CN108888778B - 基于近红外Aza-Bodipy复合的介孔二氧化硅纳米复合材料及其制备方法和应用 - Google Patents
基于近红外Aza-Bodipy复合的介孔二氧化硅纳米复合材料及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开一种基于近红外Aza‑Bodipy复合的介孔二氧化硅纳米复合材料及其制备方法和应用，该纳米复合材料内包括作为载体的嵌有富勒烯的介孔二氧化硅纳米粒子和装载在该纳米粒子孔道中的Aza‑Bodipy材料，该纳米复合粒子的粒径为50‑70nm。富勒烯嵌入的二氧化硅纳米复合材料粒径小、比表面高、负载量大、生物相容性好，作为一个良好的搭载平台成功解决了Aza‑Bodipy材料生物相容性差的问题，使得新制备的纳米复合粒子同时具有纳米材料的优势和光热转化性能，可作为光热材料应用于癌细胞和肿瘤的光热治疗中，具有较好的体内生物医学应用前景；且具有制备工艺简单、光热转化效率高和适用范围广等技术优势。
Description
技术领域
本发明属于纳米材料制备技术和特种材料技术领域，具体涉及一种基于近红外Aza-Bodipy复合的介孔二氧化硅纳米复合材料及其制备方法和应用。
背景技术
在癌症治疗中，传统的手术疗法、放射疗法和化学疗法会伤害到体内的正常组织并带来一些其他的副作用，近年来，新的治疗手段，如利用近红外光热转换的光热疗法已被研究应用于癌症治疗中。光热疗法的基本原理是在激光照射条件下，利用光热转换产生的高热量来破坏、消除癌细胞。光热治疗技术的关键是开发生物相容、高效、稳定的光热转换材料。
光热材料主要包括无机材料和有机材料。无机材料主要集中在以金、银、钯为基础的新型金属纳米颗粒等半导体纳米材料上，这些无机材料作为光热治疗材料时存在着不可忽略的问题，如金属纳米粒子的生物代谢差、长期毒性。有机光热试剂则具有良好的生物稳定性、光学稳定性和较高的光热转换效率，所以有机光热试剂的开发应用在近年来备受关注。
氮杂氟硼荧(Aza-Bodipy)衍生物是一类重要的有机染料，因其具有较长的吸收和发射波长、良好的光稳定性、窄的半峰宽等特点，在生物分析领域具有广阔的应用前景，是近年来受到广泛关注的一类新型近红外荧光染料，与具有相似结构的Bodipy染料相比，Aza-Bodipy通过其母环上中心氮原子的引入减少了HOMO-LUMO能级，使其吸收及荧光光谱红移了100nm以上，表现出更长波长的吸收，这使得它们成为有前景的光热材料。然而，大多数Aza-Bodipy衍生物具有一定程度的辐射跃迁和较差的水溶性，这种不可忽视的辐射跃迁通常会导致荧光的产生，这会损害非辐射跃迁并随后降低光热转换效率；这些特征阻碍了Aza-Bodipy作为光热材料在体内生物医学的应用；为了发挥Aza-Bodipy染料的光热作用，有必要寻找合适的载体来将其递送至肿瘤位置。
介孔二氧化硅材料是一种具有高比表面积、大孔容量、形貌和尺寸可控的新型无机生物材料，介孔二氧化硅纳米材料兼具了介孔材料和纳米材料的双重特性，具有非常高的化学稳定性、生物相容性、合成方便和成本低廉等特点，除了在传统的介孔材料应用领域外，在其他领域如生物医药和基因工程等方面也显示了极大的应用前景；富勒烯是一种新型含碳纳米材料，富勒烯及其衍生物具有抗氧化活性、细胞保护作用、抗菌活性、抗病毒作用、载带药物和肿瘤治疗等活性，因此，在生物和医学领域应用广泛，将富勒烯(C70)嵌入介孔二氧化硅基质的中心可形成水溶性良好的纳米复合材料，将其与Aza-Bodipy材料结合就可赋予Aza-Bodipy材料好的水溶性，实现Aza-Bodipy的光热作用，得到的Aza-Bodipy复合的介孔二氧化硅复合纳米材料将有望用于癌细胞和肿瘤的光热治疗。
发明内容
