CN101912616B - Alpha-tocopheryl mesoporous silicon compound using supercritical CO2 injection method and preparation method thereof - Google Patents
Alpha-tocopheryl mesoporous silicon compound using supercritical CO2 injection method and preparation method thereof Download PDFInfo
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- CN101912616B CN101912616B CN2010102577462A CN201010257746A CN101912616B CN 101912616 B CN101912616 B CN 101912616B CN 2010102577462 A CN2010102577462 A CN 2010102577462A CN 201010257746 A CN201010257746 A CN 201010257746A CN 101912616 B CN101912616 B CN 101912616B
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Abstract
The invention discloses an alpha-tocopheryl mesoporous silicon compound using a supercritical CO2 injection method and a preparation method thereof, belonging to the technical field of medicines. The preparation method comprises a step of preparing alpha-tocopheryl and mesoporous silicon into the alpha-tocopheryl mesoporous silicon compound under the environment of carbon dioxide by means of the supercritical carbon dioxide injection method. The drug-loading rate of the compound prepared by using the method of the invention is 0.58-0.76g/g. The alpha-tocopheryl/mesoporous silicon compound prepared by using the supercritical CO2 injection method can be prepared into food additives with various functions. The process has the advantages of simple process for preparing the compound, high drug-loading rate and no solvent residues, and the compound is a solid formulation.
Description
Technical field
What the present invention relates to is complex of a kind of medical technical field and preparation method thereof, specifically is a kind of supercritical CO
2Injection method alpha-tocopherol mesoporous silicon compound and preparation method thereof.
Background technology
Tocopherol has another name called vitamin E, is a kind of fatsoluble vitamin.Natural Vitamin E has 8 kinds of analog, and is wherein commonly used and biological activity is the highest with alpha-tocopherol.Except that having significant non-oxidizability, alpha-tocopherol can also be eliminated intravital free radical, angiocardiopathy preventing and cancer.Because the free phenolic hydroxyl group of alpha-tocopherol is prone at oxidant, generate quinoid under the action of ultraviolet ray and lost efficacy, therefore be necessary that the polymer of tocopherol and biocompatibility is processed complex improves its stability; In addition, tocopherol is in a liquid state at normal temperatures, and extremely difficulty is disperseed in water, processes solid composite and can also improve its dispersibility in water.
Mesoporous silica nano-particle has specific pore passage structure, big specific surface area, thereby have good permeability, and adsorptivity is commonly used to do the carrier of drug sustained release system.The common method of preparation mesoporous silicon compound is a liquid immersion method.But in the process of preparation complex, adopt liquid immersion method may destroy tocopherol, and possible organic solvent residual, limited the application of product.To the problems referred to above, supercritical fluid technology is suggested and is used to prepare nano-complex, and supercritical fluid technology has been widely used in the preparation research of active substance as a kind of technology of cleaning.Critical temperature that supercritical carbon dioxide is moderate and noble gas character can be avoided thermal sensitivity and the destruction that is prone to oxidized material; Its low viscosity, low surface tension and high osmosis and need not subsequent treatment have been saved the time greatly and have been improved efficient.At present, do not find to use supercritical CO as yet
2Injection method prepares the mesoporous silicon-immobilized nanocrystal composition of alpha-tocopherol.
Summary of the invention
The present invention is directed to the above-mentioned deficiency that prior art exists, a kind of supercritical CO is provided
2Injection method alpha-tocopherol mesoporous silicon compound and preparation method thereof, its drug loading are 0.58～0.76g/g.Adopt supercritical CO
2Injection method prepares alpha-tocopherol/mesoporous silicon-immobilized nanocrystal composition, can be prepared into various function food additives.This prepared complex flow process is simple, and drug loading is high, and no solvent residue is solid dosage forms.
The present invention realizes that through following technical scheme the present invention processes the alpha-tocopherol mesoporous silicon compound through the supercritical carbon dioxide injection method with alpha-tocopherol and mesoporous silicon under carbon dioxide environment.
