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To determine the artificial additives in dairy products, we demonstrate a simple method for rapid and massive determination of melamine in milk liquid and powder samples by surface-enhanced Raman spectroscopy (SERS) technique. The developed method utilizes silver nanoparticles (AgNPs) decorated on a cylindrical support for detecting as low as 5 μL of sample without any drying procedure. Importantly, the linear range for melamine in water was 5–400 parts per billion (ppb) with a low detection limit of 2.5 ppb (S/N = 3). In addition, for analysis of melamine in milk liquid and powder, the dilution method was successfully applied to suppress the matrix effect from real samples. Interestingly, our results indicate that a dilution factor of 75 could effectively reduce the matrix effect with partially sacrificing the sensitivity in detection. The detection limit is increased to 2 parts per million (ppm) in real sample detection, which is close to the acceptable limits regulated in milk products. More importantly, the elimination of complicated sample pre-treatments and the acceptable sensitivity in melamine detection attest our proposed method as a potential tool for rapid and massive food inspections.

Electrochemical methods are combined with shell-isolated nanoparticle-enhanced Raman spectroscopy (EC-SHINERS) for a comprehensive study of pyridine adsorption on Au(111), Au(100) and Au(110) single crystal electrode surfaces. The effects of crystallographic orientation, pyridine concentration, and applied potential are elucidated, and the formation of a second pyridine adlayer on Au(111) is observed spectroscopically for the first time. Electrochemical and SHINERS results correlate extremely well throughout this study, and we demonstrate the potential of EC-SHINERS for thorough characterization of processes occurring on single crystal surfaces. Our method is expected to open up many new possibilities in surface science, electrochemistry and catalysis. Analytical figures of merit are discussed.

A facile photoreduction strategy to attach silver nanoparticles on filter paper (AgNPs@FP) to form surface-enhanced Raman scattering (SERS) substrate array was proposed and examined. As prepared, SERS substrate array was applied to detect low concentration of adenine and other nucleobases in aqueous solutions. In addition, the formed SERS substrate array allows mass analysis of aqueous samples with a requirement of only 10 μL in sample volume. To optimize and understand the parameters in preparations, factors such as the concentrations of citrate and silver nitrate, photoreduction time, and concentration of sodium hydroxide were varied and examined. Para-nitrothiophenol was used as a Raman probe molecule and scanning electron microscope (SEM) images of the substrates were used to explore the influences of experimental factors in the preparation of SERS array. Results indicated that silver ions could be effectively reduced and deposited in/on filter paper with the presence of citrate. The formed AgNPs@FP exhibits a three-dimensional structure as the particles formed on and beneath the surface of the cellulosic fibers could be observed. Deposition of analyte on restricted substrate array rendered reproducible results and the spot-to-spot SERS intensity varied within 8%. At optimal conditions, the substrate enhancement factor approached 107. We demonstrated that the filter paper-based SERS substrates can be used as a suitable tool for biological analysis, and a limit of detection better than 160 nM was obtained in detection of adenine molecules in aqueous solutions with a linear range up to 20 μM. Copyright © 2014 John Wiley & Sons, Ltd.

In this work, a cylindrical-substrate array for surface-enhanced Raman scattering (SERS) measurements was developed to enable analysis of nucleobases in a few microliters of liquid. To eliminate uncertainties associated with SERS detection of aqueous samples, a new type of cylindrical SERS substrate was designed to confine the aqueous sample at the tip of the SERS probe. Poly(methyl methacrylate) (PMMA) optical fibers in a series of different diameters were used as the basic substrate. A solution of poly(vinylidene fluoride)/dimethylformamide (PVDF/DMF) was used to coat the tip of each fiber to increase the surface roughness and facilitate adsorption of silver nanoparticles (AgNPs) for enhancing Raman signals. A chemical reduction method was used to form AgNPs in and on the PVDF coating layer. The reagents and reaction conditions were systematically examined with the aim of estimating the optimum parameters. Unlike the spreading of aqueous sample on most SERS substrates, particularly flat ones, the new SERS substrates showed enough hydrophobicity to restrict aqueous sample to the tip area, thus enabling quantitative analysis. The required volume of sample could be as low as 1 μL with no need for a drying step in the procedure. By aligning the cylindrical SERS substrates into a solid holder, an array of cylindrical substrates was produced for mass analysis of aqueous samples. This new substrate improves both reproducibility and sensitivity for detection in aqueous samples. The enhancement factor approaches 7 orders in magnitude with a relative standard error close to 8%. Using the optimized conditions, nucleobases of adenine, cytosine, thymine, and uracil could be detected with limits approaching a few hundreds nanomolar in only a few microliters of solution.