CN1328069A - Process for preparing coating material as coating film of gastric disintegrable water medicine - Google Patents
Process for preparing coating material as coating film of gastric disintegrable water medicine Download PDFInfo
- Publication number
- CN1328069A CN1328069A CN 01115108 CN01115108A CN1328069A CN 1328069 A CN1328069 A CN 1328069A CN 01115108 CN01115108 CN 01115108 CN 01115108 A CN01115108 A CN 01115108A CN 1328069 A CN1328069 A CN 1328069A
- Authority
- CN
- China
- Prior art keywords
- methacrylic acid
- ethyl ester
- acid chlorination
- trimethylamine groups
- methyl methacrylate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Medicinal Preparation (AREA)
Abstract
A coating material for the disintegrable-in-stomach medicine is prepared from methyl methacrylate, ethyl acrylate and chloro-trimethylamine ethyl methacrylate (10 mol% for quick release or 5 mol% for slow release) through copolymerization to obtain emulsion. Its advantages are simple preparing process and lower environmental pollution.
Description
The present invention relates to controlling slow release type medicine with the preparation method of thin film coating material, specifically about the polymerization process of methyl methacrylate, ethyl propenoate, methacrylic acid chlorination trimethylamine groups ethyl ester copolymer emulsion.
Drug coating is to prevent at present that medicine is subjected to the influence of light, heat, tide etc. and rotten or cover the adverse drug taste, prevents the main method of effective ingredient evaporable.Because the polymer coating material can form tough and tensile elastica as thin as a wafer at medicinal tablet or capsule surface, again can be at oral certain hour or certain position, especially dissolving or disintegration under certain pH value replaced the easy moisture absorption gradually, easily broken and needed the sugar coating material of thicker coating membrance.The thickness of general polymer coating membrance only is the 1-2% of traditional coating membrance, and the clothing film required time that therefore reaches desired thickness can descend significantly, drops to 1-2 hour by 8-9 hour.Wherein, acrylic polymers is the most frequently used thin film coating material.See S.T.P.Pharma.Science.1997,7[6], 403﹠amp; Acta Pharm.Technolog1996,32,146.
At present, controlling slow release type esters of acrylic acid pharmaceutical film coating material is generally the multipolymer of methyl methacrylate/ethyl acrylate/methacrylic acid chlorination trimethylamine groups ethyl ester, two kinds of products are arranged, a kind of functional monomer methacrylic acid chlorination trimethylamine groups ethyl ester 10% (mol ratio) that contain, a kind of methacrylic acid chlorination trimethylamine groups ethyl ester 5% (mol ratio) that contain, the former is for oozing type soon, the latter is for oozing type slowly, both can mix use, control the two different ratios, can obtain the pharmaceutical film coating material of different controlled release speed.
Early stage control release type esters of acrylic acid pharmaceutical film coating material is obtained by mass polymerization, be dissolved in and carry out drug coating in ethanol, Virahol, the acetone and other organic solvent, because the environmental pollution aspect is replaced by the aqueous coatings material gradually, its production technique is:
Prepare the polymer coating material with mass polymerization, after the pulverizing drying, with a kind of and immiscible organic solvent dissolution of water, be scattered in then in the water, extracting goes out organic solvent again, obtains water-based emulsion.This emulsion can be directly used in drug coating, makes no longer to use organic solvent in the dressing process, has reduced environmental pollution.But owing to still will use organic solvent when coating material is produced, fundamentally do not solve environmental pollution problems, and Production Flow Chart is long, the production cost height is difficult to apply, and is difficult to substitute cheap sugar coating material on the market.
The purpose of this invention is to provide a kind of method for preparing the aqueous pharmaceutical coating material fully without organic solvent, reduce production costs, fundamentally solve the purpose of problem of environmental pollution thereby reach.