Described supercritical carbon dioxide injection method is meant: alpha-tocopherol and mesoporous silicon are placed feeding CO in back on the sintered plate that injects still
2Gas is to discharge the air that injects in the still, then with CO
2Pump into and inject still, after reaching supercritical temperature pressure, the ON cycle pump 1h that circulates, slowly the about 1h of pressure release promptly obtains the alpha-tocopherol mesoporous silicon compound to normal pressure then.
Described alpha-tocopherol and mesoporous silicon ratio, its mass ratio is 14: 1;
Described supercritical temperature pressure is meant: the carbon dioxide environment of 12～20Mpa and 30～55 ℃.
The component and the content of the alpha-tocopherol mesoporous silicon compound that the inventive method prepares are: it is that 0.58～0.76g and complex are pressed powder that every g complex contains alpha-tocopherol.
The present invention is simple to operate, and the alpha-tocopherol mesoporous silicon compound that makes is a solid composite, and no solvent residue can be applicable to various dosage forms or adds various food.
The specific embodiment
Elaborate in the face of embodiments of the invention down, present embodiment provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment being to implement under the prerequisite with technical scheme of the present invention.
Detection method of the present invention is a ultraviolet spectrophotometer.Ultraviolet spectrophotometer is Shanghai Spectrum Apparatus Co., Ltd.; The detection wavelength is 292cm; Solvent is a dehydrated alcohol, and standard curve is A=0.00653*C-0.01116, and the drug loading of alpha-tocopherol is the alpha-tocopherol quality/alpha-tocopherol mesoporous silicon compound quality of load.
Embodiment 1
Taking by weighing mass ratio is about 1: 14 mesoporous silicon (603m2/g, 0.84cm3/g 5.95nm) and alpha-tocopherol, is put on the sintered plate that injects the still different layers.In reaction system, lead to CO
2About 2min is to discharge the air in the still.With CO
2Pump into and inject still, wait to inject that the still temperature reaches 30 ℃, valve-off when pressure is 18MPa, the ON cycle pump; Circulate after 1 hour, close circulating pump, open valve; Slowly the about 1h of pressure release collects the granule that injects in the still to normal pressure, promptly obtains the mesoporous silicon-immobilized nanocrystal composition of alpha-tocopherol.
Drug loading is measured: take by weighing the mesoporous silicon-immobilized nanocrystal composition of a certain amount of alpha-tocopherol, be dissolved in the dehydrated alcohol, survey solution absorbency at the 292cm place with ultraviolet spectrophotometer.According to the standard curve A=0.00653*C-0.01116 of alpha-tocopherol under this wavelength, calculating drug loading is 67.76%.The result lists in the table 1.
Embodiment 2
Taking by weighing mass ratio is about 1: 14 mesoporous silicon (603m2/g, 0.84cm3/g 5.95nm) and alpha-tocopherol, is put on the sintered plate that injects the still different layers.In reaction system, lead to CO
2About 2min is to discharge the air in the still.With CO
2Pump into and inject still, wait to inject that the still temperature reaches 35 ℃, valve-off when pressure is 12MPa, the ON cycle pump; Circulate after 1 hour, close circulating pump, open valve; Slowly the about 1h of pressure release collects the granule that injects in the still to normal pressure, promptly obtains the mesoporous silicon-immobilized nanocrystal composition of alpha-tocopherol.Drug loading is measured with embodiment 1, and the drug loading that calculates is 63.86%, and the result lists in the table 1.
