An amperometric detector formed of highly dispersed Ni nanoparticles embedded in a graphite-like carbon film electrode for sugar determination.

We achieved improved detection limits for sugars by developing a novel thin film containing 0.8% highly dispersed Ni nanoparticles in disordered graphite-like carbon (Ni-NDC) as a detection electrode for high-performance liquid chromatography. The Ni-NDC film was prepared in one step by a simple radio frequency (rf) sputtering method at a temperature below 200 degrees C. We characterized the film by XPS, TEM, and AFM analysis and found that the average Ni nanoparticle size was 3 nm and that the film consisted of a mixture of Ni, NiO, Ni2O3, and Ni(OH)2. We studied the electrochemical detection of sugars using the 0.8% Ni-NDC film electrode. The film electrode had excellent electrocatalytic ability and good stability compared with a Ni-bulk electrode with regard to the electrooxidation of sugars. We employed the Ni-NDC film as an HPLC detection electrode. We achieved a good separation of four sugars (glucose, fructose, sucrose, lactose) at a relatively low constant detection potential (0.40 V vs Ag/AgCl) and a linearity of over 3 orders of magnitude. We obtained improved detection limits for the investigated sugars, namely, 20, 25, 50, and 37 nM for glucose, fructose, sucrose, and lactose, respectively. This is at least 1 order of magnitude lower than the detection limits obtained with a Ni-bulk electrode with the same measurement condition. The Ni-NDC film electrode also showed good reproducibility with a relative standard deviation of 1.75% for 40 consecutive injections of glucose in a flow system.