The preparation method of methyl methacrylate/ethyl acrylate provided by the invention/methacrylic acid chlorination trimethylamine groups ethyl ester copolymer emulsion is characterized in that the component and the proportioning of copolymer emulsion:
Constituent mass percentage (%) (1) methyl methacrylate 12.2-26.8 (2) ethyl acrylate 0-8.9 (3) methacrylic acid chlorination trimethylamine groups ethyl ester 3.1-5.6 (4) methyl methacrylate 12.2-26.8 (5) ethyl acrylate 0-8.9 (6) methacrylic acid chlorination trimethylamine groups ethyl ester 3.1-5.6 (7) OP emulsifying agent 0.4-0.6 (8) lauryl sodium sulfate 0.2-0.3 (9) ammonium persulfate 0.1-0.2 (10) deionized water surplus
The production technique of methyl methacrylate/ethyl acrylate of the present invention/methacrylic acid chlorination trimethylamine groups ethyl ester copolymer emulsion:
Polyoxyethylene nonylphenol ether, sodium lauryl sulphate, methyl methacrylate, ethyl propenoate, methacrylic acid chlorination trimethylamine groups ethyl ester and deionized water are mixed in the reaction flask, heat up 70-90 ℃, quick stirring and emulsifying, the initiator ammonium persulfate of disposable adding 2/3, more than the insulation reaction 1h, add 1/3 remaining initiator again, more than the insulation reaction 3h, cooling discharging obtains the stable polymer emulsion.
Copolymer emulsion of the present invention is that solvent, ammonium persulphate are that initiator, OP and sodium lauryl sulphate are compound emulsifying agent with water, batchwise polymerization, functional monomer methacrylic acid chlorination trimethylamine groups ethyl ester mol ratio in monomer are 10% to make and ooze the type copolymer emulsion soon, and the mol ratio of functional monomer methacrylic acid chlorination trimethylamine groups ethyl ester in monomer is 5% to make and ooze the type copolymer emulsion slowly.
Key problem in technology of the present invention is the selection of emulsion polymerization technique.Because water-soluble monomer methacrylic acid chlorination trimethylamine groups ethyl ester is a quaternary ammonium salt in the comonomer, and general water-based emulsion salt tolerance is not strong, easily by the salt breakdown of emulsion, and the extent of polymerization of methacrylic acid chlorination trimethylamine groups ethyl ester is the most key in the initial reaction stage aqueous solution, degree and time that the control aqueous solution polymerization carries out, just the molecular weight of water-soluble oligopolymer and concentration are determining the success or failure of letex polymerization in the aqueous solution, it is suitable to control, this oligopolymer will become the co-emulsifier of follow-up letex polymerization, just can make stable emulsion.
The present invention prepares gastric disintegrable type aqueous pharmaceutical coating material-methyl methacrylate/ethyl acrylate/methacrylic acid chlorination trimethylamine groups ethyl ester copolymer emulsion with emulsion polymerisation process, and this emulsion can be directly used in the film coating of control release type medicine with traditional coated formula.Also available traditional spray-drying process is made pulvis, is used for water-based or oiliness controlled release drug film coating.
Embodiment example 1 stomach collapses and oozes type soon
In 1 liter of reaction flask, add 405.4g deionized water, methyl methacrylate 146.4g, the methacrylic acid chlorination trimethylamine groups ethyl ester aqueous solution (78% concentration) 43.1g, OP emulsifying agent 2.8g, sodium lauryl sulphate 1.4g, mix, quick stirring and emulsifying, be warming up to 80 ℃, add the 0.6g ammonium persulphate, behind the reaction 1h, add remaining 0.3g initiator, insulation reaction 3h, cooling discharge.Methacrylic acid chlorination trimethylamine groups ethyl ester mol ratio is 10% of a monomer total amount, oozes the type product soon for stomach collapses.Example 2 stomaches collapse and ooze type soon
