CN105168181A - Preparation method for oxymatrine microcapsules - Google Patents
Preparation method for oxymatrine microcapsules Download PDFInfo
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- CN105168181A CN105168181A CN201510730479.9A CN201510730479A CN105168181A CN 105168181 A CN105168181 A CN 105168181A CN 201510730479 A CN201510730479 A CN 201510730479A CN 105168181 A CN105168181 A CN 105168181A
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Abstract
The invention discloses a preparation method for oxymatrine microcapsules. The method comprises the following steps that silicon dioxide template materials are prepared, and self-assembling is performed layer upon layer by taking poly allyamine hydrochloride and polystyrene sodium sulfonate as positive and negative polyelectrolytes to prepared template microcapsules which are not denucleated; the template microcapsules which are not denucleated are taken, hydrogen fluoride is added to enable SiO2 to be fully dissolved, and centrifugal cleaning is repeatedly performed with a NaCl solution until the pH is 7. According to the preparation method for the oxymatrine microcapsules, the prepared hollow microcapsules are uniform in size and form, the size of the microcapsules can be actively controlled through the lay number of the polyelectrolytes containing opposite charges, and the form of the microcapsules can be controlled through template nucleuses; accordingly, the drug releasing controllability and targeting property can be improved.
Description
Technical field
The application belongs to field of medicine preparing technology, is specifically related to a kind of preparation method of oxymatrine microcapsule.
Background technology
Oxymatrine is the alkaloid separated from the dry root of leguminous plant Radix Sophorae Flavescentis (Sophoraflavescensait) or leguminous plant root of subprostrate sophora (SophorasubprostrataChunetT.Chen), and the domestic and international research about matrine at present shows: matrine can by the synthesis of inhibition tumor cell DNA, by inducing tumor cell generation apoptosis such as the activity of the impact gene expression relevant to tumor cell, inhibitory enzyme.
LBL self-assembly method (Selflayer-by-layer, LbL) utilizes supermolecule electrostatic self-assembled principle, adsorbed the polyelectrolyte of oppositely charged by the effect of electrostatic attraction successively, thus form the ultrathin membrane with several functions.This method preparation technology is simple, only need simple alternately dip-coating just can assemble at the molecule of material surface, and the mild condition needed for preparation, can complete in normal-temperature water solution, is conducive to the effective efficiency keeping drug molecule.
There is no LBL self-assembly legal system at present for the application of matrine microcapsule, there is bad dispersibility in the method that tradition prepares oxymatrine microcapsule, shell rough surface, freezing nuclei, the uncontrollability of the size of hollow capsule, form, heavy wall, the problems such as the release of medicine is uncontrollable.
Summary of the invention
In view of this, technical problems to be solved in this application be exist in prior art prepare oxymatrine microcapsule time there is the uncontrollability of the size of hollow capsule, form, heavy wall, the uncontrollable problem of release of medicine.
In order to solve the problems of the technologies described above, this application discloses a kind of preparation method of oxymatrine microcapsule, comprising the following steps:
The preparation of step 1, mold materials silicon dioxide: add dehydrated alcohol and ammonia in beaker, beaker is put into ultrasonic washing instrument and carries out supersound process, add ethyl orthosilicate, ultrasonic 1-3h, aged overnight after completing, obtains the alcohol dispersion liquid of silicon dioxide;
In alcohol dispersion liquid, put into stirrer, place it on blender and stir, add 3-aminopropyl triethoxysilane simultaneously, stirring reaction 8-16h, then carries out concentrating under reduced pressure, until crystalline particles thing is separated out, with deionized water wash to neutral, obtain amido modified template particles;
Step 2, by SiO
2ultrasonic 3-8min carries out dispersion and prepares SiO
2dispersion liquid, measures SiO
2dispersion liquid and PAH aqueous solution, by SiO2 dispersion liquid and PAH aqueous solution ultrasonic, leave standstill and carry out centrifugal treating, the PAH that removing upper strata is unnecessary, add ultra-pure water and carry out ultrasonic cleaning 3 times, add kayexalate aqueous solution, stir 5-15min to make to react completely, and carry out centrifugal treating, the kayexalate that removing upper strata is unnecessary, add ultra-pure water and carry out ultrasonic cleaning 3 times, repeat step until PAH/PSS forms 10 layers, obtain the template microcapsule of non-enucleation;
Step 3, get the template microcapsule of non-enucleation, add hydrogen fluoride reaction 30min, make SiO
2abundant decomposition, with the cleaning of NaCl solution repeated centrifugation until pH is 7.
