二氧化硅基杂化材料的设计制备及其在药物可控释放中的应用
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摘要
本论文的目的是设计制备二氧化硅基可控释放材料来研究药物的可控释放机理,控制水溶性小分子药物的释放,在提高药物负载量的同时,找到一种简单、灵活、有效的控制药物释放的方法。
为深入理解可控释放机理,以酸碱指示剂为可控释放的活性成分,研究其在SiO_2及杂化SiO_2凝胶中的酸碱响应及释放行为。在凝胶制备的过程中采用Si(OC_2H_5)_4(TEOS),(C_2H_5O)_3Si(CH_2)_2CH_3(PTES)和(CH3_O)_3Si(CH_2)_6Si(OCH_3)_3(TSH)为前驱物。实验结果表明具有有机官能团的有机硅的加入减小了凝胶的孔径和孔体积,因而抑制了指示剂的释放,但对凝胶中指示剂的酸碱响应没有明显影响。总的来说,指示剂从凝胶中的释放量在酸性溶液中的小于在碱性溶液中的;在酸性溶液中的整个释放过程,以及在碱性溶液中释放的起始阶段,指示剂从凝胶中的释放量具有相同的顺序,即TEOS凝胶> TEOS/PTES凝胶> TEOS/TSH凝胶。整个释放过程受指示剂从凝胶中的扩散控制,释放主要受凝胶的孔结构、凝胶与指示剂之间的相互作用、以及指示剂溶解度的影响。
为找到一个可以有效控制水溶性小分子药物释放的凝胶体系,研究了水杨酸钠(SS)从(CH3O)3Si(CH2)3NH(CH2)3Si(OCH3)3(TSPA)凝胶或TSPA/TEOS杂化凝胶中的释放行为。实验结果表明通过调节TSPA和TEOS的比例可以很容易控制SS的释放。在制备凝胶时增大TSPA与TEOS的比例可以降低凝胶的比表面积和孔体积,同时加强了药物和凝胶基质之间的相互作用,达到有效降低药物释放的效果。TSPA既能溶于水,又能溶于常见的有机溶剂,以其为前驱物制备的凝胶既适用于亲水药物、又适用于疏水药物的可控释放,尤其是适用于水溶性小分子药物的释放。
为了提高药物的负载量,同时找到一种简单、灵活、有效的控制药物释放的方法,首先制备了负载维生素B1(VB1)的介孔SiO2压片,然后在压片表面涂了一系列溶胶-凝胶膜后,研究VB1的释放行为,综合考察了涂膜前驱物的种类、涂膜液组成、涂膜次数、干燥温度和释放介质对VB1可控释放的影响。研究结果表明,VB1的释放可以比较容易地通过改变涂膜前驱物的种类和涂膜次数得到控制。这种压片之后涂膜的方法是一种灵活有效的控制药物释放的方法,既通过介孔SiO2提高了药物的负载量,又通过改变涂膜条件灵活而有效地控制了药物的释放。
The purpose of this thesis is to design and prepare some silica-based materials to study the drug release mechanisms, to control the release of water-soluble drugs of small molecules, to raise the drug loading in the carrier materials, and at the same time to find an easy, flexible, and effective strategy to control the drug release.
In order to understand the release mechanisms, the reactivity and release of acid-base indicators entrapped in silica and hybrid silica gels were studied. Tetraethoxysilane (TEOS), n-propyltriethoxysilane (PTES), and bis(trimethoxysilyl)hexane (TSH) were used as gel precursors. The experimental results suggest that adding the organosilanes lower the pore size and pore volume of the gels and therefore, suppress the indicator release, but do not present any obvious effects on the acid-base reactivity of the entrapped indicators. In general more indicators were found to release in basic solutions than in acidic solutions. For all the entrapped indicators in acidic solutions through the while release process, and in basic solutions at the beginning of the release, the indicator release was found to follow the sequence of TEOS Gel > TEOS/PTES Gel > TEOS/TSH Gel. The overall release process was found to be diffusion-controlled, and the release was mainly affected by the textural properties of the gels, the interactions between the gel matrices and the indicators, and the indicator solubility.
In order to find a good recipe to effectively control the release of water-soluble drugs of small molecules, the controlled release of sodium salicylate (SS) from the gels derived from bis(trimethoxysilylpropyl)amine (TSPA) or the mixture of TSPA with tetraethoxysilane (TEOS) was investigated. The experimental results suggest that the release of SS can be easily controlled by adjusting the ratio between TSPA and TEOS. Increasing the ratio between TSPA and TEOS lowers the surface area and pore volume of the gels, while enhances the interactions between the drug and the gel matrix, therefore, reduces the release rate of the drug effectively. TSPA can dissolve in both water and common organic solvents. It was found to be a very convenient and effective precursor for the preparation of gels for controlled release of both hydrophilic and hydrophobic drugs, especially water-soluble drugs of small molecules.
In order to raise the drug loading in the carrier materials, and at the same time to find an easy, flexible, and effective strategy to control the drug release, the controlled release of vitamin B1 (VB1, thiamine hydrochloride) from mesoporous silica tablets coated with a series of sol-gel films were investigated. The effects of organosilane type and concentration, coating time, drying temperature, and release media on VB1 release from the coated mesoporous silica tablets were examined comprehensively. VB1 release decreased with the increase in coating time and drying temperature. The experimental results show that drug release can be easily controlled by changing the organosilane type and coating time. The method used in this study appears to be an effective and flexible way to control drug release because of the high drug loading in the mesoporous silica carrier and the ease control of the release by manipulating the coatings.