In 1 liter of reaction flask, add 405.4g deionized water, methyl methacrylate 97.6g, ethyl propenoate 48.8g, methacrylic acid chlorination trimethylamine groups ethyl ester aqueous solution 43.1g, OP emulsifying agent 2.8g, sodium lauryl sulphate 1.4g, mix, quick stirring and emulsifying, be warming up to 80 ℃, add the 0.6g ammonium persulphate, behind the reaction 1h, add remaining 0.3g initiator, insulation reaction 3h, cooling discharge.Methacrylic acid chlorination trimethylamine groups ethyl ester mol ratio is 10% of a monomer total amount, oozes the type product soon for stomach collapses.Example 3 stomaches collapse and ooze type slowly
In 1 liter of reaction flask, add 409.4g deionized water, methyl methacrylate 161.4g, methacrylic acid chlorination trimethylamine groups ethyl ester aqueous solution 23.8g, OP emulsifying agent 2.8g, sodium lauryl sulphate 1.4g, mix, quick stirring and emulsifying, be warming up to 80 ℃, add the 0.8g ammonium persulphate, behind the reaction 1h, add remaining 0.4g initiator, insulation reaction 3h, cooling discharge.Methacrylic acid chlorination trimethylamine groups ethyl ester mol ratio is 5% of a monomer total amount, oozes the type product slowly for stomach collapses.Example 4 stomaches collapse and ooze type slowly and add 409.4g deionized water, methyl methacrylate 107.6g, ethyl propenoate 53.8g, methacrylic acid chlorination trimethylamine groups ethyl ester aqueous solution 23.8g, OP emulsifying agent 2.8g, sodium lauryl sulphate 1.4g in 1 liter of reaction flask, mix, quick stirring and emulsifying, be warming up to 80 ℃, add the 0.8g ammonium persulphate, behind the reaction 2h, add remaining 0.4g initiator, insulation reaction 3h, cooling discharge.Methacrylic acid chlorination trimethylamine groups ethyl ester mol ratio is 5% of a monomer total amount, oozes the type product slowly for stomach collapses.
The production technique of methyl methacrylate/ethyl acrylate of the present invention/methacrylic acid chlorination trimethylamine groups ethyl ester copolymer emulsion fully need not any organic solvent, more traditional production technique has shortened step greatly, and environmental pollution degree and production cost all descend greatly.
Claims (2)
1, the preparation method of coating material as coating film of gastric disintegrable water medicine methyl methacrylate/ethyl acrylate/methacrylic acid chlorination trimethylamine groups ethyl ester copolymer emulsion is characterized in that the component and the proportioning of copolymer emulsion:
Constituent mass percentage (%) (1) methyl methacrylate 12.2-26.8 (2) ethyl acrylate 0-8.9 (3) methacrylic acid chlorination trimethylamine groups ethyl ester 3.1-5.6 (4) methyl methacrylate 12.2-26.8 (5) ethyl acrylate 0-8.9 (6) methacrylic acid chlorination trimethylamine groups ethyl ester 3.1-5.6 (7) OP emulsifying agent 0.4-0.6 (8) lauryl sodium sulfate 0.2-0.3 (9) ammonium persulfate 0.1-0.2 (10) deionized water surplus
The production technique of methyl methacrylate/ethyl acrylate of the present invention/methacrylic acid chlorination trimethylamine groups ethyl ester copolymer emulsion:
Polyoxyethylene nonylphenol ether, sodium lauryl sulphate, methyl methacrylate, ethyl propenoate, methacrylic acid chlorination trimethylamine groups ethyl ester and deionized water are mixed in the reaction flask, heat up 70-90 ℃, quick stirring and emulsifying, the initiator ammonium persulfate of disposable adding 2/3, more than the insulation reaction 1h, add 1/3 remaining initiator again, more than the insulation reaction 3h, cooling discharging obtains the stable polymer emulsion.
