CN105999277B - 一种梭形Fe3O4@C/Zn3(PO4)2纳米粒子的制备方法 - Google Patents
一种梭形Fe3O4@C/Zn3(PO4)2纳米粒子的制备方法 Download PDFInfo
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Abstract
本发明提供一种梭形Fe3O4@C/Zn3(PO4)2纳米粒子的制备方法及其应用。首先，以梭形Fe2O3纳米粒子为核，在异丙醇‑水体混合体系中，对Fe2O3纳米粒子进行PAA/Zn3(PO4)2包覆，再在氩气保护下煅烧，既可得到梭形Fe3O4@C/Zn3(PO4)2纳米粒子。所得产品分散性好、光热转换效率高、磁性强、生物相容性好，且具有孔道结构，在药物输送、光热治疗及生物成像等领域具有非常广阔的应用前景。
Description
技术领域
本发明属于纳米复合材料技术领域，具体涉及一种梭形Fe3O4@C/Zn3(PO4)2纳米粒子的制备方法。
背景技术
癌症在全球的危害不断加重，已成为本世纪威胁人类健康的头号杀手。不论性别、年龄、社会地位，癌症都直接或间接的影响着人们的生活，它已不单是个人的健康问题，还是家庭、社会密切关注的社会问题。在现有的癌症治疗方法中，药物或治疗手段对癌细胞的靶向性不高，特别是化疗等药物分子具有很高的细胞毒性，在治疗过程中不能有效区分癌细胞和正常细胞，在较高用药剂量下，杀死癌细胞的同时也对正常组织器官造成很大损伤，但是小剂量用药，又不能达到预期的治疗效果。纳米科学的快速进步，为生物医学带来了新的发展机遇。通过发展和利用纳米技术，开发新型的基于纳米材料的纳米输送系统成为了富有挑战性的课题，同时纳米输送系统在癌症的预防、诊断和治疗中的应用也将有望突破传统方法无法避免的弊端，达到高效、低副作用的治疗效果。
近期，采用无创光热治疗方法选择性地对某种癌细胞进行治疗的研究受到了广泛关注。由于体内组织对近红外光的吸收很弱，近红外光穿透皮肤的同时对健康的组织也不会造成损伤，因此借助纳米粒子的对癌细胞的靶向性作用，结合近红外光的照射，从而实现对某种癌细胞专一性的光热治疗。少数几种纳米材料对近红外光的照射有很强的吸收能力，如碳材料、金纳米壳、金纳米棒、硫化铜等。[参考文献: Y. Tao, E. G. Ju, J. S.Ren, X. G. Qu, Biomaterials, 2014, 35, 9963; A. H. Lu, X. Q. Zhang, Q. Sun,Y. Zhang, Q. W. Song, F. Schüth, C. Y. Chen, F. Cheng, Nano Res., 2016, 9,1460; M. Li, X. J. Yang, J. S. Ren, K. G. Qu and X. G. Qu, Adv. Mater., 2012,24, 1722;L. L. Li, C. F. Chen, H. Y. Liu, C. H. Fu, L. F. Tan, S. H. Wang, S.Y. Fu, X. Liu, X. W. Meng and H. Liu, Adv. Funct. Mater., 2016, 26, 4252; G.S. Hong, S. Diao, A. L. Antaris and H. J. Dai, Chem. Rev., 2015, 115, 10816.]当有近红外光照射时，这些纳米材料吸收近红外光的能量，并将其有效地转化为热能，起到杀死癌细胞的作用[[参考文献：Z. Xu, C. Li, X. Kang, J Phys Chem C, 2010, 114,16343; P. Botella, A. Corma, M. T. Navarro, J Mater Chem, 2009, 19, 3168.]。另外，具有光、磁、pH刺激响应型的无机介孔纳米粒子因在药物缓释、光学、核磁共振（MR）成像、磁靶向等方面的优异性能也备受关注[参考文献：R. J. Xing, A. A, B., S. Wang,X. L. Sun, G. Liu, L. Hou, X. Y. Chen, Nano Res., 2013, 6, 1; R. Lv, P. Yang,, F. He, S. Gai, C. Li, Y. Dai, G. Yang, J. Lin, ACS Nano, 2015, 9, 1630.]