Top Runner Incubation Center for Academic-Industry Fusion, Nagaoka University of Technology, 1603-1 Kamitomioka, Nagaoka, Niigata 940-2188, Japan.
Anal Chim Acta. 2011 Mar 9;689(1):103-9. doi: 10.1016/j.aca.2011.01.032. Epub 2011 Jan 25.
A new detection membrane for filtration enrichment combined with colorimetric determination of Cd(II), Zn(II), Pb(II) and Cu(II) ions is presented. We have demonstrated the use of a dye nanoparticle coated test strip (DNTS) structured with a reagent layer for on-site analysis of trace metal ions. In this study, a [TMPyP/SA] DNTS coated with a nanocomposite layer (average thickness: 5.39 μm) of α,β,γ,δ-Tetrakis(1-methylpyridinium-4-yl)porphine (TMPyP) and silica-SA on the top surface of a cellulose ester membrane filter was fabricated by a simple filtration of an aqueous TMPyP/silica-SA nanocomposite dispersion through a membrane filter. The nanocomposite formation of cationic TMPyP and negatively charged colloidal SA (9-80 nm) was based on electrostatic interaction and was confirmed in the 120-800 nm diameter range by a dynamic light scattering photometer (DLS). To optimize the DNTS nanocomposite layer, surface uniformity, mechanical strength, the percent retention of TMPyP, and sensitivity to Cd(II) detection for six DNTSs with five different types of silica were examined. A half[TMPyP/SA] DNTS with an average layer thickness of 2.60 μm, which was prepared by controlling the amount of TMPyP and SA, demonstrated the highest sensitivity to Cd(II) ion because it had the lowest background absorbance. In addition, factors that affected the percent retention of TMPyP, such as pH and TMPyP/SA ratio, were determined. More than 99% of the TMPyP was retained on a membrane filter at pH 7.8 with a TMPyP and SA concentration of 2 × 10(-5) M and 4 × 10(-5) wt%, respectively. Filtration enrichment of 100mL of an aqueous solution containing Cd(II), Zn(II), and Pb(II) at ppb levels was achieved by concentrating the metal ions in a nanocomposite layer (the effective TMPyP area was 1.77 cm(2), pH 10.2). The signaling surface changed from a brown color to green when the ions were captured. The percent extraction for metal ions on a half[TMPyP/SA] DNTS were estimated by TLC scanning and ICP-MS. It was observed that, when using the half[TMPyP/SA] DNTS, Cd(II) concentrations as low as 1 ppb were detectable at a filtration rate of 4.0-5.0 mL min(-1).
一种用于过滤富集的新型检测膜,结合比色法测定 Cd(II)、Zn(II)、Pb(II) 和 Cu(II) 离子,本文提出。我们已经证明了一种染料纳米粒子涂覆的测试带(DNTS)在现场分析痕量金属离子中的用途,该测试带结构带有试剂层。在这项研究中,通过将带正电荷的 TMPyP 和带负电荷的胶体 SA(9-80nm)的纳米复合材料层(平均厚度:5.39μm)过滤到纤维素酯膜过滤器的顶部表面上,制备了涂覆有[TMPyP/SA]DNTS 的纳米复合材料层。纳米复合材料的形成基于静电相互作用,通过动态光散射光度计(DLS)在 120-800nm 直径范围内得到证实。为了优化 DNTS 纳米复合材料层,我们研究了具有五种不同类型二氧化硅的六种 DNTS 的表面均匀性、机械强度、TMPyP 的保留率和对 Cd(II)检测的灵敏度。通过控制 TMPyP 和 SA 的量,制备了具有平均层厚 2.60μm 的半[TMPyP/SA]DNTS,对 Cd(II)离子具有最高的灵敏度,因为它具有最低的背景吸光度。此外,还确定了影响 TMPyP 保留率的因素,例如 pH 值和 TMPyP/SA 比值。在 pH 值为 7.8 时,TMPyP 和 SA 的浓度分别为 2×10(-5)M 和 4×10(-5)wt%时,超过 99%的 TMPyP 保留在膜过滤器上。通过在纳米复合材料层中浓缩金属离子(有效 TMPyP 面积为 1.77cm(2),pH 值为 10.2),实现了在 ppb 水平下过滤富集 100ml 含 Cd(II)、Zn(II)和 Pb(II)的水溶液。当离子被捕获时,信号表面从棕色变为绿色。通过 TLC 扫描和 ICP-MS 估算了金属离子在半[TMPyP/SA]DNTS 上的萃取率。观察到,当使用半[TMPyP/SA]DNTS 时,Cd(II)浓度低至 1ppb 时,在 4.0-5.0mLmin(-1)的过滤速度下即可检测到。