CN108785686B - 基于钯纳米片双面神纳米粒子的制备方法及其应用 - Google Patents

基于钯纳米片双面神纳米粒子的制备方法及其应用 Download PDF

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CN108785686B
CN108785686B CN201810686022.6A CN201810686022A CN108785686B CN 108785686 B CN108785686 B CN 108785686B CN 201810686022 A CN201810686022 A CN 201810686022A CN 108785686 B CN108785686 B CN 108785686B
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张凌宇
李鹿
王春刚
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Northeast Normal University
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Abstract

本发明提供一种单分散双面神结构环糊精‑钯纳米片/类沸石咪唑骨架‑8(CD‑PdNS/ZIF‑8)纳米粒子的制备方法及其应用。本发明借助二维钯纳米片独特的两个大的表面，利用聚丙烯酸的导向作用，结合选择性生长及修饰的方法开发一种简单的方法制备单分散双面神结构CD‑PdNS/ZIF‑8纳米粒子，所得产品分散性好，粒径均匀，生物相容性好，在双药物输送等领域具有非常广阔的应用前景。

Description

基于钯纳米片双面神纳米粒子的制备方法及其应用
技术领域
本发明属于纳米复合材料及其应用技术领域，具体涉及一种双面神结构环糊精-钯纳米片/类沸石咪唑骨架-8(CD-PdNS/ZIF-8)纳米粒子的制备方法及其应用。
背景技术
自从1991年Pierre-Gilles de Gennes教授在诺贝尔颁奖大会上首次提出双面神粒子，这种能将两种材料本身性质、表面性质或其他性质结合到一个粒子上的特性在化学，生物学，传感学，催化学以及应用光学等领域都得到广泛的应用。尤其是与传统杂化纳米粒子，如核-壳、蛋黄-蛋壳结构纳米粒子相比，双面神纳米粒子克服了其他结构纳米材料表面单一、多重修饰时分子间相互干扰的弊端，为各个领域的科学研究带来了新的希望，特别是在生物医学方向更是得到广泛的关注。[参考文献：A.Walther,A.H.E.Müller,Chem.Rev.2013,113,5194；J.Du,R.K.O'Reilly,Chem.Soc.Rev.2011,40,2402.]尤其是基于金属的双面神纳米材料，例如金属-聚合物，金属-金属，金属-氧化物等，因为其不仅仅融合了金属的化学，表面等离子共振，电学性质，还融合了和其结合的另一个材料的性质。[参考文献：T.Chen,G.Chen,S.Xing,T.Wu,H.Chen,Chem.Mater.2010,22,3826；H.Kim,R.P.Carney,J.Reguera,Q.K.Ong,X.Liu,F.Stellacci,Adv.Mater.2012,24,3857；K.A.Kuttiyiel,K.Sasaki,G.-G.Park,M.B.Vukmirovic,L.Wu,Y.Zhu,J.G.Chen,R.R.Adzic,Chem.Commun.2017,53,1660.]但是，目前关于金属-有机金属框架(MOFs)的研究十分少。并且，现在合成基于金属的双面神纳米粒子的方法主要是在金属的部分表面选择性生长不同材料。在这些基于金属的双面神材料中，基于零维球形和一维棒状金属的双面神纳米材料报道相对比较多。据我们所知，现在还没有基于二维金属纳米片双面神纳米材料的报道。与零维和一维材料相比，二维材料具有完全不同的性质，这得益于其独特的二维形态，例如很薄的厚度，相对大的更利于生长和修饰的两个表面。因此，目前亟需开发新的方法，合成基于金属纳米片的双面神纳米材料。