Embodiment 3
Take by weighing mass ratio and be about 1: 14 mesoporous silicon (603m
2/ g, 0.84cm
3/ g 6nm) and alpha-tocopherol, is put on the sintered plate that injects the still different layers.In reaction system, lead to CO
2About 2min is to discharge the air in the still.With CO
2Pump into and inject still, wait to inject that the still temperature reaches 35 ℃, valve-off when pressure is 15MPa, the ON cycle pump; Circulate after 1 hour, close circulating pump, open valve; Slowly the about 1h of pressure release collects the granule that injects in the still to normal pressure, promptly obtains the mesoporous silicon-immobilized nanocrystal composition of alpha-tocopherol.Drug loading is measured with embodiment 1, and the drug loading that calculates is 69.53%, and the result lists in the table 1.
Embodiment 4
Take by weighing mass ratio and be about 1: 14 mesoporous silicon (603m
2/ g, 0.84cm
3/ g 6nm) and alpha-tocopherol, is put on the sintered plate that injects the still different layers.In reaction system, lead to CO
2About 2min is to discharge the air in the still.With CO
2Pump into and inject still, wait to inject that the still temperature reaches 35 ℃, valve-off when pressure is 18MPa, the ON cycle pump; Circulate after 1 hour, close circulating pump, open valve; Slowly the about 1h of pressure release collects the granule that injects in the still to normal pressure, promptly obtains the mesoporous silicon-immobilized nanocrystal composition of alpha-tocopherol.Drug loading is measured with embodiment 1, and the drug loading that calculates is 76.14%, and the result lists in the table 1.
Embodiment 5
Take by weighing mass ratio and be about 1: 14 mesoporous silicon (86m
2/ g, 0.54cm
3/ g 25nm) and alpha-tocopherol, is put on the sintered plate that injects the still different layers.In reaction system, lead to CO
2About 2min is to discharge the air in the still.With CO
2Pump into and inject still, wait to inject that the still temperature reaches 35 ℃, valve-off when pressure is 18MPa, the ON cycle pump; Circulate after 1 hour, close circulating pump, open valve; Slowly the about 1h of pressure release collects the granule that injects in the still to normal pressure, promptly obtains the mesoporous silicon-immobilized nanocrystal composition of alpha-tocopherol.Drug loading is measured with embodiment 1, and the drug loading that calculates is 58.30%, and the result lists in the table 1.
Embodiment 6
Take by weighing mass ratio and be about 1: 14 mesoporous silicon (576m
2/ g, 0.85cm
3/ g 6nm) and alpha-tocopherol, is put on the sintered plate that injects the still different layers.In reaction system, lead to CO
2About 2min is to discharge the air in the still.With CO
2Pump into and inject still, wait to inject that the still temperature reaches 35 ℃, valve-off when pressure is 18MPa, the ON cycle pump; Circulate after 1 hour, close circulating pump, open valve; Slowly pressure release is collected the granule that injects in the still to normal pressure, promptly obtains the mesoporous silicon-immobilized nanocrystal composition of alpha-tocopherol.Drug loading is measured with embodiment 1, and the drug loading that calculates is 73.05%, and the result lists in the table 1.
Embodiment 7
Take by weighing mass ratio and be about 1: 14 mesoporous silicon (449m
2/ g, 1.95cm
3/ g 17nm) and alpha-tocopherol, is put on the sintered plate that injects the still different layers.In reaction system, lead to CO
2About 2min is to discharge the air in the still.With CO
2Pump into and inject still, wait to inject that the still temperature reaches 35 ℃, valve-off when pressure is 18MPa, the ON cycle pump; Circulate after 1 hour, close circulating pump, open valve; Slowly the about 1h of pressure release collects the granule that injects in the still to normal pressure, promptly obtains the mesoporous silicon-immobilized nanocrystal composition of alpha-tocopherol.Drug loading is measured with embodiment 1, and the drug loading that calculates is 79.88%, and the result lists in the table 1.
