CN102232921A - Technique for preparing rod-like sustained-release preparation by using blending-modified corn zein as skeleton material and preparation prepared by technique - Google Patents
Technique for preparing rod-like sustained-release preparation by using blending-modified corn zein as skeleton material and preparation prepared by technique Download PDFInfo
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- CN102232921A CN102232921A CN2011100963763A CN201110096376A CN102232921A CN 102232921 A CN102232921 A CN 102232921A CN 2011100963763 A CN2011100963763 A CN 2011100963763A CN 201110096376 A CN201110096376 A CN 201110096376A CN 102232921 A CN102232921 A CN 102232921A
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Abstract
The invention belongs to a technique for preparing rod-like sustained-release preparation by using blending-modified corn zein as a skeleton material and a preparation prepared by the technique, in particular to a method for preparing a biocompatible and environment-friendly rod-like sustained-release preparation. The method has the main technical characteristics that: corn zein, a blended modifying material, medicines and other active ingredients are mixed uniformly in solvent such as water and alcohol according to a certain ratio; the mixture is extruded into a mold by a mold filling mode to be formed into rod shape; the rod-like material is taken out and dried to form green rod; and the green rod is coated by a coating material such as ethylcellulose, cellulose acetate, chitosan and polycaprolactone, the coating is dried, and the preparation is obtained. The rod-like material has excellent zero or highchi release behavior, the release time of active ingredients such as the medicines can be adjusted from 10 hours to 6 months, and the rod-like material can be used in human oral preparations, sustained-release pesticides, sustained-release fertilizers and the like, which need sustained release of active ingredients. The technique is low in processing cost and can meet industrial production needs completely.
Description
Technical field
The invention belongs to medicine, agricultural and daily life field, can be used for the technology of preparing of the inside and outside slow releasing preparation of human body.
Background technology
China Food and Drug Admistraton (SFDA) unified the called after slow releasing preparation from 2006 with slow release and " controlled release " preparation.Slow releasing preparation is exactly that medicine or other active substances and appropriate carriers are made preparation by certain form, makes medicine or other active substance dosage by design, discharges with certain rate of release in the time range that requires.At field of medicaments, slow releasing preparation is compared with traditional administering mode, and medicinal slow release agent not only can reduce administration number of times, keep the concentration of blood Chinese medicine, but also reduces drug toxicity, improves the curative effect of medicine.Be usually used in methylcellulose, hypromellose, carboxymethyl cellulose, polyvinylpyrrolidone, carbomer, polymethacrylates, polyvinyl alcohol, silicone rubber, chitosan, alginate, ethylene-vinyl acetate copolymer or the like being arranged at present as what the slow releasing preparation material was used.
Zein is the hydrophobin in the corn, belongs to natural high molecular substance, has excellent biological compatibility and biological degradability, as a kind of Biodegradable material wide application prospect is arranged.Zein is at field of medicaments, in China always as the coating material of tablet, research ([1] Sun Qingshen as medicinal slow release formulation is arranged in recent years, Lin Zhixin, Liu Xinming, Deng. the exploration of zein microsphere preparation condition and release in vitro behavioral study [J]. HEILONGJIANG ANIMAL SCIENCE AND VETERINARY MEDICINE, 2005,10:13-15.[2] Wang Huajie, Wang Linsong, Wang Jinye. the preparation of zein-heparin microsphere and slow release [J]. science and technology and engineering, 2003,3 (6): 557-560.), produce lysozyme-Zein sustained-release micro-spheres (Qixin Zhong, Minfeng Jin as human supercritical methanol technologies such as Qixin Zhong, P.Michael Davidson and Svetlana Zivanovic, Food Chemistry, 2009,115 (2): 697-700); People such as S.K.Mehta make Zein sustained-release micro-spheres (S.K.Mehta with rifampicin under mild acid conditions, Gurpreet Kaur and Anil Verma, Fabrication of plant protein microspheres for encapsulation, stabilization and in vitro release of multiple anti-tuberculosis drugs, Colloids and Surfaces A:Physicochemical and Engineering Aspects, 2011,375 (1-3): 219-230).
Mostly existing slow release formulation is tablet or microsphere, as antidiabetic drug glibenclamide slow releasing tablet, contac sustained-release micro-spheres.The present invention proposes a kind of bar-shaped slow releasing preparation, and with the zein is stock, with hydrophilic or hydrophobic material co-blended modification with it, regulate the rate of release of active substance, thereby be prepared into a kind of new sustained release preparation, its advantage has: 1) bar-shaped specific surface area is bigger than tablet or microsphere, discharges comparatively abundant; 2) clavate can be as the microsphere sample easily with the inserts mixing but be easy to roll unlike microsphere and be deposited in or easily washed away by fluids such as rainwater, and this point in actual use highly significant; 3) excellent core zein water-swellable promotes the release of medicine by turgor pressure.By regulating the prescription and the preparation technology of coating prescription or excellent core, the present invention can realize the clavate slow releasing agent of medicine isoreactivity material from several hours to the several months, and this clavate slow releasing agent promptly can be used for the human body oral formulations and can be used for the usefulness that external any needs slowly discharge certain material again.