Further, in step 1, Ultrasonic Conditions is: ultrasonic electric power 130W-170W, and water temperature is 20 DEG C-30 DEG C.
Further, in step 1, the volume ratio of dehydrated alcohol, ammonia and ethyl orthosilicate is 2:2-6:40-60; The volume ratio of the alcohol dispersion liquid of described 3-aminopropyl triethoxysilane and silicon dioxide is 1:5-1:15.
Further, in step 1, concentrating under reduced pressure condition is: pressure is 0.05MPa, and water temperature is 30 DEG C, and rotating speed is 20 revs/min.
Further, SiO in step 2
2the volume ratio of dispersion liquid and PAH aqueous solution is 1:1-1:3; Kayexalate aqueous solution and SiO
2the volume ratio of dispersion liquid is 1:1-3:1.
Further, in step 2, SiO2 dispersion liquid and PAH aqueous solution are carried out ultrasonic 10-20min, leave standstill 25-35min, with the centrifugal 3-8min of 2500rpm-3500rpm rotating speed, the PAH that removing upper strata is unnecessary, and with the centrifugal 3-8min of 2500rpm-3500rpm rotating speed, the kayexalate that removing upper strata is unnecessary.
Further, the molecular weight of PAH is 70kDa, and the mass concentration of described PAH is 3mg/mL, and the molecular weight of described kayexalate is 70kDa, and the mass concentration of described kayexalate is 3mg/mL.
Further, hydrofluoric volumetric concentration is 98%, and the concentration of NaCl solution is 0.5mmol/L.
Compared with prior art, the application can obtain and comprise following technique effect:
The application's preparation condition is relatively simple; Hollow micro capsule size prepared by the application, form are homogeneous, and the size of microcapsule can by the number of plies ACTIVE CONTROL of the polyelectrolyte of packaging opposite charges, and form controls by template core; This method improves controllability, the targeting of drug release, selects PAH and kayexalate to be enclose material, has pH sensitivity, effectively discharge under can making microcapsule acid condition under one's belt, to reach controllability, targeting effect.
Certainly, the arbitrary product implementing the application must not necessarily need to reach above-described all technique effects simultaneously.
Detailed description of the invention
Embodiment will be coordinated below to describe the embodiment of the application in detail, by this to the application how application technology means solve technical problem and the implementation procedure reaching technology effect can fully understand and implement according to this.
The application provides a kind of preparation method of oxymatrine microcapsule, comprises the following steps:
The preparation of step 1, mold materials silicon dioxide: add dehydrated alcohol and ammonia in beaker, beaker is put into ultrasonic washing instrument, ultrasonic electric power 130W-170W, water temperature 20 DEG C of-30 DEG C of conditions are ultrasonic, add ethyl orthosilicate (TEOS), ultrasonic 1-3h, aged overnight after completing, obtain the alcohol dispersion liquid of silicon dioxide, wherein, the volume ratio of dehydrated alcohol, ammonia and ethyl orthosilicate is 2:2-6:40-60;
Stirrer is put in alcohol dispersion liquid, place it on blender and stir, add 3-aminopropyl triethoxysilane (APTES), stirring reaction 8-16h simultaneously, then at 0.05MPa, water temperature 30 DEG C, carries out concentrating under reduced pressure under rotating speed 20 revs/min of conditions, until crystalline particles thing is separated out, with deionized water wash to neutral, obtain amido modified template particles, wherein, the volume ratio of the alcohol dispersion liquid of 3-aminopropyl triethoxysilane and silicon dioxide is 1:5-15;
Step 2, with PAH (PAH, molecular weight 70kDa) and kayexalate (PSS, molecular weight 70kDa) for positive and negative polyelectrolyte self assembly microcapsule layer by layer, concrete steps are as follows: by SiO
2ultrasonic 3-8min disperses, and prepares SiO
2dispersion liquid; Measure SiO
2dispersion liquid and the ultrasonic 10-20min of PAH aqueous solution, wherein, the volume ratio of SiO2 dispersion liquid and PAH aqueous solution is 1:1-1:3, leave standstill 25-35min, with the centrifugal 3-8min of 2500rpm-3500rpm rotating speed, the PAH that removing upper strata is unnecessary, adds ultra-pure water and carries out ultrasonic cleaning 3 times; Add kayexalate aqueous solution, wherein, the volume ratio of kayexalate aqueous solution and SiO2 dispersion liquid is 1:1-3:1, stir 5-15min to make to react completely, with the centrifugal 3-8min of 2500rpm-3500rpm rotating speed, the kayexalate that removing upper strata is unnecessary, adds ultra-pure water and carries out ultrasonic cleaning 3 times, repeat step until PAH/PSS forms 10 layers, obtain the template microcapsule of non-enucleation;
Step 3, get the template microcapsule of non-enucleation, add volumetric concentration be 98% fluohydric acid gas (HF) react 30min, make SiO
2abundant decomposition, repeats eccentric cleaning until pH is 7 with 0.5mmol/LNaCl solution.
PAH in preparation method and kayexalate, have opposite charges, can effectively be packaged into above template layer by layer, and this bi-material has certain pH sensitivity, effectively can discharge in acid condition, reach controlled-release effect.
Centrifugal rotating speed and time after each packaging in this method Central Shanxi Plain completes, if rotating speed and time are more than 3500rpm, 8min can make silicon dioxide mutually adhere to, be difficult to again ultrasonic disperse open, dispersibility is deteriorated, if the enclose material removing that rotating speed and time can make upper strata free lower than 2500rpm, 3min is incomplete, the enclose material reaction of the oppositely charged that can and newly add, affects the enclose of template.
Embodiment 1
In beaker, add 50mL dehydrated alcohol and ammonia 4mL, beaker put into ultrasonic washing instrument, open ultrasonic after, add 2mL ethyl orthosilicate (TEOS), ultrasonic 2h, aged overnight after completing, obtain the alcohol dispersion liquid of silicon dioxide.Stirrer is put in the alcohol dispersion liquid of silicon dioxide, place it on blender and stir, add 2mL3-aminopropyl triethoxysilane (APTES) simultaneously, stirring reaction 12h, then concentrating under reduced pressure is carried out, until crystalline particles thing is separated out, with deionized water wash to neutral, obtain amido modified template particles.
By SiO
2ultrasonic 5min disperses, and prepares SiO
2dispersion liquid; Measure 2mLSiO
2dispersion liquid and the ultrasonic 15min of 2mL3mg/mLPAH aqueous solution, leave standstill 30min, and with the centrifugal 5min of 3000rpm rotating speed, the PAH that removing upper strata is unnecessary, adds ultra-pure water and carry out ultrasonic cleaning 3 times.Add 2mL3mg/mL aqueous solution PSS again, stir 10min and make to react completely, with the centrifugal 5min of 3000rpm rotating speed, the PSS that removing upper strata is unnecessary, adds ultra-pure water and carries out ultrasonic cleaning 3 times, repeats step until PAH/PSS forms 10 layers.Get the template microcapsule of the non-enucleation of 2mL, add the HF reaction 30min that concentration is 98%, make SiO
2abundant decomposition, repeats eccentric cleaning until pH is 7 with 0.5mmol/LNaCl solution.