Embodiment 8
Take by weighing mass ratio and be about 1: 14 mesoporous silicon (603m
2/ g, 0.84cm
3/ g 6nm) and alpha-tocopherol, is put on the sintered plate that injects the still different layers.In reaction system, lead to CO
2About 2min is to discharge the air in the still.With CO
2Pump into and inject still, wait to inject that the still temperature reaches 35 ℃, valve-off when pressure is 20MPa, the ON cycle pump; Circulate after 1 hour, close circulating pump, open valve; Slowly pressure release is collected the granule that injects in the still to normal pressure, promptly obtains the mesoporous silicon-immobilized nanocrystal composition of alpha-tocopherol.Drug loading is measured with embodiment 1, and the drug loading that calculates is 74.93%, and the result lists in the table 1.
Embodiment 9
Take by weighing mass ratio and be about 1: 14 mesoporous silicon (603m
2/ g, 0.84cm
3/ g 6nm) and alpha-tocopherol, is put on the sintered plate that injects the still different layers.In reaction system, lead to CO
2About 2min is to discharge the air in the still.With CO
2Pump into and inject still, wait to inject that the still temperature reaches 45 ℃, valve-off when pressure is 18MPa, the ON cycle pump; Circulate after 1 hour, close circulating pump, open valve; Slowly the about 1h of pressure release collects the granule that injects in the still to normal pressure, promptly obtains the mesoporous silicon-immobilized nanocrystal composition of alpha-tocopherol.Drug loading is measured with embodiment 1, and the drug loading that calculates is 63.77%, and the result lists in the table 1.
Embodiment 10
Take by weighing mass ratio and be about 1: 14 mesoporous silicon (603m
2/ g, 0.84cm
3/ g 6nm) and alpha-tocopherol, is put on the sintered plate that injects the still different layers.In reaction system, lead to CO
2About 2min is to discharge the air in the still.With CO
2Pump into and inject still, wait to inject that the still temperature reaches 55 ℃, valve-off when pressure is 18MPa, the ON cycle pump; Circulate after 1 hour, close circulating pump, open valve; Slowly the about 1h of pressure release collects the granule that injects in the still to normal pressure, promptly obtains the mesoporous silicon-immobilized nanocrystal composition of alpha-tocopherol.Drug loading is measured with embodiment 1, and the drug loading that calculates is 60.55%, and the result lists in the table 1.
Table 1
| Embodiment | Temperature | Pressure | Drug loading % |
| 1 | 30 | 18 | 67.76 |
| 2 | 35 | 12 | 63.86 |
| 3 | 35 | 15 | 69.53 |
| 4 | 35 | 18 | 76.14 |
| 5 | 35 | 18 | 58.30 |
| 6 | 35 | 18 | 73.05 |
| 7 | 35 | 18 | 79.88 |
| 8 | 35 | 20 | 74.93 |
| 9 | 45 | 18 | 63.77 |
| 10 | 55 | 18 | 60.55 |
Claims (2)
1. supercritical CO
2The method for preparing of injection method alpha-tocopherol mesoporous silicon compound is characterized in that, through the supercritical carbon dioxide injection method alpha-tocopherol and mesoporous silicon is processed the alpha-tocopherol mesoporous silicon compound under carbon dioxide environment;
Described supercritical carbon dioxide injection method is meant: alpha-tocopherol and mesoporous silicon are placed feeding CO in back on the sintered plate that injects still
2Gas is to discharge the air that injects in the still, then with CO
2Pump into and inject still, after reaching supercritical temperature pressure, the ON cycle pump 1h that circulates, slowly the about 1h of pressure release promptly obtains the alpha-tocopherol mesoporous silicon compound to normal pressure then;
Described alpha-tocopherol and mesoporous silicon ratio, its mass ratio is 14: 1;
Described supercritical temperature pressure is meant: the carbon dioxide environment of 12～20Mpa and 30～55 ℃.
2. supercritical CO
2Injection method alpha-tocopherol mesoporous silicon compound is characterized in that, prepares through the said method of claim 1, and the mass percentage content of alpha-tocopherol wherein is 58%～76%.
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