2. the preparation method of copolymer emulsion according to claim 1, it is characterized in that: described functional monomer methacrylic acid chlorination trimethylamine groups ethyl ester mol ratio in monomer is 10% to make and ooze the type copolymer emulsion soon, and the mol ratio of functional monomer methacrylic acid chlorination trimethylamine groups ethyl ester in monomer is 5% to make and ooze the type copolymer emulsion slowly.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011151080A CN1156500C (en) | 2001-07-02 | 2001-07-02 | Process for preparing coating material as coating film of gastric disintegrable water medicine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011151080A CN1156500C (en) | 2001-07-02 | 2001-07-02 | Process for preparing coating material as coating film of gastric disintegrable water medicine |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1328069A true CN1328069A (en) | 2001-12-26 |
| CN1156500C CN1156500C (en) | 2004-07-07 |
Family
ID=4661695
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011151080A Expired - Fee Related CN1156500C (en) | 2001-07-02 | 2001-07-02 | Process for preparing coating material as coating film of gastric disintegrable water medicine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1156500C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1697649B (en) * | 2003-04-29 | 2010-05-12 | 罗姆两合公司 | Dosage form and method for producing the same |
| CN105482028A (en) * | 2015-12-26 | 2016-04-13 | 悦康药业集团安徽天然制药有限公司 | Preparation method of polymer |
| CN106432616A (en) * | 2016-11-08 | 2017-02-22 | 张建国 | Polymerizable emulsifier structure containing acrylic resin medicinal auxiliary material and preparation method thereof |
| CN111040070A (en) * | 2019-12-25 | 2020-04-21 | 悦康药业集团安徽天然制药有限公司 | Preparation method of ammonium polymethacrylate |
-
2001
- 2001-07-02 CN CNB011151080A patent/CN1156500C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1697649B (en) * | 2003-04-29 | 2010-05-12 | 罗姆两合公司 | Dosage form and method for producing the same |
| CN105482028A (en) * | 2015-12-26 | 2016-04-13 | 悦康药业集团安徽天然制药有限公司 | Preparation method of polymer |
| CN106432616A (en) * | 2016-11-08 | 2017-02-22 | 张建国 | Polymerizable emulsifier structure containing acrylic resin medicinal auxiliary material and preparation method thereof |
| CN106432616B (en) * | 2016-11-08 | 2019-05-03 | 张建国 | A kind of acrylic resin pharmaceutic adjuvant and preparation method thereof containing polymerisable emulsifier structure |
| CN111040070A (en) * | 2019-12-25 | 2020-04-21 | 悦康药业集团安徽天然制药有限公司 | Preparation method of ammonium polymethacrylate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1156500C (en) | 2004-07-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US6433061B1 (en) | Rheology modifying copolymer composition | |
| CN103608001B (en) | Be applicable to the coated composition of medicine or dietetic product dosage form | |
| JP3697157B2 (en) | Method for producing aqueous dispersion of latex particles having heterogeneous morphology, latex particles obtained by this method, dispersion, redispersible powder, | |
| CN101787231B (en) | Hydrophobic modified association type thickening agent and preparation method thereof | |
| US6998140B2 (en) | Dispersion comprising a non-ionic emulsifier | |
| US8349387B2 (en) | Method for production of coated preparations | |
| CA2839494C (en) | Coating composition suitable for pharmaceutical or nutraceutical dosage forms | |
| SK280487B6 (en) | Coating and binder compositions for pharmaceutical forms and pharmaceutical forms prepared therewith | |
| CN103403043A (en) | Cold water soluble polyvinyl alcohol/alkyl acrylate copolymers and films thereof | |
| SK106295A3 (en) | Thermoplastic for drug covers production, manufacturing process and use thereof | |
| CN101186666A (en) | Method for preparing polyvinylidene chloride and acrylic ester copolymerization latex | |
| JP2003529645A (en) | Polymerizable compounds and uses thereof | |
| JP4018363B2 (en) | Water-soluble or water-dispersible (co) polymers of hydroxyalkyl (meth) acrylates, processes for their preparation and their use as coatings, binders and / or film-forming excipients in pharmaceutical dosage forms | |
| CN110124059A (en) | A kind of preparation method being sustained bacteriostatic agent | |
| JPS63264687A (en) | Basic active component permeable contact pressure adhesive polymer material and its production | |
| JP2003506497A (en) | Temperature sensitive polymer | |
| US20070224274A1 (en) | Polymer Particles Containing Active Agents | |
| CN106279506B (en) | A kind of acrylate polymer emulsion and preparation method thereof | |
| CN1156500C (en) | Process for preparing coating material as coating film of gastric disintegrable water medicine | |
| JP2013543026A (en) | Process for producing (meth) acrylate copolymers containing tertiary amino groups by free radical polymerization in solution | |
| CN1152067C (en) | Aqueous high molecular film material for medicine coating | |
| CN102432737B (en) | Controlled-release enteric acrylic resin latex and preparation method thereof | |
| CN102167754A (en) | Active free radical polymerization method taking bithiaxanthene diol and derivatives thereof as initiator | |
| CN103041396A (en) | Enteric polyacrylic resin medicament film coating aqueous dispersion and preparation method thereof | |
| JP3091366B2 (en) | Vinyl acetylsalicylate-vinyl alcohol copolymer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |