CN101020058A - Application of pure silicon based monodisperse spherical mesoporous molecular sieve in slow release of medicine - Google Patents
Application of pure silicon based monodisperse spherical mesoporous molecular sieve in slow release of medicine Download PDFInfo
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- CN101020058A CN101020058A CN 200710061610 CN200710061610A CN101020058A CN 101020058 A CN101020058 A CN 101020058A CN 200710061610 CN200710061610 CN 200710061610 CN 200710061610 A CN200710061610 A CN 200710061610A CN 101020058 A CN101020058 A CN 101020058A
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Abstract
The application of pure silicon based monodisperse spherical mesoporous molecular sieve in slow release of medicine includes adding the medicine into organic solvent to obtain medicine solution A of 10.0-40.0 mg/ml concentration; adding the pure silicon based monodisperse spherical mesoporous molecular sieve of hexagonal structure, 2.0-5.0 nm pore size, 800-1500 sq m/g specific surface area and 100-1000 nm particle size into the solution A in the ratio between the molecular sieve to solution volume of 0.2-0.5 g to 20.0-50.0 ml; stirring at room temperature for 0.5-3 days, centrifuging and drying the solid at 40-60 deg.c to obtain a solid preparation. The present invention has the features of stale structure, no biological toxicity, high medicine carrying amount and long medicine releasing period.
Description
Technical field
The present invention relates to the application of a kind of pure silicon based monodisperse spherical molecular sieve in medicine absorption, slow release, relate in particular to and have six side's phase structures, have of the application of the pure silicon based monodisperse spherical molecular sieve of variable grain size at medicine absorption, slow release.
Technical background
In the past few decades, the medicament slow release technology be always with fastest developing speed in the modern biomedicine field, also be the most promising drug preparation technique.For traditional pharmaceutical dosage form, such as typical tablet, intravenous injection, often owing to the fluctuation of blood drug level causes toxic and side effects to the patient.When blood drug level is lower than minimum effective blood drug concentration, just do not have due therapeutical effect, and when blood drug level is higher than safe blood drug level, can cause toxic and side effects, directly threaten patient's life even.The medicament of employing controlled release technologies then can make the drug level in the blood remain on a comparatively constant level in than the long time, has advantages such as efficient, as to reduce poisonous side effect of medicine, raising patient sensation comfort level and reduction medical expense.
Many proud premium properties that the appearance of mesoporous silicon and mesoporous silicon itself has, as high-ratio surface, large pore volume, narrowly distributing and in relative broad range adjustable aperture, surface be easy to modification and excellent biological compatibility etc., indicating that mesoporous silicon is expected to be developed to a kind of novel medicament controlled release carrier material.Regi and partner thereof (M.Vallet-Reg í, A.R á mila, R.P.del Real, J.P é rez-Pariente, Chem.Mater.13,308-311 (2001)), utilizes the surface silanol group of mesoporous material and the interaction of hydrogen bond between the medicine ibuprofen, realized the controllable release that the high drug load of ibuprofen in silicon-based mesoporous material adsorbs and assemble medicine in simulated body fluid.Be subjected to the inspiration of this work, people have carried out comparatively deep research to it.U.S. Pat 2002164380 is a structure directing agent with vitamin E TPGS (Vitamin E d-[alpha]-tocopherylpolyethylene glycol 1000 succinate), has synthesized the drug carrier material with mesoporous feature on the basis of adding the A1 source.
In the research in the past, people to silicon-based mesoporous material the application in medicament slow release mainly investigate by organic-inorganic is functionalized and improve medicine adsorbance and controlling slow release time, and the molecular sieve pattern is less to the influence research of the medicine rate of adsorption, medicine adsorbance and medicament slow release performance.But D.Zhao then finds in the adsorption process of research enzyme, enzyme on molecular sieve carrier adsorbance and the pattern of the rate of adsorption and molecular sieve very direct relation (Micro.Mesopor.Mater.73,121-128 (2004)) is arranged.And the drug carrier material in above-mentioned United States Patent (USP) is taken Al possible in the process patient and is run off and also be unfavorable for taking for a long time.