Summary of the invention
The object of the present invention is to provide a kind of new slow releasing preparation technology of preparing.Slow releasing preparation inanimate object toxicity of the present invention, cheap and easy to get, preparation is simple.
The object of the present invention is achieved like this:
1. be the clavate slow releasing agent of framework material with the zein blended modifier, the composition characteristic of its plain rod is:
Comprise that following component and each composition weight proportioning are:
Zein 20%～30%
Wherein blended modifier comprises one or more mixture in polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP), polyacrylic acid (PPA), Polyethylene Glycol (PEG), polyoxyethylene (PEO), tween, span, glycerol, oleic acid, the stearic acid;
Active substance comprises chemical medicine, Chinese medicine extract, spice, pigment, chemical fertilizer, pesticide;
According to 1 described be the preparation method of the plain rod of clavate slow releasing agent of framework material with the zein blended modifier, it is characterized in that:
Modified corn alcohol soluble protein and active matter pledge are blended in the alcohol solvent by weight ratio, stir and to make mix homogeneously, adopt injection molding that the mixture extruding is entered and form bar-shapedly in the mould, club is taken out dry plain rod.
3. be that the clavate slow releasing agent of framework material is characterized in that according to 1 and 2 with the zein blended modifier:
The draw ratio of plain rod is 100～0.1: 10～0.005.
4. be the clavate sustained release coating agent of framework material with the zein blended modifier, the composition characteristic of its coating is:
Plain rod 95%～55%
Wherein coating material is that biodegradable and environment-friendly material comprise hypromellose (HPMC), ethyl cellulose (EC), cellulose acetate (CA or TCA), polycaprolactone (PCL), polycaprolactam, chitosan, dibutyl phthalate (DBP), tributyl phosphate, getting wherein a kind of or several makes solution and carries out coating, drying according to a conventional method to containing the active substance club.
According to 1 and 2 with the zein blended modifier be framework material the clavate slow releasing agent or 3 described be the clavate slow releasing agent coating materials of framework material with the zein blended modifier, it is characterized in that:
The kind that can be by various components in proportions in the regulin rod or coating membrane and the release timeliness of thickness adjusted active substance were at 10 hours to 6 months.
According to claim 1 and 2 with the zein blended modifier be framework material the clavate slow releasing agent or 3 described be the clavate slow releasing agent coating materials of framework material with the zein blended modifier, it is characterized in that:
This contains active substance clavate slow releasing agent or clavate slow releasing agent coating materials can be used for oral formulations, insecticide, balm, slow release fertilizer and need slow release purpose part to use.
Advantage of the present invention and good effect are:
1. used cheap and easy to get, the environmental protection of the present invention, biodegradable zein are that framework material is worth slow releasing preparation.
2. the present invention adopts the stub shape, specific surface wants high with respect to spheroid or tablet, help drug release, it has the microsphere can be with the inserts mixing but be easy to roll unlike microsphere and be deposited in, so it scatter in helping afield and the characteristics that are difficult for being washed away by fluids such as rainwater.
3. by being framework material with the blending and modifying zein, again in the skeleton outer coatings, by the consumption of hydrophilic material and the structure and the thickness of coating membrane in the adjusting skeleton intermingling material, realization can produce the release in different time limits for active substance not of the same race.
Description of drawings
Fig. 1 is embodiment one an external release profiles
Fig. 2 is blood drug level-time graph in the embodiment one
Fig. 3 is embodiment one reference preparation blood drug level-time graph
Fig. 4 is embodiment two external release profiles
Fig. 5 is embodiment two drug-time curves (TB:NFP slow release rods; R: commercially available reference ordinary tablet)
Fig. 6 is embodiment three external release profiles
Fig. 7 is the outer release profiles of embodiment limbs
The specific embodiment
Below embodiments of the invention are further described:
Embodiment one: 5-fluorouracil (5-Fu) slow release rod (12h)
Plain rod prescription:
5-FU 1.80g
Zein 0.45g
PVPK30 0.75g
The coating prescription:
Preparation method:
Take by weighing the supplementary material of recipe quantity, mix 15min, make abundant mixing.Add an amount of 95% ethanol, heating in water bath makes dissolving.Annotate moulded rod, drying, it is standby to put exsiccator.
Press in recipe quantity DBP and PEG400 to the 20ml acetone, magnetic agitation 1h adds recipe quantity CA, and magnetic agitation 10h makes abundant dissolving, and it is standby to make coating solution.Coating increases weight about 10%.
The release in vitro degree is measured:
Release medium: distilled water 900ml; Sample point: 1,2,4,6,8,10,12 hours; 37 ℃; Measure wavelength 263nm.
The cumulative release degree:
Release profiles is seen Fig. 1.
The release dynamics Higuchi equation, sustainable 12 hours of release time.
Assay method in the body:
Be subjected to the test preparation group after administration 0.5,1.0,1.5,2.0,2.5,3.0,4.0,5.0,6.0,8.0,12.0,24.0,36.0,48.0h gets blood from the rat eye socket respectively; After treatment, high performance liquid chromatogram is measured.Blood drug level data following (four rats) in the body:
Blood drug level-time graph is seen Fig. 2.
Reference preparation (commercially available) blood drug level-time graph is seen Fig. 3.
Reference C-t curve
The statistical moment fitting parameter of 5-FU coating rod and commercially available reference preparation
*P＜0.05
From the blood drug level-time graph area A UC of body intrinsic parameter as can be seen, this patent slow release rod is higher about 8 times than commercially available, and mean residence time prolongs about 7 times.
Embodiment two: nifedipine (NFP) slow release rod (24h)
Prescription:
NFP 1.0g(60.0％)
PEG 1.4g
Zein 1.05g
The coating prescription:
Preparation method:
Take by weighing NFP1.0g, mPEG-g-Zein2.0g by recipe quantity, mix the back and cross 80 mesh sieves, make the mixture mix homogeneously, adds 80% an amount of acetone, put the two is dissolved fully after, add an amount of Zein, volatilize solvent, system is excellent.With the plain rod dry 4h in baking oven that makes, it is standby that exsiccator is put in taking-up.
It is an amount of to get the excellent core for preparing,
Aqueous solution bag internal layer clothing, drying is placed in the exsiccator standby after the cooling.The coating weightening finish is: about 10%.
The release in vitro degree is measured:
Release medium: 0.5%SDS distilled water 900ml; Sample point: 1,3,6,9,10,14,24h; 37 ℃, discharge data and see the following form:
Release profiles is seen Fig. 4.
The release dynamics Higuchi equation, sustainable 24 hours of release time.
The body inner analysis:
Animal subject is a rat, and eye socket is got blood on time, after treatment, high-efficient liquid phase analysis, blood drug level-time graph is seen Fig. 5.
Drug-time curve (TB:NFP slow release rod; R: commercially available reference ordinary tablet)
From drug-time curve figure as can be seen: this patent slow release rod Cmax Cmax significantly is lower than marketed tablet, and the Cmax time of occurrence is significant prolongation also.
Embodiment three: 5-FU slow release rod (1 month)
Prescription
5-FU 0.5g
Zein 0.5g
Coating solution
Preparation method
5-FU and zein are crossed 100 mesh sieves respectively, take by weighing 5-FU and zein, fully mix two materials by recipe quantity, the dissolve with ethanol zein of reuse 95%, heated and stirred in thermostatic water bath, compound concentration is 0.65gml
-1The zein colloid.Then colloid is injected in the mould, release behind the vacuum drying 8h.The PLGA compound concentration is 20% chloroformic solution coating, weightening finish 15%.
Release in vitro:
Release medium: water 900ml, 37 ℃ of temperature, sample time and release see the following form:
Releasing curve diagram 6.
Release dynamics meets 0 grade of equation, 28 days release time.
Embodiment four:
Plain rod prescription:
5-FU 0.4g
Zein 0.6g
The prescription of coating solution:
Preparation:
Behind the 5-FU and Zein mix homogeneously with recipe quantity, behind the heated and stirred 30min, casting is put into 40 ℃ of oven dry of baking oven to 95% alcoholic solution of adding 1ml, is label in 50 ℃ of water-baths.Get the 20%PCL chloroformic solution, coating.Coating weightening finish 32%.
Drug release determination:
Discharge in the water, room temperature, about 90 rev/mins of electronic stirrings record the cumulative release data and see the following form:
| ?Time(d) | 1 | 3 | 10 | 18 | 23 | 30 | 37 | 44 | 51 | 58 | 65 | 72 | 93 | 100 |
| Accumulation % | 1.5 | 4.4 | 8.9 | 22 | 28.5 | 33.8 | 35.5 | 40.8 | 48.7 | 54.6 | 63.9 | 74.5 | 88.6 | 90.1 |
[0105]Release profiles is seen Fig. 7.
Release dynamics meets 0 grade of equation, about 100 days of release time.
