磁性核壳Ag/PDA@SiO2@CoFe2O4复合纳米材料的制备、表征及其抑菌性能研究

doi:10.15541/jim20160427

摘要/Abstract

摘要：

采用溶剂热法制备单分散的CoFe₂O₄亚微米球, 分别用正硅酸乙酯(TEOS)和多巴胺(DA)为前体通过溶胶-凝胶法和自聚合法对CoFe₂O₄核表面进行修饰形成具有多层核壳结构的PDA@SiO₂@CoFe₂O₄, 最外层为聚多巴胺(PDA)。采用原位还原法在PDA表面沉积均匀的银纳米粒子, 合成Ag/PDA@SiO₂@CoFe₂O₄磁性复合粒子。采用透射电子显微镜(TEM)、X射线粉末衍射(XRD)、X射线光电子能谱分析(XPS)、振动探针式磁强计(VSM)和电感耦合等离子发射光谱仪(ICP-OES)对样品的形貌、结构等进行表征, 并研究其对大肠杆菌(E.Coli)和金黄色葡萄球菌(S.Aureas)的抑菌性能。结果表明, 当Ag浓度在0.6 mg/mL时, Ag/PDA@SiO₂@CoFe₂O₄对E.Coli和S.Aureas的抑菌率均在92%以上。除了优异的抑菌性能, 它具有很强的磁性, 可以通过外加磁场回收利用。

关键词: 磁性, 聚多巴胺, 纳米复合材料, 抑菌性能

Abstract:

Monodisperse submicron CoFe₂O₄ spheres were prepared by solvothermal method. Polydopamine-coated silica@CoFe₂O₄ composite particles were synthesized by combination of Sol-Gel process and in situ self-polymerization method, in which tetraethyl orthosilicate (TEOS) and dopamine were used as the precursor for silica and polydopamine (PDA), respectively. The PDA@SiO₂@CoFe₂O₄ composites had a multilayer core-shell structure with PDA as the outermost layer shell. Then, numerous of silver nanoparticles were assembled on the surface of PDA@SiO₂@CoFe₂O₄ via the reduction of Ag⁺ by the surface PDA on the composites. The morphology, structure, and composition of the composites were characterized by transmission electron microscope (TEM), X-ray powder diffraction (XRD), X-ray photoelectron spectrometry (XPS), vibrating sample magnetometry (VSM), and inductively coupled plasma optical emission spectrometry (ICP-OES). Antibacterial experiments indicated that the as-prepared composites could restrict up to 92% Escherichia Coli (E.Coli) and Staphylococcus Aureus (S.Aureas) at 0.6 mg/mL Ag. In addition, the composites showed a strong magnetic response to an externally applied magnetic field, so it could be reused.

Key words: magnetic, polydopamine, nanocomposites, antibacterial activity

中图分类号:

O649

廖凡, 马剑琪, 葛红光. 磁性核壳Ag/PDA@SiO₂@CoFe₂O₄复合纳米材料的制备、表征及其抑菌性能研究[J]. 无机材料学报, 2017, 32(5): 523-528.

LIAO Fan, MA Jian-Qi, GE Hong-Guang. Preparation, Characterization and Antimicrobial Activity of Core-satellite Ag/PDA@SiO₂@CoFe₂O₄ Magnetic Composites[J]. Journal of Inorganic Materials, 2017, 32(5): 523-528.

图/表 7

图1 CoFe2O4(a, b), SiO2@CoFe2O4(c, d), PDA@SiO2@CoFe2O4(e,f)和Ag/PDA@SiO2@CoFe2O4(g, h)样品的透射电镜照片

Fig. 1 TEM images of magnetic nanoparticles (a, b), silica-coated magnetic nanoparticles (c, d), polydopamine coated SiO2@CoFe2O4 (e, f) and Ag/PDA@SiO2@CoFe2O4 (g, h) NPs

图2 CoFe2O4(a)、PDA@SiO2@CoFe2O4(b)和Ag/PDA@SiO2@CoFe2O4(c)样品的XRD图谱

Fig. 2 XRD patterns of CoFe2O4 (a), PDA@SiO2@CoFe2O4(b) and Ag/PDA@SiO2@CoFe2O4(c) particles

图3 Ag/PDA@SiO2@CoFe2O4样品的XPS图谱

Fig. 3 XPS spectra of the Ag/PDA@SiO2@CoFe2O4 NPs

图4 CoFe2O4、PDA@SiO2@CoFe2O4和Ag/PDA@SiO2@CoFe2O4样品的饱和磁化强度

Fig. 4 Hysteresis loops of the magnetic CoFe2O4 core, PDA@SiO2@CoFe2O4 and Ag/PDA@SiO2@CoFe2O4 NPs

图5 无菌水、PDA@SiO2@CoFe2O4、Ag/PDA@SiO2@CoFe2O4 和商品 Ag滤纸片扩散抑菌图

Fig. 5 Inhibition zones of Sterile water, PDA@SiO2@CoFe2O4, Ag/PDA@SiO2@CoFe2O4 and Ag NPs against (a) E.Coli and (b) B.Subtilis (a1-a4, b1-b4 samples containing Ag at concentrations of 0.2, 0.4, 0.6, and 0.8 mg /mL)

表1 Ag/PDA@SiO2@CoFe2O4和商品Ag抑菌圈尺寸

Table 1 Inhibition zone diameters of the Ag/PDA@SiO2@CoFe2O4 and Ag NPs against E.coli and S.aureas (Diffusion (cm) = final inhibition zonediameter(cm)-initial diameter(cm)

Concentration/(mg·mL^-1)	E.coli Inhibition zones/cm		B.subtilis Inhibition zones/cm
Concentration/(mg·mL^-1)	B	C	B	C
0.2	0.5	0.3	0.2	0.1
0.4	0.7	0.5	0.4	0.2
0.6	0.8	0.6	0.8	0.5
0.8	1.0	0.8	1.1	0.7

图6 无菌水、Ag/PDA@SiO2@CoFe2O4和商品Ag菌落计数法抑菌图

Fig. 6 Images of colonies on MH agar plates cultured of E.Coli and B.Subtilis

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磁性核壳Ag/PDA@SiO₂@CoFe₂O₄复合纳米材料的制备、表征及其抑菌性能研究

Preparation, Characterization and Antimicrobial Activity of Core-satellite Ag/PDA@SiO₂@CoFe₂O₄ Magnetic Composites

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