钯纳米片是一种典型的二维纳米材料，其具有可调控的厚度，大小，并可调节其近红外表面等离子共振峰的位置，继而使得其具有光热性能，这些独特的性质使得钯纳米材料成为一种新兴的可以在催化，癌症诊疗方面具有很大应用潜力纳米材料，也是国内外研究的热点。[参考文献：X.Huang,S.Tang,X.Mu,Y.Dai,G.Chen,Z.Zhou,F.Ruan,Z.Yang,N.Zheng,Nat.Nanotech.2010,6,28；X.Huang,S.Tang,X.Mu,Y.Dai,G.Chen,Z.Zhou,F.Ruan,Z.Yang,N.Zheng,Nat.Nanotech.2010,6,28.]目前，关于钯纳米片杂化纳米材料的光热研究主要集中于近红外第一窗口，关于可以穿透组织到更深层次的第二窗口的研究比较罕见。因此，在生物应用领域，对于基于钯纳米片的杂化纳米材料的研究，尤其在第二窗口的应用研究十分重要。近期，很多基于钯的杂化纳米材料，比如金包覆钯，银包覆钯，二氧化硅包覆钯等核壳结构纳米材料的研究，用于改善单纯钯的不利性质。[参考文献：X.Huang,S.Tang,B.Liu,B.Ren,N.Zheng,Adv.Mater.2011,23,3420；M.Chen,S.Tang,Z.Guo,X.Wang,S.Mo,X.Huang,G.Liu,N.Zheng,Adv.Mater.2014,26,8210；W.Fang,S.Tang,P.Liu,X.Fang,J.Gong,N.Zheng,Small 2012,8,3816.]但是，这些材料的合成方法大多是在整个钯纳米片上生长同一种物质。而关于在二维钯纳米片的两个相对大的表面分别修饰不同材料，比如有机金属框架和有机化合物，得到新颖的纳米结构和新的性质是个极大的挑战。而且，得到这种基于二维钯纳米片的双面神结构纳米材料能为纳米材料的合成及应用带来更多的提示。
从以上叙述中可以看出，由于钯纳米片的特殊性能，使其在纳米医药领域表现出很高的应用价值，但是，对基于二维钯纳米片的多功能复杂纳米结构构筑的研究较少，特别是对于以钯纳米片为主体材料的单分散双面神结构CD-PdNS/ZIF-8纳米粒子的构筑还未有报道。现有合成双面神结构纳米粒子方法普遍存在分散性差、纳米尺寸难调控、整体形貌较差等缺陷。因此，开发具一种简单易行，制备单分散、纳米尺寸的多功能单分散双面神结构CD-PdNS/ZIF-8纳米粒子是一个具有挑战性的新课题。
发明内容
本发明提供一种单分散双面神结构CD-PdNS/ZIF-8纳米粒子的制备方法及其应用。使用该方法制备的单分散双面神结构CD-PdNS/ZIF-8纳米粒子具有分散性好、粒径均匀在纳米尺度、生物相容性好等特点，可用于具有不同性质(亲水和疏水)的双药物输送等领域。
本发明单分散双面神结构CD-PdNS/ZIF-8纳米粒子的制备方法包括如下步骤：
(1)取32mg乙酰丙酮钯，20mg柠檬酸，120mg十六烷基三甲基溴化铵，60mg聚乙烯吡咯烷酮(K30)溶解在20mL二甲基甲酰胺中在氩气条件下搅拌1h。然后加入200mg六羰基钨。在80℃条件下搅拌1h。然后加入丙酮离心，分散在10mL去离子水里。
(2)室温条件下，取上述1mL钯纳米片水溶液，在其中加入10～20μL聚丙烯酸(Mw＝1800，0.2mg mL-1)，然后，加入8～30μL氨水(25-28％)，再滴加20mL异丙醇。搅拌12～24h使其混合均匀。
(3)取25～50μL硝酸锌(0.1M)和25～50μL的2-甲基咪唑(0.1M)加入到(2)中，反应12～24h后8000～9000rpm离心8～10min后重新分散在乙醇中待用。
(4)在室温条件下，取1mL含有1～2mg的巯基-环糊精的二甲基亚砜溶液加入到(3)中，搅拌12～24h。
(5)将步骤(4)得到的混合溶液进行离心分离(8000～9000rpm，8～10min)，所得固体再用水洗涤1～3次，即得CD-PdNS/ZIF-8纳米粒子。
本发明具有如下优点：
1.本发明合成方法简单，合成高分散、粒径为纳米尺度均一的单分散双面神结构CD-PdNS/ZIF-8纳米粒子。在此反应过程中，借助二维钯纳米片独特的两个大的表面，利用聚丙烯酸的导向作用，结合再生长和修饰得到两个表面分别具有不同材料的、形貌独特的环糊精修饰钯纳米片和ZIF-8结合的多功能纳米粒子。
2.本发明得到的单分散双面神结构CD-PdNS/ZIF-8纳米粒子，粒径均匀、为纳米尺度，可在双面神纳米粒子的两侧分别负载两种不同性质药物(亲水和疏水)用于双药物输送。
3.由于双面神的特殊结构，相比单纯钯纳米片，双面神结构CD-PdNS/ZIF-8纳米粒子具有更大载药量，且可以在其两边分别负载两种具有不同性质药物，并通过光热调节释放及光热治疗。
附图说明