Claims (6)
1. be the clavate slow releasing agent of framework material with the zein blended modifier, the composition characteristic of its plain rod is:
Comprise that following component and each composition weight proportioning are:
Zein 20%～75%
Blended modifier 5%～40%
Active substance 20～40%
Wherein blended modifier comprises one or more mixture in polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP), polyacrylic acid (PPA), Polyethylene Glycol (PEG), polyoxyethylene (PEO), tween, span, glycerol, oleic acid, the stearic acid;
Active substance comprises chemical medicine, Chinese medicine extract, spice, pigment, chemical fertilizer, pesticide.
2. according to claim 1 is the preparation method of the plain rod of clavate slow releasing agent of framework material with the zein blended modifier, it is characterized in that:
Modified corn alcohol soluble protein and active matter pledge are blended in the alcohol solvent by weight ratio, stir and to make mix homogeneously, adopt injection molding that the mixture extruding is entered and form bar-shapedly in the mould, club is taken out dry plain rod.
3. be that the clavate slow releasing agent of framework material is characterized in that according to claim 1 and 2 with the zein blended modifier: the draw ratio of plain rod is 100～0.1: 10～0.005.
4. be the clavate sustained release coating agent of framework material with the zein blended modifier, the composition characteristic of its coating is:
Plain rod 95%～75%
Coating material 5～25%
Wherein coating material is that biodegradable and environment-friendly material comprise hypromellose (HPMC), ethyl cellulose (EC), cellulose acetate (CA or TCA), polycaprolactone (PCL), polycaprolactam, chitosan, getting wherein a kind of or several makes solution and carries out coating, drying according to a conventional method to containing the active substance club.
According to claim 1 and 2 with the zein blended modifier be the clavate slow releasing agent of framework material or claim 3 described be the clavate sustained release coating agent of framework material with the zein blended modifier, it is characterized in that:
The kind that can be by various components in proportions in the regulin rod or coating membrane or the release time of thickness adjusted active substance were at 10 hours to 6 months.
According to claim 1 and 2 with the zein blended modifier be framework material the clavate slow releasing agent or 3 described be the clavate sustained release coating agent of framework material with the zein blended modifier, it is characterized in that:
This contains active substance clavate slow releasing agent or the agent of clavate sustained release coating can be used for oral formulations, insecticide, balm, slow release fertilizer and need slow release purpose part to use.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011100963763A CN102232921A (en) | 2010-04-08 | 2011-04-08 | Technique for preparing rod-like sustained-release preparation by using blending-modified corn zein as skeleton material and preparation prepared by technique |
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| CN201010143897.5 | 2010-04-08 | ||
| CN201010143897A CN101849901A (en) | 2010-04-08 | 2010-04-08 | Technique for preparing controlled-release preparation of zero-order release bar and preparation thereof |
| CN2011100963763A CN102232921A (en) | 2010-04-08 | 2011-04-08 | Technique for preparing rod-like sustained-release preparation by using blending-modified corn zein as skeleton material and preparation prepared by technique |
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| CN2011100963763A Pending CN102232921A (en) | 2010-04-08 | 2011-04-08 | Technique for preparing rod-like sustained-release preparation by using blending-modified corn zein as skeleton material and preparation prepared by technique |
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| CN103242088A (en) * | 2013-04-25 | 2013-08-14 | 苏州谷力生物科技有限公司 | Slow-release leaf surface selenium fertilizer |
| CN105967921A (en) * | 2016-02-25 | 2016-09-28 | 马鞍山市全润农业科技有限公司 | Modified-Chinese-chestnut-protein-coated slow-release medicinal fertilizer |
| CN108997060A (en) * | 2018-09-12 | 2018-12-14 | 石河子大学 | Coated slow release fertilizer and its preparation method and application based on microelement in humic-acid kind material chelating |
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2010
- 2010-04-08 CN CN201010143897A patent/CN101849901A/en active Pending
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2011
- 2011-04-08 CN CN2011100963763A patent/CN102232921A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103242088A (en) * | 2013-04-25 | 2013-08-14 | 苏州谷力生物科技有限公司 | Slow-release leaf surface selenium fertilizer |
| CN105967921A (en) * | 2016-02-25 | 2016-09-28 | 马鞍山市全润农业科技有限公司 | Modified-Chinese-chestnut-protein-coated slow-release medicinal fertilizer |
| CN108997060A (en) * | 2018-09-12 | 2018-12-14 | 石河子大学 | Coated slow release fertilizer and its preparation method and application based on microelement in humic-acid kind material chelating |
| CN108997060B (en) * | 2018-09-12 | 2021-09-03 | 石河子大学 | Coated slow-release fertilizer chelating medium and trace elements based on humic acid materials and preparation method and application thereof |
| CN109350609A (en) * | 2018-11-14 | 2019-02-19 | 常州大学 | A kind of preparation of chitosan package zeins nanoparticle and the application for loading acacetin sodium salt |
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Application publication date: 20111109 |