本发明的目的在于解决现有技术中的不足，提供一种基于近红外Aza-Bodipy复合的介孔二氧化硅纳米复合材料，富勒烯嵌入的介孔二氧化硅纳米复合材料具有良好的生物相容性，是一个良好的载体平台，装载上光热试剂近红外Aza-Bodipy材料后，具有光热性能，并解决了Aza-Bodipy材料生物相容性差的问题，为癌细胞和肿瘤治疗技术领域提供了更加优越的医学材料。
本发明的具体技术方案如下所述：
一种基于近红外Aza-Bodipy复合的介孔二氧化硅纳米复合材料，包括作为载体的嵌有富勒烯的介孔二氧化硅纳米粒子和装载在该纳米粒子孔道中的Aza-Bodipy材料，该纳米复合粒子的粒径为50-70nm。
进一步地，所述Aza-Bodipy材料的结构如下：
进一步地，该纳米复合材料的具体制备步骤为：
1)将TritonX-100、正己醇、环己烷、去离子水以一定的体积比混合在一起，形成反相微乳液；
2)将C70富勒烯溶解在甲苯溶液里并加入到上述反相微乳液中，之后添加氢氧化铵和四乙氧基硅烷，在室温下反应40-50h；
3)加入乙醇以停止反应，所得产物用乙醇离心洗涤三次以获得富勒烯嵌入的二氧化硅纳米材料；
4)将浓度为1mg/mL的富勒烯嵌入的二氧化硅纳米材料乙醇溶液与浓度为1mg/mL的Aza-Bodipy的乙醇溶液在室温下剧烈搅拌反应24h，即得目标物质。
进一步地，所述步骤1)中TritonX-100、正己醇、环己烷和去离子水的体积比为5：2.5：50：1。
进一步地，所述步骤4)中富勒烯嵌入的二氧化硅纳米材料乙醇溶液与Aza-Bodipy的乙醇溶液的体积比为1：1。
进一步地，上述制备方法的步骤2)中的C70富勒烯结构式如下：
进一步地，该纳米复合材料可作为光热材料应用于癌细胞和肿瘤的光热治疗中。
本发明具有以下有益效果：
1、本发明所述的富勒烯嵌入的二氧化硅纳米复合材料粒径小、比表面高、负载量大、生物相容性好，作为一个良好的搭载平台成功解决了Aza-Bodipy材料生物相容性差的问题，使得新制备的纳米复合材料同时具有纳米材料的优势和光热转化性能，可作为光热材料应用于癌细胞和肿瘤的光热治疗中，具有较好的体内生物医学应用前景；
2、所述纳米复合材料的制备方法简单、原料丰富、适用范围广、可用于工业化生产。
附图说明
图1是本发明实施例2中获得的C70S@Bodipy材料的扫描电子显微镜图；
图2是本发明实施例2中获得的C70S@Bodipy材料的透射电子显微镜图；
图3是本发明实施例2中获得的C70S@Bodipy材料的紫外-可见吸收光谱图；
图4是本发明实施例2中对C70S@Bodipy材料进行光热测试后获得的不同浓度的材料经激光照射后温度随时间变化的统计图；
图5是本发明实施例2中对C70S@Bodipy材料进行光热测试后获得的光稳定性图。
具体实施方式
以下实施例进一步说明本发明的内容，但不应理解为对本发明的限制。在不背离本发明实质的情况下，对本发明方法、步骤或条件所作的修改和替换，均属于本发明的范围。
实施例1、基于近红外Aza-Bodipy复合的富勒烯嵌入的介孔二氧化硅纳米复合材料的制备：
(1)将1mL Triton X-100，0.5mL正己醇，10mL环己烷和0.2mL去离子水混合在一起以形成反相微乳液；
(2)将4mg C70富勒烯溶解在甲苯溶液里并加入到上述反相微乳液中，之后缓慢添加氢氧化铵和四乙氧基硅烷，在室温下反应48h；
(3)在样品中加入2mL乙醇以停止反应，所得产物用乙醇离心洗涤三次以获得富勒烯嵌入的二氧化硅纳米材料；
(4)将1mL浓度为1mg/mL的富勒烯嵌入的二氧化硅纳米材料乙醇溶液与1mL浓度为1mg/mL的Aza-Bodipy的乙醇溶液在室温下剧烈搅拌反应24h，即得目标物质。
实施例2：为了更好地理解本实施例1获得的目标物质的性能，通过以下测试进行表征：
1.近红外Aza-Bodipy复合的富勒烯嵌入的介孔二氧化硅(即C70S@Bodipy)纳米复合材料的形貌和粒径分布测试：
图1为本发明提供的C70S@Bodipy纳米复合材料的扫描电子显微镜图。