Embodiment 2
A kind of preparation method of oxymatrine microcapsule, comprise the following steps: in beaker, add dehydrated alcohol and ammonia, beaker is put into ultrasonic washing instrument, ultrasonic electric power 130W, water temperature 30 DEG C of conditions are ultrasonic, add ethyl orthosilicate, ultrasonic 1h, aged overnight after completing, obtains the alcohol dispersion liquid of silicon dioxide, wherein, the volume ratio of dehydrated alcohol, ammonia and ethyl orthosilicate is 2:2:60; Stirrer is put in alcohol dispersion liquid, place it on blender and stir, add 3-aminopropyl triethoxysilane simultaneously, stirring reaction 8h, then at 0.05MPa, water temperature 30 DEG C, carries out concentrating under reduced pressure under rotating speed 20 revs/min of conditions, until crystalline particles thing is separated out, with deionized water wash to neutral, obtain amido modified template particles, wherein, the volume ratio of the alcohol dispersion liquid of 3-aminopropyl triethoxysilane and silicon dioxide is 1:5; By SiO
2ultrasonic 3-8min disperses, and prepares SiO
2dispersion liquid; Measure SiO
2dispersion liquid and the ultrasonic 10min of PAH aqueous solution, wherein, SiO
2the volume ratio of dispersion liquid and PAH aqueous solution is 1:1, leaves standstill 25min, and with the centrifugal 8min of 2500rpm rotating speed, the PAH that removing upper strata is unnecessary, adds ultra-pure water and carry out ultrasonic cleaning 3 times; Add kayexalate aqueous solution, wherein, kayexalate aqueous solution and SiO
2the volume ratio of dispersion liquid is 1:1, stirs 15min and makes to react completely, with the centrifugal 8min of 2500rpm rotating speed, the kayexalate that removing upper strata is unnecessary, add ultra-pure water and carry out ultrasonic cleaning 3 times, repeat step until PAH/PSS forms 10 layers, obtain the template microcapsule of non-enucleation; Get the template microcapsule of the non-enucleation of 2mL, add the fluohydric acid gas (HF) that volumetric concentration is 98%2mL and react 30min, make SiO
2abundant decomposition, repeats eccentric cleaning until pH is 7 with 0.5mmol/LNaCl solution.
Embodiment 3
A kind of preparation method of oxymatrine microcapsule, comprise the following steps: in beaker, add dehydrated alcohol and ammonia, beaker is put into ultrasonic washing instrument, ultrasonic electric power 170W, water temperature 20 DEG C of conditions are ultrasonic, add ethyl orthosilicate, ultrasonic 3h, aged overnight after completing, obtains the alcohol dispersion liquid of silicon dioxide, wherein, the volume ratio of dehydrated alcohol, ammonia and ethyl orthosilicate is 2:6:40; Stirrer is put in alcohol dispersion liquid, place it on blender and stir, add 3-aminopropyl triethoxysilane simultaneously, stirring reaction 16h, then at 0.05MPa, water temperature 30 DEG C, carries out concentrating under reduced pressure under rotating speed 20 revs/min of conditions, until crystalline particles thing is separated out, with deionized water wash to neutral, obtain amido modified template particles, wherein, the volume ratio of the alcohol dispersion liquid of 3-aminopropyl triethoxysilane silicon dioxide is 1:15; By SiO
2ultrasonic 3-8min disperses, and prepares SiO
2dispersion liquid; Measure SiO
2dispersion liquid and the ultrasonic 10-20min of PAH aqueous solution, wherein, SiO
2the volume ratio of dispersion liquid and PAH aqueous solution is 1:3, leaves standstill 35min, and with the centrifugal 3min of 3500rpm rotating speed, the PAH that removing upper strata is unnecessary, adds ultra-pure water and carry out ultrasonic cleaning 3 times; Add kayexalate aqueous solution, wherein, kayexalate aqueous solution and SiO
2the volume ratio of dispersion liquid is 3:1, stirs 5min and makes to react completely, with the centrifugal 3min of 3500rpm rotating speed, the kayexalate that removing upper strata is unnecessary, add ultra-pure water and carry out ultrasonic cleaning 3 times, repeat step until PAH/PSS forms 10 layers, obtain the template microcapsule of non-enucleation; Get the template microcapsule of the non-enucleation of 2mL, add the fluohydric acid gas (HF) that volumetric concentration is 98%2mL and react 30min, SiO2 is fully decomposed, repeat eccentric cleaning until pH is 7 with 0.5mmol/LNaCl solution.
