Department of Chemistry, Gandhigram Rural University, Gandhigram 624302, Dindigul, Tamilnadu, India.
Anal Chim Acta. 2010 Mar 24;663(2):158-64. doi: 10.1016/j.aca.2010.01.045. Epub 2010 Feb 1.
We are reporting the highly sensitive determination of hydroxylamine (HA) using 2-mercapto-4-methyl-5-thiazoleacetic acid (TAA) capped fused spherical gold nanoparticles (AuNPs) modified Au electrode. The fused TAA-AuNPs were immobilized on (3-mercaptopropyl)-trimethoxysilane (MPTS) sol-gel film, which was pre-assembled on Au electrode. The immobilization of fused TAA-AuNPs on MPTS sol-gel film was confirmed by UV-vis absorption spectroscopy and atomic force microscopy (AFM). The AFM image showed that the AuNPs retained the fused spherical morphology after immobilized on sol-gel film. The fused TAA-AuNPs on MPTS modified Au electrode were used for the determination of HA in phosphate buffer (PB) solution (pH=7.2). When compared to bare Au electrode, the fused AuNPs modified electrode not only shifted the oxidation potential of HA towards less positive potential but also enhanced its oxidation peak current. Further, the oxidation of HA was highly stable at fused AuNPs modified electrode. Using amperometric method, determination of 17.5 nM HA was achieved for the first time. Further, the current response of HA increases linearly while increasing its concentration from 17.5 nM to 22 mM and a detection limit was found to be 0.39 nM (S/N=3). The present modified electrode was also successfully used for the determination of 17.5 nM HA in the presence of 200-fold excess of common interferents such as urea, NO(2)(-), NH(4)(+), oxalate, Mn(2+), Na(+), K(+), Mg(2+), Ca(2+), Ba(2+) and Cu(2+). The practical application of the present modified electrode was demonstrated by measuring the concentration of HA in ground water samples.
我们报道了使用 2-巯基-4-甲基-5-噻唑乙酸(TAA)封端的融合球形金纳米粒子(AuNPs)修饰金电极对羟胺(HA)进行高灵敏度测定。融合的 TAA-AuNPs 被固定在(3-巯丙基)-三甲氧基硅烷(MPTS)溶胶-凝胶膜上,该溶胶-凝胶膜预先组装在 Au 电极上。通过紫外可见吸收光谱和原子力显微镜(AFM)证实了融合的 TAA-AuNPs 在 MPTS 溶胶-凝胶膜上的固定。AFM 图像显示,AuNPs 在固定在溶胶-凝胶膜上后保留了融合的球形形态。在磷酸盐缓冲液(PB)溶液(pH=7.2)中,将融合的 TAA-AuNPs 固定在 MPTS 修饰的 Au 电极上用于测定 HA。与裸 Au 电极相比,融合的 AuNPs 修饰电极不仅使 HA 的氧化电位向更正的方向移动,而且还增强了其氧化峰电流。此外,在融合的 AuNPs 修饰电极上,HA 的氧化非常稳定。首次使用安培法实现了对 17.5 nM HA 的测定。进一步发现,随着 HA 浓度从 17.5 nM 增加到 22 mM,电流响应呈线性增加,检测限为 0.39 nM(S/N=3)。该修饰电极还成功用于测定存在 200 倍过量常见干扰物如尿素、NO(2)(-)、NH(4)(+)、草酸盐、Mn(2+)、Na(+)、K(+)、Mg(2+)、Ca(2+)、Ba(2+)和 Cu(2+)时的 17.5 nM HA。通过测量地下水样品中 HA 的浓度,证明了本修饰电极的实际应用。