为深入理解可控释放机理,以酸碱指示剂为可控释放的活性成分,研究其在SiO_2及杂化SiO_2凝胶中的酸碱响应及释放行为。在凝胶制备的过程中采用Si(OC_2H_5)_4(TEOS),(C_2H_5O)_3Si(CH_2)_2CH_3(PTES)和(CH3_O)_3Si(CH_2)_6Si(OCH_3)_3(TSH)为前驱物。实验结果表明具有有机官能团的有机硅的加入减小了凝胶的孔径和孔体积,因而抑制了指示剂的释放,但对凝胶中指示剂的酸碱响应没有明显影响。总的来说,指示剂从凝胶中的释放量在酸性溶液中的小于在碱性溶液中的;在酸性溶液中的整个释放过程,以及在碱性溶液中释放的起始阶段,指示剂从凝胶中的释放量具有相同的顺序,即TEOS凝胶> TEOS/PTES凝胶> TEOS/TSH凝胶。整个释放过程受指示剂从凝胶中的扩散控制,释放主要受凝胶的孔结构、凝胶与指示剂之间的相互作用、以及指示剂溶解度的影响。
为找到一个可以有效控制水溶性小分子药物释放的凝胶体系,研究了水杨酸钠(SS)从(CH3O)3Si(CH2)3NH(CH2)3Si(OCH3)3(TSPA)凝胶或TSPA/TEOS杂化凝胶中的释放行为。实验结果表明通过调节TSPA和TEOS的比例可以很容易控制SS的释放。在制备凝胶时增大TSPA与TEOS的比例可以降低凝胶的比表面积和孔体积,同时加强了药物和凝胶基质之间的相互作用,达到有效降低药物释放的效果。TSPA既能溶于水,又能溶于常见的有机溶剂,以其为前驱物制备的凝胶既适用于亲水药物、又适用于疏水药物的可控释放,尤其是适用于水溶性小分子药物的释放。
为了提高药物的负载量,同时找到一种简单、灵活、有效的控制药物释放的方法,首先制备了负载维生素B1(VB1)的介孔SiO2压片,然后在压片表面涂了一系列溶胶-凝胶膜后,研究VB1的释放行为,综合考察了涂膜前驱物的种类、涂膜液组成、涂膜次数、干燥温度和释放介质对VB1可控释放的影响。研究结果表明,VB1的释放可以比较容易地通过改变涂膜前驱物的种类和涂膜次数得到控制。这种压片之后涂膜的方法是一种灵活有效的控制药物释放的方法,既通过介孔SiO2提高了药物的负载量,又通过改变涂膜条件灵活而有效地控制了药物的释放。
The purpose of this thesis is to design and prepare some silica-based materials to study the drug release mechanisms, to control the release of water-soluble drugs of small molecules, to raise the drug loading in the carrier materials, and at the same time to find an easy, flexible, and effective strategy to control the drug release.
In order to understand the release mechanisms, the reactivity and release of acid-base indicators entrapped in silica and hybrid silica gels were studied. Tetraethoxysilane (TEOS), n-propyltriethoxysilane (PTES), and bis(trimethoxysilyl)hexane (TSH) were used as gel precursors. The experimental results suggest that adding the organosilanes lower the pore size and pore volume of the gels and therefore, suppress the indicator release, but do not present any obvious effects on the acid-base reactivity of the entrapped indicators. In general more indicators were found to release in basic solutions than in acidic solutions. For all the entrapped indicators in acidic solutions through the while release process, and in basic solutions at the beginning of the release, the indicator release was found to follow the sequence of TEOS Gel > TEOS/PTES Gel > TEOS/TSH Gel. The overall release process was found to be diffusion-controlled, and the release was mainly affected by the textural properties of the gels, the interactions between the gel matrices and the indicators, and the indicator solubility.
In order to find a good recipe to effectively control the release of water-soluble drugs of small molecules, the controlled release of sodium salicylate (SS) from the gels derived from bis(trimethoxysilylpropyl)amine (TSPA) or the mixture of TSPA with tetraethoxysilane (TEOS) was investigated. The experimental results suggest that the release of SS can be easily controlled by adjusting the ratio between TSPA and TEOS. Increasing the ratio between TSPA and TEOS lowers the surface area and pore volume of the gels, while enhances the interactions between the drug and the gel matrix, therefore, reduces the release rate of the drug effectively. TSPA can dissolve in both water and common organic solvents. It was found to be a very convenient and effective precursor for the preparation of gels for controlled release of both hydrophilic and hydrophobic drugs, especially water-soluble drugs of small molecules.
In order to raise the drug loading in the carrier materials, and at the same time to find an easy, flexible, and effective strategy to control the drug release, the controlled release of vitamin B1 (VB1, thiamine hydrochloride) from mesoporous silica tablets coated with a series of sol-gel films were investigated. The effects of organosilane type and concentration, coating time, drying temperature, and release media on VB1 release from the coated mesoporous silica tablets were examined comprehensively. VB1 release decreased with the increase in coating time and drying temperature. The experimental results show that drug release can be easily controlled by changing the organosilane type and coating time. The method used in this study appears to be an effective and flexible way to control drug release because of the high drug loading in the mesoporous silica carrier and the ease control of the release by manipulating the coatings.
引文
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