Before this, R.Nooney has obtained variable grain size, monodispersed spherical MCM-41 (Chem.Mater.14 by the amount that changes surfactant in pure water mixed solvent, 4721-4728 (2002)), the molecular screen material aperture is at 2.0-5.0nm, specific surface 800-1100m
2/ g etc., spherical particle size be at 100-740nm, but they not to these molecular sieves possible application inquire into.Although A.Katiyar (J.Chromatogr.A.1122,13-20 (2006)) and
Szegedi (Appl.Catal.A:Gen.272,257-266 (2004)) has reported the application of spherical molecular sieve in chromatographic isolation and catalysis respectively, but the application in medicine absorption and slow release still rarely has report to spherical molecular sieve.
Summary of the invention
The object of the invention provides the method that a kind of pure silicon based monodisperse spherical mesoporous molecular sieve is applied to medicine absorption and slow release.
Pure silicon based monodisperse spherical mesoporous molecular sieve of the present invention is to have six side's phase structures, aperture at 2.0-5.0nm, specific surface 800-1500m
2/ g etc., spherical particle size are at 100-1000nm, and the concrete preparation method of pure silicon based monodisperse spherical mesoporous molecular sieve is seen Chem.Mater.14,4721-4728 (2002) document.
The present invention includes following steps:
1. medicine is joined in the organic solvent, making drug concentrations is 10.0-40.0mg/mL, obtains solution A;
2. will have six side's phase structures, aperture at 2.0-5.0nm, specific surface 800-1500m
2/ g etc., spherical particle size are in the solution A that the pure silicon based monodisperse spherical mesoporous molecular sieve of 100-1000nm joins, make molecular sieve: solution A is 0.2-0.5g: 20.0-50.0mL, stir centrifugalize after 0.5-3 days under the room temperature, centrifugal gained solid is placed under 40-600 ℃ be drying to obtain solid powder.
The solid powder of the present invention's preparation can also carry out tabletting under 2.0-4.0MPa pressure, promptly get tablet.
Aforesaid medicine is antibiotic, anti-pathogenic microorganism medicine, antitumor medication, cardiovascular drugs, medicine for respiratory system, consumption systems medicine or blood system medicine.
Aforesaid organic solvent is methanol, ethanol, acetone, normal hexane or chloroform.
The characteristics that the present invention compared with prior art has are:
1. the molecular sieve by selecting varying particle size can regulating medicine reaches capacity in molecular sieve the time of absorption;
2. the molecular sieve by selecting different specific surfaces, pore volume, aperture can the maximal absorptive capacity of regulating medicine in molecular sieve;
3. the sustained release rate that the molecular sieve by selecting varying particle size, aperture, specific surface can regulating medicine, the advantage that pharmaceutical release time is long;
4. selected molecular sieve has Stability Analysis of Structures, drug loading (mass percent 25%-33%) that physiology is nontoxic and high.
The specific embodiment
Embodiment 1
Synthetic test: according to the synthetic particle size of document (Chem.Mater.14,4721-4728 (2002)) is the mesopore molecular sieve of 100nm.The specific surface of gained molecular sieve is 1100cm
2/ g, pore volume 1.05cm
3/ g.
Medicine absorption: the 0.9g ibuprofen is added in the 30mL normal hexane, and making the concentration of ibuprofen is 30.0mg/mL, obtains solution A 1.Getting the 0.3g particle size is that the 100nm sieve sample joins among the solution A l, stirs centrifugalize after 0.5 day under the room temperature, and centrifugal gained solid is placed 50 ℃ of dryings down.Promptly obtain sample B1.
Medicament slow release test: get 0.3g sample B1 solid powder or under 3.0MPa pressure resulting tablet, put into 140mL simulated body fluid SBF.37 ℃ of constant temperature.Through after the predefined time, take out a spot of solution and measure the solution drug level, simultaneously the fresh simulation physiological fluid of adding equivalent in the slow-releasing system at once with UV-vis.The 5h medicine discharges substantially fully.
Embodiment 2
Synthetic test: according to the synthetic particle size of document (Chem.Mater.14,4721-4728 (2002)) is the mesopore molecular sieve of 500nm.The specific surface of gained molecular sieve is 950cm
2/ g, pore volume 0.83cm
3/ g.
Medicine absorption: the 0.9g ibuprofen is added in the 30mL normal hexane, and making the concentration of ibuprofen is 30.0mg/mL, obtains solution A 2.Getting the 0.3g particle size is that the 500nm sieve sample joins in the solution A 2, stirs centrifugalize after 2 days under the room temperature, and centrifugal gained solid is placed 50 ℃ of dryings down.Promptly obtain sample B2.
The time that the medicament slow release test discharges fully with embodiment 1. medicines is 15h.
Embodiment 3
Synthetic test: according to document (Chem.Mater.14,4721-4728 (2002)), its method is carried out certain improvement, all change water and alcoholic acid volume into 300mL, the amount of Surfactant CTAB changes 1.5g into.Synthetic particle size is the mesopore molecular sieve of 900nm.The specific surface of gained molecular sieve is 810cm
2/ g, pore volume 0.86cm
3/ g.
Medicine absorption: the 0.8g ibuprofen is added in the 20mL normal hexane, and making the concentration of ibuprofen is 40.0mg/mL, obtains solution A 3.Getting the 0.2g particle size is that the 900nm sieve sample joins in the solution A 3, stirs centrifugalize after 3 days under the room temperature, and centrifugal gained solid is placed 50 ℃ of dryings down.Promptly obtain sample B3.
The time that the medicament slow release test discharges fully with embodiment 1. medicines is 40h.
Embodiment 4
Synthetic test is with embodiment 1.
Medicine absorption: the 0.9g mecillinam is added in the 30mL dehydrated alcohol, and making the concentration of mecillinam is 30.0mg/mL, obtains solution A 4.Getting the 0.3g particle size is that the 100nm sieve sample joins in the solution A 4, stirs centrifugalize after 0.5 day under the room temperature, gets a certain amount of upper solution and tests with ultraviolet-visual spectrometer.Centrifugal gained solid is placed 50 ℃ of dryings down.Promptly obtain sample B4.
The medicament slow release test is with embodiment 1.The time that medicine discharges fully is 10h.
Embodiment 5
Synthetic test is with embodiment 1.
Medicine absorption: the 0.9g famciclovir is added in the 30mL acetone, and making the concentration of famciclovir is 30.0mg/mL, obtains solution A 5.Getting the 0.3g particle size is that the 100nm sieve sample joins in the solution A 5, stirs centrifugalize after 0.5 day under the room temperature, gets a certain amount of upper solution and tests with ultraviolet-visual spectrometer.Centrifugal gained solid is placed 50 ℃ of dryings down.Promptly obtain sample B5.
The time that the medicament slow release process of the test discharges fully with embodiment 1. medicines is 8h.
Embodiment 6
Synthetic test is with embodiment 1.
Medicine absorption: go FPL-60278 to add in the 30mL chloroform 0.9g, making the concentration of FPL-60278 is 30.0mg/mL, obtains solution A 6.Getting the 0.3g particle size is that the 100nm sieve sample joins in the solution A 6, stirs centrifugalize after 0.5 day under the room temperature, gets a certain amount of upper solution and tests with ultraviolet-visual spectrometer.Centrifugal gained solid is placed 50 ℃ of dryings down.Promptly obtain sample B6.
The time that the medicament slow release process of the test discharges fully with embodiment 1. medicines is 8h.
Embodiment 7
Synthetic test is with embodiment 1.
Medicine absorption: the 0.9g doxifluridine is added in the 30mL absolute methanol, and making the concentration of oxygen floxuridine is 30.0mg/mL, obtains solution A 7.Getting the 0.3g particle size is that the 100nm sieve sample joins in the solution A 7, stirs centrifugalize after 0.5 day under the room temperature, gets a certain amount of upper solution and tests with ultraviolet-visual spectrometer.Centrifugal gained solid is placed 50 ℃ of dryings down.Promptly obtain sample B7.