图1、为本发明制备得到的单分散双面神结构CD-PdNS/ZIF-8纳米粒子透射电镜图片，插图为单个单分散双面神结构CD-PdNS/ZIF-8纳米粒子透射电镜图片；
图2、为本发明制备得到的单分散双面神结构CD-PdNS/ZIF-8纳米粒子的X射线衍射图谱；
图3单分散双面神结构CD-PdNS/ZIF-8纳米粒子对Balb/c鼠的体内光热成像图片；
图4、负载阿霉素和喜树碱双药物单分散双面神结构CD-PdNS/ZIF-8纳米粒子对Balb/c鼠的肿瘤抑制效果。
具体实施方式
下面结合具体实施例进一步阐述本发明，实施例仅用于说明本发明而不用于限制本发明的保护范围。
具体实施例
实施例1：
在室温条件下，取钯纳米片1mL水溶液，在其中加入10μL聚丙烯酸(Mw＝1800，0.2mg mL-1)，然后，加入15μL氨水(25-28％)，再滴加20mL异丙醇。搅拌12h使其混合均匀，然后加入50μL硝酸锌(0.1M)和50μL的2-甲基咪唑(0.1M)，反应24h后9000rpm离心10min后重新分散在乙醇中，再加入1mL含有1mg的巯基-环糊精二甲基亚砜溶液，搅拌24h。最后得到产物9000rpm离心10min后水洗涤2次，即得CD-PdNS/ZIF-8纳米粒子。
实施例2：
在室温条件下，圆底烧瓶内依次加入钯纳米片1mL水溶液，6μL聚丙烯酸(Mw＝1800，0.2mg mL-1)，10μL氨水(25-28％)，20mL异丙醇。搅拌24h后加入50μL硝酸锌(0.1M)，搅拌10min后再加入50μL的2-甲基咪唑(0.1M)，反应12h后8000rpm离心8min后重新分散在乙醇，再加入1mL含有2mg的巯基-环糊精二甲基亚砜溶液，搅拌12h。最后得到产物8000rpm离心8min后水洗涤3次，即得CD-PdNS/ZIF-8纳米粒子。
实施例3：
在室温条件下，20μL聚丙烯酸(Mw＝1800，0.2mg mL-1)加入钯纳米片1mL水溶液，超声10min，加入30μL氨水(25-28％)，搅拌10min后滴加20mL异丙醇。加入1mL含有2mg的巯基-环糊精二甲基亚砜溶液，搅拌24h。加入25μL的2-甲基咪唑(0.1M)和25μL硝酸锌(0.1M)，分两次加入，每样总计50μL。反应24h后，得到产物9000rpm离心10min后水洗涤2次，即得CD-PdNS/ZIF-8纳米粒子。
上述制备出的单分散双面神结构CD-PdNS/ZIF-8纳米粒子可用于载具有不同性质(亲水和疏水)的双药达到联合化学及光热治疗癌症的目的。
体内光热成像步骤为：将用PBS配制的双面神结构CD-PdNS/ZIF-8纳米粒子溶液通过尾静脉注射入小鼠体内。24h后，按照每千克给麻药10mL(戊巴比妥钠0.7％)的量麻醉小鼠。然后，用1064nm近红外激光照射肿瘤部位，然后用Sweden-T460SC光热成像仪获得光热图像。
体内肿瘤抑制步骤为：对小鼠分别通过尾静脉注射PBS，双面神结构CD-PdNS/ZIF-8纳米粒子，负载阿霉素和喜树碱的双面神结构CD-PdNS/ZIF-8纳米粒子(每组10只)。24h后，从以上每组选出来5只老鼠为其对应激光组，在其肿瘤部位照近红外激光(1064nm，1.0W，5min)。每2天注射药物一次，激光组是隔日照射激光。第11天处死老鼠，取出肿瘤观察其对肿瘤抑制效果。

Claims (2)

1.单分散双面神结构CD-PdNS/ZIF-8纳米粒子的制备方法，包括如下步骤：
(1)室温条件下，取1mL钯纳米片水溶液，在其中加入10～20μL，Mw为1800，浓度为0.2mgmL-1的聚丙烯酸，然后，加入8～30μL浓度为25-28％的氨水，再滴加20mL异丙醇， 搅拌12～24h使其混合均匀；
(2)取25～50μL，浓度为0.1M的硝酸锌和25～50μL浓度为0.1M的2-甲基咪唑加入到(1)中，反应12～24h后8000～9000rpm离心8～10min后重新分散在乙醇中待用；
(3)在室温条件下，取1mL含有1～2mg的巯基-环糊精的二甲基亚砜溶液加入到(2)中，搅拌12～24h；
(4)将步骤(3)得到的混合溶液进行8000～9000rpm离心8～10min分离，所得固体再用水洗涤1～3次，即得CD-PdNS/ZIF-8纳米粒子。
2.按照权利要求1所述的方法制备双面神结构CD-PdNS/ZIF-8纳米粒子。
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