, Volume 403, Issue 7, pp 2009-2017
Date: 04 May 2012

Detection of melamine in milk by surface-enhanced Raman spectroscopy coupled with magnetic and Raman-labeled nanoparticles

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A new method based on surface-enhanced Raman spectroscopy (SERS) has been developed for sensitive and rapid detection of melamine. Spherical magnetic-core gold-shell nanoparticles (AuNPs) and rod-shaped gold nanoparticles (nanorods) labeled with a Raman-active compound were used to form a complex with the melamine molecules. 5,5′-Dithiobis(2-nitrobenzoic acid) was used as Raman-active compound because it is readily adsorbed by a gold nanoparticle surface forming a self-assembled monolayer (SAM) and has strong Raman scattering at 1330 cm−1, because of the symmetric NO2 stretch. The calibration curve was obtained by plotting Raman band area at 1330 cm−1 against melamine concentration. A linear relationship was obtained with a high determination coefficient (R 2 = 0.997). The method was validated for linearity, sensitivity, precision (intra-day and inter-day repeatability), and recovery. In the model system, the limits of detection (LOD) and quantification (LOQ) were 0.38 and 1.27 mg L−1, respectively. For melamine-spiked milk samples, LOD and LOQ values were 0.39 mg L−1 and 1.30 mg L−1, respectively. Intra and inter-day precision were 3.73 and 4.94 %, respectively. This method was applied to samples of skimmed milk that had been spiked with melamine at different concentrations. The recovery of the method was 95–109 % in the concentration range 2–15 mg L−1, and average RSD was 1.71 %. Total analysis time was less than 15 min.

Figure 1

Melamine acts as a cross linker molecule between the magnetic AuNPs and Raman-labeled nanorods