The time that the medicament slow release process of the test discharges fully with embodiment 1. medicines is 9h.
Embodiment 8
Synthetic test is with embodiment 1.
Medicine absorption: the 0.9g tranilast is added in the 30mL chloroform, and making the concentration of tranilast is 30.0mg/mL, obtains solution A 8.Getting the 0.3g particle size is that the 100nm sieve sample joins in the solution A 8, stirs centrifugalize after 0.5 day under the room temperature, gets a certain amount of upper solution and tests with ultraviolet-visual spectrometer.Centrifugal gained solid is placed 50 ℃ of dryings down.Promptly obtain sample B8.
The time that the medicament slow release process of the test discharges fully with embodiment 1. medicines is 10h.
Embodiment 9
Synthetic test is with embodiment 1.
Medicine absorption: the 0.9g norfloxacin is added in the 30mL absolute methanol, and making the concentration of norfloxacin is 30.0 mg/mL, obtains solution A 9.Getting the 0.3g particle size is that the 100nm sieve sample joins in the solution A 9, stirs centrifugalize after 0.5 day under the room temperature, gets a certain amount of upper solution and tests with ultraviolet-visual spectrometer.Centrifugal gained solid is placed 50 ℃ of dryings down.Promptly obtain sample B9.
The time that the medicament slow release process of the test discharges fully with embodiment 1. medicines is 12h.
Claims (4)
1, the application of a kind of pure silicon based monodisperse spherical mesoporous molecular sieve in medicament slow release is characterized in that comprising the steps:
(1). medicine is joined in the organic solvent, and making drug concentrations is 10.0-40.0mg/mL, obtains solution A;
(2). will have six side's phase structures, aperture at 2.0-5.0nm, specific surface 800-1500m
2/ g etc., spherical particle size are in the solution A that the pure silicon based monodisperse spherical mesoporous molecular sieve of 100-1000nm joins, make molecular sieve: solution A is 0.2-0.5g:20.0-50.0mL, stir centrifugalize after 0.5-3 days under the room temperature, centrifugal gained solid is placed under 40-60 ℃ be drying to obtain solid powder.
2, the application of a kind of pure silicon based monodisperse spherical mesoporous molecular sieve as claimed in claim 1 in medicament slow release is characterized in that described solid powder carries out tabletting under 2.0-4.0MPa pressure.
3, the application of a kind of pure silicon based monodisperse spherical mesoporous molecular sieve as claimed in claim 1 or 2 in medicament slow release is characterized in that described medicine is antibiotic, anti-pathogenic microorganism medicine, antitumor medication, cardiovascular drugs, medicine for respiratory system, consumption systems medicine or blood system medicine.
4, the application of a kind of pure silicon based monodisperse spherical mesoporous molecular sieve as claimed in claim 1 or 2 in medicament slow release is characterized in that described organic solvent is methanol, ethanol, acetone, normal hexane or chloroform.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106913546A (en) * | 2015-12-28 | 2017-07-04 | 山东新时代药业有限公司 | A kind of Minodronic acid tablets of Fast Stripping and preparation method thereof |
| CN111603564A (en) * | 2020-06-03 | 2020-09-01 | 太原师范学院 | High-load Y-type molecular sieve-adriamycin nano-drug and preparation method and application thereof |
-
2007
- 2007-03-20 CN CN 200710061610 patent/CN101020058A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106913546A (en) * | 2015-12-28 | 2017-07-04 | 山东新时代药业有限公司 | A kind of Minodronic acid tablets of Fast Stripping and preparation method thereof |
| CN106913546B (en) * | 2015-12-28 | 2021-06-22 | 山东新时代药业有限公司 | Fast-dissolving minodronic acid tablet and preparation method thereof |
| CN111603564A (en) * | 2020-06-03 | 2020-09-01 | 太原师范学院 | High-load Y-type molecular sieve-adriamycin nano-drug and preparation method and application thereof |
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