The beneficial effect of the application is described below in conjunction with concrete experimental result:
Accurately take oxymatrine 1mg powder and be placed in 10mL volumetric flask, be the mother solution of 0.1mg/mL with ultra-pure water standardize solution, mother solution is diluted to 10 respectively, 5, 2.5, 1.25, 0.625ug/mL series standard liquid, under maximum absorption wavelength is 220nm condition, measure its absorbance by ultraviolet spectrophotometer and be respectively 0.762, 0.419, 0.224, 0.125, 0.076, with the concentration (x) of oxymatrine standard sample for abscissa, with the absorbance of corresponding concentration for vertical coordinate (y) draws concentration standard curve, obtain standard curve equation y=0.0732x+0.0375R2=0.9988, result shows that Oxymatrine alkali concn is good in 0.625-10ug/mL scope internal linear relation.
Precision takes appropriate oxymatrine, is dissolved in ultra-pure water and is configured to the solution that concentration is 1mg/mL, adds 2mL hollow micro capsule dispersion liquid in centrifuge tube, then adds above-mentioned matrine solution 200uL toward it, stirs and hatch 12h under room temperature condition.Suspension, with the centrifugal 5min of 8000rpm rotating speed, is got supernatant 200uL, is settled to 10mL with ultra-pure water, and take ultra-pure water as reference, ultraviolet spectrophotometer sends out the absorbance being determined at 220nm place.The absorbance measured is 0.064.The Cf of oxymatrine can be conversed by standard curve equation y=0.0732x+0.0375R2=0.9988, by EN%=(1-Cf/Ct) × 100%, wherein, Cf is the amount of free drug, Ct is the medicine total amount added, and obtaining envelop rate is 80.08%.
Also it should be noted that, term " comprises ", " comprising " or its any other variant are intended to contain comprising of nonexcludability, thus make to comprise the commodity of a series of key element or system not only comprises those key elements, but also comprise other key elements clearly do not listed, or also comprise by this commodity or the intrinsic key element of system.When not more restrictions, the key element limited by statement " comprising ... ", and be not precluded within the commodity or system comprising described key element and also there is other identical element.
Above-mentioned explanation illustrate and describes some preferred embodiments of the application, but as previously mentioned, be to be understood that the application is not limited to the form disclosed by this paper, should not regard the eliminating to other embodiments as, and can be used for other combinations various, amendment and environment, and can in invention contemplated scope described herein, changed by the technology of above-mentioned instruction or association area or knowledge.And the change that those skilled in the art carry out and change do not depart from the spirit and scope of the application, then all should in the protection domain of the application's claims.
Claims (8)
1. a preparation method for oxymatrine microcapsule, is characterized in that, comprises the following steps:
The preparation of step 1, mold materials silicon dioxide: add dehydrated alcohol and ammonia in beaker, beaker is put into ultrasonic washing instrument and carries out supersound process, add ethyl orthosilicate, ultrasonic 1-3h, aged overnight after completing, obtains the alcohol dispersion liquid of silicon dioxide;
In alcohol dispersion liquid, put into stirrer, place it on blender and stir, add 3-aminopropyl triethoxysilane simultaneously, stirring reaction 8-16h, then carries out concentrating under reduced pressure, until crystalline particles thing is separated out, with deionized water wash to neutral, obtain amido modified template particles;
Step 2, by SiO
2ultrasonic 3-8min carries out dispersion and prepares SiO
2dispersion liquid, measures SiO
2dispersion liquid and PAH aqueous solution, by SiO
2dispersion liquid and PAH aqueous solution ultrasonic, leave standstill and carry out centrifugal treating, the unnecessary PAH in removing upper strata, adds ultra-pure water and carries out ultrasonic cleaning 3 times; Add kayexalate aqueous solution, stir 5-15min and make to react completely, and carry out centrifugal treating, the kayexalate that removing upper strata is unnecessary, add ultra-pure water and carry out ultrasonic cleaning 3 times, repeat step until PAH/PSS forms 10 layers, obtain the template microcapsule of non-enucleation;
Step 3, get the template microcapsule of non-enucleation, add hydrogen fluoride reaction 30min, make SiO
2abundant decomposition, with the cleaning of NaCl solution repeated centrifugation until pH is 7.
