A simple, fast, reproducible and efficient one-step fabrication method was successfully developed to prepare gold nanoparticle/carbon nanosheet (Au NP/CNS) hybrids by using sonoelectrochemistry. This method involved simultaneous generation of carbon nanosheets (CNSs) by oxidation of a graphite anode and generation of Au NPs by reduction of AuCl4(-) on the surface of the cathode. Then the Au NPs modified with poly(diallyl dimethyl ammonium chloride) were self-assembled on the surface of the CNS. A homemade sonoelectrochemical device that provided both high-intensity electric and ultrasonic fields was applied. The ability to obtain Au NPs with a controlled size and distribution on the surface of the CNS benefitted from the synergistic effect of the electric field and ultrasonic field. The Au NPs on the CNS surface exhibited distinctive and high-quality SERS activity. The enhancement factor of the developed substrate was 1.2 × 10(6) using 4-aminothiophenol as the probe molecule. The Au NP/CNS hybrid showed a great increase of Raman signals for aromatic molecules because of the high affinity of the CNS for aromatic molecules and the SERS activity of Au NPs. This SERS substrate also showed charge selectivity for cationic aromatic dyes, due to the negative charge on the surface of the CNS. Subsequently, the potential practical application of the SERS substrate was evaluated by quantitative analysis of adenine. The results suggest that Au NP/CNS materials as sensitive SERS-active substrates have great potential for detection of biomolecules.
The surface-enhanced Raman spectroscopy (SERS) technique is of great importance for insight into the transient reaction intermediates and mechanistic pathways involved in heterogeneously catalyzed chemical reactions under actual reaction conditions, especially in water. Herein, we demonstrate a facile method for in situ synthesis of nanocrystalline magnesium oxide-Ag(0) (nano MgO-Ag(0)) hybrid nanomaterials with dispersed Ag nanoparticles (Ag NPs) on the surface of nanocrystalline magnesium oxide (nano MgO) via Sn(2+) linkage and reduction. As a benefit from the synergy effect of nano MgO and Ag NPs, the nano MgO-Ag(0) exhibited both excellent SERS and catalytic activities for the reduction of 4-nitrothiophenol in the presence of NaBH4. The nano MgO-Ag(0) was used for real-time monitoring of the catalytic reaction process of 4-nitrothiophenol to 4-aminothiophenol in an aqueous medium by observing the SERS signals of the reactant, intermediate and final products. The intrinsic reaction kinetics and reaction mechanism of this reaction were also investigated. This SERS-based synergy technique provides a novel approach for quantitative in situ monitoring of catalytic chemical reaction processes.
Microextraction techniques can extract efficiently the analytes from a sample matrix to the polymers or organic solvents of microvolume, and integrate sampling, extraction, concentration and injection into one single step. They have the advantages of simple, time-efficient and solvent-free. They have been successfully coupled with a variety of analytical tools, such as gas chromatography and high performance liquid chromatography. Molecularly imprinted polymers have specific recognition ability. They can separate and enrich analytes from complicated matrix with high selectivity, and they have great application prospects in complicated sample preparation. This review summarizes the progress in the molecularly imprinted microextraction techniques, including molecularly imprinted-solid phase microextraction, molecularly imprinted-stir bar adsorptive extraction, magnetic molecularly imprinted beads extraction, etc. A total of 75 references are cited.
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