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Development of high-resolution determination methods for nanoparticles

纳米粒子高分辨率测定方法的开发

基本信息

批准号：
20550073
负责人：
TAKEUCHI Toyohide
金额：
$ 3.08万
依托单位：
Gifu University
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (C)
财政年份：
2008
资助国家：
日本
起止时间：
2008 至 2010
项目状态：
已结题

项目摘要

Hydrodynamic chromatography (HDC) conditions have been examined for the separation of silica colloids with 5-78 nm diameters. Conventional HPLC columns with 25 cm×4.6 mm I.D. were prepared and employed for HDC.Interstitial spaces among packing materials are usually employed in HDC. Considering the size of silica colloids, non-porous silica gel with 2-5 μm was packed for the HDC separation of silica colloids. Eluents for HDC of silica colloids were examined in detail, and phosphate buffer solutions with pH larger than 7 gave reasonable elution volumes for silica colloids. A 10 mM phosphate buffer with pH 7.1 was the optimum eluent for silica colloids. The separation column with smaller particle diameter provided better resolution for silica colloids. The silica colloids were detected with a UV detector based on turbidimetry, and the larger colloid gave larger signal intensity.The elution volume of silica colloids slightly increased with decreasing flow rate. It was speculated that lower … More flow rate enhanced the diffusion of analytes into narrower channels.It is required to use smaller particles or to use a longer column in order to improve the resolution. However, higher pressure drop over such separation columns are indispensable, and preparation of such columns is not easy. Since monolithic silica columns having higher permeability and better resolution will overcome these drawbacks, hydrodynamic capillary chromatography (HDCC) was examined for the separation of colloidal particles.Monolithic silica capillary columns with 50-200 μm were prepared and examined for the HDCC separation of colloidal silica and gold nanoparticles with 13-61 nm particle diameters. It was found that smaller elution volumes were observed for larger nanoparticles. In order to minimize the extra-column dispersion, the injection volume was reduced to 20 nL or less, and the on-column detection was carried out. It was expected that the monolithic silica capillary columns possessed mesopore with 10-15 nm and size-exclusion effect could be involved for the elution of smaller nanoparticles. Furthermore, eluents were examined in detail so as not to cause adsorption and coagulation of nanoparticles while passing through the separation column and connecting tubes. It was found that phosphate buffers with pH 7 were good for silica colloids, while aqueous sodium dodecylsulfate solutions were good for gold colloids. Monolithic silica capillary columns with 50 cm in length provided resolution comparable to 25-cm packed columns. It was expected that longer monolithic silica capillary columns would achieve better resolution. Less

已经检查了分离直径为 5-78 nm 的二氧化硅胶体的流体动力色谱 (HDC) 条件。内径 25 cm×4.6 mm 的常规 HPLC 色谱柱制备并用于HDC。填充材料之间的间隙空间通常用于HDC。考虑到二氧化硅胶体的尺寸，填充2-5μm的无孔硅胶用于二氧化硅胶体的HDC分离。对二氧化硅胶体 HDC 的洗脱液进行了详细研究，pH 大于 7 的磷酸盐缓冲溶液为二氧化硅胶体提供了合理的洗脱体积。 pH 7.1 的 10 mM 磷酸盐缓冲液是二氧化硅胶体的最佳洗脱液。粒径较小的分离柱为二氧化硅胶体提供了更好的分离度。采用基于比浊法的紫外检测器对硅胶进行检测，胶体越大，信号强度越大。随着流速的降低，硅胶的洗脱体积略有增加。据推测，较低的流速增强了分析物向较窄通道的扩散。需要使用较小的颗粒或使用较长的色谱柱以提高分辨率。然而，此类分离塔的较高压降是必不可少的，并且此类塔的制备并不容易。由于整体硅胶柱具有更高的渗透性和更好的分辨率将克服这些缺点，因此研究了流体动力毛细管色谱（HDCC）用于胶体颗粒的分离。制备了50-200μm的整体硅胶毛细管柱，并测试了HDCC分离胶体二氧化硅和粒径为13-61nm的金纳米颗粒。发现对于较大的纳米颗粒，观察到较小的洗脱体积。为了尽量减少柱外分散，将进样量减少至20 nL以下，并进行柱上检测。预计整体式硅胶毛细管柱具有10-15 nm的介孔，并且可以参与尺寸排阻效应，以洗脱更小的纳米颗粒。此外，对洗脱液进行了详细检查，以免在通过分离柱和连接管时引起纳米颗粒的吸附和凝聚。研究发现，pH 7 的磷酸盐缓冲液适合二氧化硅胶体，而十二烷基硫酸钠水溶液适合金胶体。长度为 50 cm 的整体硅胶毛细管柱提供的分辨率与 25 cm 填充柱相当。预计较长的整体式硅胶毛细管柱将获得更好的分辨率。较少的