具体测试步骤是：取20μL浓度为0.2mg/mL的样品溶液滴在硅片上，待样品干燥后进行形貌测试，C70S@Bodipy纳米粒子的粒径为50-70nm，从图1的扫描电子显微镜图示结果可以看出本发明提供的纳米粒子的粒径均一，分散性良好；
图2为本发明提供的C70S@Bodipy纳米复合材料的透射电子显微镜图。
具体测试步骤是：取20μL浓度为0.2mg/mL的样品溶液滴在铜网上，待样品干燥后进行形貌测试，C70S@Bodipy纳米粒子的粒径为50-70nm，从透射电子显微镜图示结果可以看出本发明提供的纳米粒子的粒径均一，与扫描电子显微镜图示结果一致。
2.吸收光谱测试
图3为本发明提供的C70S@Bodipy纳米复合材料的紫外可见吸收光谱图。具体测试步骤是：分别取2mL样品水溶液和近红外Aza-Bodipy材料的二氯甲烷溶液于比色皿中，测得两种材料的紫外可见吸收光谱。由图3可知,C70S@Bodipy的吸收峰与近红外Aza-Bodipy材料的吸收峰一致，并且发生了红移，说明纳米粒子成功吸附了Aza-Bodipy。
3.光热性能测试
将实施例1中得到的C70S@Bodipy材料配制成不同浓度的溶液(0，20，40，60和80μM)，在808nm的激光器下用0.5W/cm2的功率光照7min，所得到的不同浓度的材料的温度随时间的变化曲线如图4所示，60μM浓度的C70S@Bodipy材料的光稳定性图如图5所示。
从图4和图5中可知，制得的C70S@Bodipy材料具有明显的光热功能，且随着反应材料浓度的增加和光照时间的延长，材料的升温愈加明显，并且具有一定的光热稳定性。根据Roper’s方法计算光热转换效率，可知光热转换效率为34.5％，该种材料将有望作为光热材料用于癌细胞和肿瘤的光热治疗中。
以上显示和描述了本发明的基本原理、主要特征及优点。但是以上所述仅为本发明的具体实施例，本发明的技术特征并不局限于此，任何本领域的技术人员在不脱离本发明的技术方案下得出的其他实施方式均应涵盖在本发明的专利范围之中。
Claims (3)
1.一种基于近红外Aza-Bodipy复合的介孔二氧化硅纳米复合材料的制备方法，其特征在于，具体制备步骤为：
1)将TritonX-100、正己醇、环己烷、去离子水以5：2.5：50：1的体积比混合在一起，形成反相微乳液；
2)将C70富勒烯溶解在甲苯溶液里并加入到上述反相微乳液中，之后添加氢氧化铵和四乙氧基硅烷，在室温下反应40-50h；
3)加入乙醇以停止反应，所得产物用乙醇离心洗涤三次以获得富勒烯嵌入的二氧化硅纳米材料；
4)以1:1的体积比将浓度为1mg/mL的富勒烯嵌入的二氧化硅纳米材料乙醇溶液与浓度为1mg/mL的Aza-Bodipy的乙醇溶液在室温下剧烈搅拌反应24h，即得目标物质，Aza-Bodipy材料装载在嵌有富勒烯的介孔二氧化硅纳米粒子的孔道中；所得目标物质的粒径为50-70nm。
2.如权利要求1所述的基于近红外Aza-Bodipy复合的介孔二氧化硅纳米复合材料的制备方法，其特征在于，所述Aza-Bodipy材料的结构如下：
3.如权利要求1所述的基于近红外Aza-Bodipy复合的介孔二氧化硅纳米复合材料的制备方法，其特征在于，所述步骤2)中的C70富勒烯结构式如下：
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| BODIPY-doped silica nanoparticles with reduced dye leakage and enhanced singlet oxygen generation;Zhuyuan Wang et al.;《Scientific Reports》;20150727;第5卷;第12602页 * |
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