。磁性纳米颗粒作为药物载体，在外磁场的引导下集中于病患部位，进行定位变治疗，利于提高药效，减少副作用，我们一直在思考如何将碳光热材料和具有磁性的纳米粒子有效的结合起来制备出集多功能于一体新型复合结构纳米粒子，并用于肿瘤诊治一体化研究， 特别是对于以磷酸锌为主体材料的单分散梭形Fe3O4@C/Zn3(PO4)2纳米粒子的构筑还未有报道。
发明内容
本发明提供一种梭形Fe3O4@C/Zn3(PO4)2纳米粒子的制备方法。使用该方法制备的梭形Fe3O4@C/Zn3(PO4)2纳米粒子具有分散性好、光热转换效率高、磁性强、生物相容性好等特点，在药物输送、光热治疗及生物成像等领域具有非常广阔的应用前景。
本发明梭形Fe3O4@C/Zn3(PO4)2纳米粒子的制备方法包括如下步骤：
(1)准确称量1 ~ 1.5 g无水三氯化铁、0.02 ~ 0.03 g磷酸二氢钾和400 mL去离子水加入到500 mL圆底烧瓶中，然后将烧瓶置于100 oC油浴中，在磁力搅拌下回流反应70~ 80 h。
(2)将步骤（1）得到的混合溶液进行离心分离，所得固体再用去离子水和无水乙醇交替洗涤数次，沉淀在50 ~ 100 oC烘箱中烘干8 ~ 10 h，即得干燥梭形Fe2O3纳米粒子。
(3)将4 ~ 6 mg步骤（2）得到的梭形Fe2O3纳米粒子、15 ~ 20 mg聚丙烯酸、3 ~ 6mg氧化锌粉末和10 ~ 15 mL去离子水加入100 mL烧瓶中，超声分散10 ~ 20 min。
(4)在磁力搅拌下将30 ~ 50 mL异丙醇缓慢滴加入步骤（3）得到的溶液中，滴加完毕后再向溶液中加入3 ~ 6 mg磷酸二氢氨，在25 ~ 30 oC条件下搅拌反应10 ~ 15 h。
(5)将步骤（4）得到的混合溶液进行离心分离（7000 ~ 9000 rpm，8 ~ 10 min），所得沉淀在50 ~ 100 oC烘箱中烘干12 ~ 20 h。
(6)将步骤（5）得到的固体置于管式炉中，在350 ~ 450 oC氩气保护下煅烧4 ~ 6h，得到梭形Fe3O4@C/Zn3(PO4)2纳米粒子。
本发明具有如下优点：
1. 本发明得到的梭形Fe3O4@C/Zn3(PO4)2纳米粒子粒径均匀、磁性强，具有高光热转换效率和良好的生物相容性，可用于光热治疗、药物输送及生物成像。
2.本发明得到的梭形Fe3O4@C/Zn3(PO4)2纳米粒子具有超好分散性，且包覆层厚度可调。
3. 本发明得到的梭形Fe3O4@C/Zn3(PO4)2纳米粒子具有pH响应可控药物释放性能。
附图说明
图1、不同厚度梭形Fe3O4@C/Zn3(PO4)2纳米粒子的透射电镜图片；
图2、梭形Fe3O4@C/Zn3(PO4)2纳米粒子EDX谱图；
图3、梭形Fe3O4@C/Zn3(PO4)2纳米粒子XPS谱图；
图4、梭形Fe3O4@C/Zn3(PO4)2纳米粒子氮气吸附-脱附等温曲线；
图5、梭形Fe3O4@C/Zn3(PO4)2纳米粒子在溶液和细胞中的核磁成像图片；
图6、不同浓度梭形Fe3O4@C/Zn3(PO4)2纳米粒子水溶液光热效果曲线；
图7、不同浓度空白碳/梭形Fe3O4@C/Zn3(PO4)2纳米粒子、装载阿霉素的梭形Fe3O4@C/ Zn3(PO4)2纳米粒子、激光照射下装载阿霉素的梭形Fe3O4@C/Zn3(PO4)2纳米粒子及游离阿霉素溶液对Hep-A-22 细胞的体外细胞毒性。
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：
