CN1156500C - 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
- CN1156500C CN1156500C CNB011151080A CN01115108A CN1156500C CN 1156500 C CN1156500 C CN 1156500C CN B011151080 A CNB011151080 A CN B011151080A CN 01115108 A CN01115108 A CN 01115108A CN 1156500 C CN1156500 C CN 1156500C
- Authority
- CN
- China
- Prior art keywords
- methacrylic acid
- ethyl ester
- methyl methacrylate
- acid chlorination
- copolymer emulsion
- 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.)
- Expired - Fee Related
Links
Landscapes
- Medicinal Preparation (AREA)
Abstract
The present invention uses an emulsion polymerization method, and methyl methacrylate, ethyl acrylate and chloride trimethylamine ethyl ester of methacrylic acid are used as co-monomers for preparing control slow release type medicinal polymer film coating materials. The present invention uses an intermittent emulsion polymerization method, and the molar ratios of the water soluble monomer, namely the chloride trimethylamine ethyl ester of methacrylic acid, in the total amount of the monomers are respectively 10% and 5% for respectively preparing gastric disintegrable quick release type and gastric disintegrable slow release type polymer film coating materials. Obtained emulsion can be directly applied to a medicine coating using water as a solvent. Compared with the existing production technology steps, the production technological steps of the production technology of the present invention are greatly shortened, and environmental pollution extent is greatly reduced.
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 per-cent (%)
(1) methyl methacrylate 12.2-26.8
(2) ethyl propenoate 0-8.9
(3) methacrylic acid chlorination trimethylamine groups ethyl ester 3.1-5.6
(4) OP emulsifying agent 0.4-0.6
(5) sodium lauryl sulphate 0.2-0.3
(6) ammonium persulphate 0.1-0.2
(7) deionized water surplus
The production technique of methyl methacrylate/ethyl acrylate of the present invention/methacrylic acid chlorination trimethylamine groups ethyl ester copolymer emulsion:
With polyoxyethylene nonylphenol ether (polyoxyethylene nonylphenol ether), sodium lauryl sulphate, methyl methacrylate, ethyl propenoate and deionized water are mixed in the reaction flask, be warming up to 70-90 ℃, quick stirring and emulsifying, disposable 2/3 the initiator ammonium persulfate that adds, insulation reaction 1h adds 1/3 remaining initiator again, insulation reaction 3h, cooling discharging obtain the stable polymer emulsion.
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, heat up 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
In 1 liter of reaction flask, 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, mix, quick stirring and emulsifying, heat up 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 per-cent (%)
(1) methyl methacrylate 12.2-26.8
(2) ethyl propenoate 0-8.9
(3) methacrylic acid chlorination trimethylamine groups ethyl ester 3.1-5.6
(4) polyoxyethylene nonylphenol ether emulsifying agent 0.4-0.6
(5) sodium lauryl sulphate 0.2-0.3
(6) ammonium persulphate 0.1-0.2
(7) 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, be warming up to 70-90 ℃, quick stirring and emulsifying, the initiator ammonium persulfate of disposable adding 2/3, insulation reaction 1h, add 1/3 remaining initiator again, insulation reaction 3h, cooling discharging obtain 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 second fat 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 CN1328069A (en) | 2001-12-26 |
| CN1156500C true 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) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| MXPA04010956A (en) * | 2003-01-30 | 2005-01-25 | Roehm Gmbh | Pharmaceutical dosage form and method for the production thereof. |
| 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 |
| 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 |
-
2001
- 2001-07-02 CN CNB011151080A patent/CN1156500C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1328069A (en) | 2001-12-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Chambon et al. | Facile synthesis of methacrylic ABC triblock copolymer vesicles by RAFT aqueous dispersion polymerization | |
| US6433061B1 (en) | Rheology modifying copolymer composition | |
| Zhang et al. | Well-defined amphiphilic block copolymers and nano-objects formed in situ via RAFT-mediated aqueous emulsion polymerization | |
| US5739210A (en) | Polymers comprising reversible hydrophobic functionalities | |
| Guinaudeau et al. | Facile access to poly (N-vinylpyrrolidone)-based double hydrophilic block copolymers by aqueous ambient RAFT/MADIX polymerization | |
| US20120164424A1 (en) | Cold Water Soluble Polyvinyl Alcohol/Alkyl Acrylate Copolymers and Films Thereof | |
| BRPI0610206B8 (en) | use of polymer blends for the production of coated pharmaceutical formulations, and mixed polymer-coated pharmaceutical formulation | |
| JPH10506422A (en) | Process for preparing aqueous solution of poly (N-vinyl-ε-caprolactam) and use thereof | |
| EP2181716A1 (en) | Process for producing coated preparation | |
| CA2839689A1 (en) | Coating composition suitable for pharmaceutical or nutraceutical dosage forms | |
| CA2839494A1 (en) | Coating composition suitable for pharmaceutical or nutraceutical dosage forms | |
| KR930017922A (en) | Process for preparing multistage polymer latex cement modifier | |
| CN1156500C (en) | Process for preparing coating material as coating film of gastric disintegrable water medicine | |
| Baskar et al. | Comblike polymers with octadecyl side chain and carboxyl functional sites: scope for efficient use in miniemulsion polymerization | |
| CN109929083A (en) | A kind of segmented copolymer of Narrow Molecular Weight Distribution and preparation method thereof | |
| ZA200609155B (en) | Polymer particles containing active agents | |
| JP2013543026A (en) | Process for producing (meth) acrylate copolymers containing tertiary amino groups by free radical polymerization in solution | |
| JP2002179741A (en) | Water-soluble or water-dispersible (co)polymer of hydroxyalkyl (meth)acrylate, method of producing the same, and use of the same as coating agent, binder and/or film-forming excipient in pharmaceutical dosage form | |
| CN104761673A (en) | Carbomer and preparation method thereof | |
| CN1152067C (en) | Aqueous high molecular film material for medicine coating | |
| CN102432737B (en) | Controlled-release enteric acrylic resin latex and preparation method thereof | |
| CN103041396A (en) | Enteric polyacrylic resin medicament film coating aqueous dispersion and preparation method thereof | |
| JP3091366B2 (en) | Vinyl acetylsalicylate-vinyl alcohol copolymer | |
| CN106008788B (en) | A kind of hypotonicity Sustained release coating materials and preparation method thereof | |
| CN107722168A (en) | A kind of preparation method of the medicinal EUDRAGIT aqueous copolymer dispersion of middle osmotic sustained release of low monomer residue |
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 |