strange s100 and HPMC E5; The weight ratio of slow-release material and porogen is selected from 5:1-18:1, preferred 10:1.
9. the preparation method of each described venlafaxine hydrochloride sustained-release pellet preparations according to claim 1-8, it is characterized in that may further comprise the steps: a, be saturated solution or the supersaturation suspension of the ethanol-water solution preparation VENLAFAXINE HCL of 50%-95% with concentration, and in this solution, add Pulvis Talci, under stirring state with the pastille solution spray to celphere, make and contain pill, contain drug solns and comprise VENLAFAXINE HCL, Pulvis Talci and ethanol water, concrete spray parameters is: inlet temperature is 50-65 ℃, temperature of charge is 40-50 ℃, the feed flow rotating speed is 50rpm, the blower fan frequency is 25Hz, and atomizing pressure is 0.14Mpa; B, with described ethanol-water solution preparation sustained release coating liquid, it is sprayed to makes sustained-release pellet preparation on the pill containing that step a makes, design parameter is: inlet temperature is 45-55 ℃, temperature of charge is 35-45 ℃, the feed flow rotating speed is 65rpm, and the blower fan frequency is 25Hz, and atomizing pressure is 0.12Mpa.
10. the preparation method of venlafaxine hydrochloride sustained-release pellet preparations according to claim 9 is characterized in that, the ethanol-water solution among described step a, the b is preferably 75% alcoholic solution.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103893153A (en) * | 2014-04-17 | 2014-07-02 | 石家庄市华新药业有限责任公司 | Venlafaxine hydrochloride sustained-release capsule and preparation method of venlafaxine hydrochloride sustained-release capsule |
| CN105055330A (en) * | 2015-08-11 | 2015-11-18 | 杭州康恩贝制药有限公司 | Venlafaxine hydrochloride long-acting controlled-release pellets and preparation method thereof |
| CN106176679A (en) * | 2016-07-13 | 2016-12-07 | 河北龙海药业有限公司 | A kind of venlafaxine hydrochloride slow-release capsule and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004047718A2 (en) * | 2002-11-28 | 2004-06-10 | Themis Laboratories Private Limited | Process for manufacturing sustained release microbeads containing venlafaxine hci |
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2012
- 2012-11-29 CN CN201210496984.8A patent/CN102935071B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004047718A2 (en) * | 2002-11-28 | 2004-06-10 | Themis Laboratories Private Limited | Process for manufacturing sustained release microbeads containing venlafaxine hci |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103893153A (en) * | 2014-04-17 | 2014-07-02 | 石家庄市华新药业有限责任公司 | Venlafaxine hydrochloride sustained-release capsule and preparation method of venlafaxine hydrochloride sustained-release capsule |
| CN103893153B (en) * | 2014-04-17 | 2016-04-13 | 石家庄市华新药业有限责任公司 | A kind of venlafaxine hydrochloride slow-release capsule and preparation method thereof |
| CN105055330A (en) * | 2015-08-11 | 2015-11-18 | 杭州康恩贝制药有限公司 | Venlafaxine hydrochloride long-acting controlled-release pellets and preparation method thereof |
| CN105055330B (en) * | 2015-08-11 | 2019-01-25 | 杭州康恩贝制药有限公司 | A kind of VENLAFAXINE HCL long-acting slow-release pellet and preparation method thereof |
| CN106176679A (en) * | 2016-07-13 | 2016-12-07 | 河北龙海药业有限公司 | A kind of venlafaxine hydrochloride slow-release capsule and preparation method thereof |
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Effective date of registration: 20140603 Address after: 266101 Shandong Province, Qingdao city Laoshan District Four Keyuan Road No. 17 Applicant after: Qingdao Huanghai Pharmaceutical Co., Ltd. Applicant after: QINGDAO HUAHAI PHARMACEUTICAL RESEARCH INSTITUTE CO., LTD. Address before: 266101 Shandong Province, Qingdao city Laoshan District Four Keyuan Road No. 17 Applicant before: Qingdao Huanghai Pharmaceutical Co., Ltd. |
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Effective date of registration: 20171107 Address after: 266101 Shandong Province, Qingdao city Laoshan District Four Keyuan Road No. 17 Patentee after: Qingdao Huanghai Pharmaceutical Co., Ltd. Address before: 266101 Shandong Province, Qingdao city Laoshan District Four Keyuan Road No. 17 Co-patentee before: QINGDAO HUAHAI PHARMACEUTICAL RESEARCH INSTITUTE CO., LTD. Patentee before: Qingdao Huanghai Pharmaceutical Co., Ltd. |