称取1.5 g无水三氯化铁、0.03 g磷酸二氢钾和400 mL去离子水加入到500 mL圆底烧瓶中，然后将烧瓶置于100 oC油浴中，在磁力搅拌下回流反应80 h。所得混合溶液进行离心分离，再用去离子水和无水乙醇交替洗涤数次，沉淀在80 oC烘箱中烘干12 h。将5 mg上述固体粉末、20 mg聚丙烯酸、5 mg氧化锌粉末和15 mL去离子水加入100 mL烧瓶中，超声分散10 min。在磁力搅拌下将30 mL异丙醇缓慢滴加入溶液中，滴加完毕后再向溶液中加入3 mg磷酸二氢氨，在25 oC条件下搅拌反应10 h。得到的混合溶液进行离心分离（7000 rpm，10 min），所得沉淀在50 oC烘箱中烘干12 h。得到的固体置于管式炉中，在350 oC氩气保护下煅烧4 h，得到梭形Fe3O4@C/Zn3(PO4)2纳米粒子。
实施例2：
称取1 g无水三氯化铁、0.02 g磷酸二氢钾和400 mL去离子水加入到500 mL圆底烧瓶中，然后将烧瓶置于100 oC油浴中，在磁力搅拌下回流反应70 h。所得混合溶液进行离心分离，再用去离子水和无水乙醇交替洗涤数次，沉淀在50 oC烘箱中烘干10 h。将4 mg上述固体粉末、15 mg聚丙烯酸、3 mg氧化锌粉末和10 mL去离子水加入100 mL烧瓶中，超声分散20 min。在磁力搅拌下将50 mL异丙醇缓慢滴加入溶液中，滴加完毕后再向溶液中加入6mg磷酸二氢氨，在30 oC条件下搅拌反应15 h。得到的混合溶液进行离心分离（8000 rpm，8min），所得沉淀在100 oC烘箱中烘干12 h。得到的固体置于管式炉中，在400 oC氩气保护下煅烧5 h，得到梭形Fe3O4@C/Zn3(PO4)2纳米粒子。
实施例3：
称取1.2 g无水三氯化铁、0.03 g磷酸二氢钾和400 mL去离子水加入到500 mL圆底烧瓶中，然后将烧瓶置于100 oC油浴中，在磁力搅拌下回流反应72 h。所得混合溶液进行离心分离，再用去离子水和无水乙醇交替洗涤数次，沉淀在80 oC烘箱中烘干12 h。将6 mg上述固体粉末、16 mg聚丙烯酸、4 mg氧化锌粉末和12 mL去离子水加入100 mL烧瓶中，超声分散13 min。在磁力搅拌下将40 mL异丙醇缓慢滴加入溶液中，滴加完毕后再向溶液中加入4 mg磷酸二氢氨，在25 oC条件下搅拌反应12h。得到的混合溶液进行离心分离（9000 rpm，9min），所得沉淀在70 oC烘箱中烘干12 h。得到的固体置于管式炉中，在450 oC氩气保护下煅烧5 h，得到梭形Fe3O4@C/Zn3(PO4)2纳米粒子。
Claims (1)
1.一种梭形Fe3O4@C/Zn3(PO4)2纳米粒子的制备方法，其特征是具体步骤如下：
(1)准确称量1 ~ 1.5 g无水三氯化铁、0.02 ~ 0.03 g磷酸二氢钾和400 mL去离子水加入到500 mL圆底烧瓶中，然后将烧瓶置于100 oC油浴中，在磁力搅拌下回流反应70 ~ 80h；
(2)将步骤（1）得到的混合溶液进行离心分离，所得固体再用去离子水和无水乙醇交替洗涤数次，沉淀在50 ~ 100 oC烘箱中烘干8 ~ 10 h，即得干燥梭形Fe2O3纳米粒子；
(3)将4 ~ 6 mg步骤（2）得到的梭形Fe2O3纳米粒子、15 ~ 20 mg聚丙烯酸、3 ~ 6 mg氧化锌粉末和10 ~ 15 mL去离子水加入100 mL烧瓶中，超声分散10 ~ 20 min；
(4)在磁力搅拌下将30 ~ 50 mL异丙醇缓慢滴加入步骤（3）得到的溶液中，滴加完毕后再向溶液中加入3 ~ 6 mg磷酸二氢氨，在25 ~ 30 oC条件下搅拌反应10 ~ 15 h；
(5)将步骤（4）得到的混合溶液进行离心分离7000 ~ 9000 rpm，8 ~ 10 min，所得沉淀在50 ~ 100 oC烘箱中烘干12 ~ 20 h；
(6)将步骤（5）得到的固体置于管式炉中，在350 ~ 450 oC氩气保护下煅烧4 ~ 6 h，得到梭形Fe3O4@C/Zn3(PO4)2纳米粒子。
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| "基于聚丙烯酸为模板的多功能核壳结构纳米粒子的制备及应用研究";高露露;《中国优秀硕士学位论文全文数据库》;20150115;B020-192页 * |
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