2. the preparation method of oxymatrine microcapsule according to claim 1, is characterized in that, in described step 1, Ultrasonic Conditions is: ultrasonic electric power 130W-170W, and water temperature is 20 DEG C-30 DEG C.
3. the preparation method of oxymatrine microcapsule according to claim 1, is characterized in that, in described step 1, the volume ratio of dehydrated alcohol, ammonia and ethyl orthosilicate is 2:2-6:40-60; The volume ratio of the alcohol dispersion liquid of described 3-aminopropyl triethoxysilane and silicon dioxide is 1:5-1:15.
4. the preparation method of oxymatrine microcapsule according to claim 1, is characterized in that, in described step 1, concentrating under reduced pressure condition is: pressure is 0.05MPa, and water temperature is 30 DEG C, and rotating speed is 20 revs/min.
5. the preparation method of oxymatrine microcapsule according to claim 1, is characterized in that, SiO in described step 2
2the volume ratio of dispersion liquid and PAH aqueous solution is 1:1-1:3; Kayexalate aqueous solution and SiO
2the volume ratio of dispersion liquid is 1:1-3:1.
6. the preparation method of oxymatrine microcapsule according to claim 1, is characterized in that, by SiO in step 2
2dispersion liquid and PAH aqueous solution carry out ultrasonic 10-20min, leave standstill 25-35min, with the centrifugal 3-8min of 2500rpm-3500rpm rotating speed, the PAH that removing upper strata is unnecessary, and with the centrifugal 3-8min of 2500rpm-3500rpm rotating speed, the kayexalate that removing upper strata is unnecessary.
7. the preparation method of oxymatrine microcapsule according to claim 1, is characterized in that, the molecular weight of described PAH is 70kDa, and the mass concentration of described PAH is 3mg/mL; The molecular weight of described kayexalate is 70kDa, and the mass concentration of described kayexalate is 3mg/mL.
8. the preparation method of oxymatrine microcapsule according to claim 1, is characterized in that, described hydrofluoric volumetric concentration is 98%, and the concentration of NaCl solution is 0.5mmol/L.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112602841A (en) * | 2020-12-15 | 2021-04-06 | 南京农业大学 | Oxymatrine and tributyrin composite microcapsule as well as preparation method and application thereof |
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| CN101773483A (en) * | 2010-01-20 | 2010-07-14 | 华东理工大学 | Preparation method of water-insoluble drug microcapsule |
| CN102580641A (en) * | 2012-03-01 | 2012-07-18 | 天津大学 | Method for producing natural polysaccharide-base nanocapsules |
| CN102744022A (en) * | 2012-07-23 | 2012-10-24 | 北京理工大学 | Hollow microcapsule, acidic or alkaline controlled-release microcapsule and preparation methods thereof |
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Patent Citations (4)
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| WO2005044272A1 (en) * | 2003-11-04 | 2005-05-19 | Scottsdale Scientific Dba Allergy Research Group/Nutricology, Inc. | Compositions and methods for treating cellular proliferation disorders |
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| CN102580641A (en) * | 2012-03-01 | 2012-07-18 | 天津大学 | Method for producing natural polysaccharide-base nanocapsules |
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| CN112602841A (en) * | 2020-12-15 | 2021-04-06 | 南京农业大学 | Oxymatrine and tributyrin composite microcapsule as well as preparation method and application thereof |
| CN112602841B (en) * | 2020-12-15 | 2022-03-29 | 南京农业大学 | Oxymatrine and tributyrin composite microcapsule as well as preparation method and application thereof |
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