Vortex-assisted microextraction of melamine from milk samples using green short chain ionic liquid solvents coupled with high performance liquid chromatography determination

Melamine is added illegally to milk and dairy products to increase the amount of apparent protein. This organic nitrogen rich chemical compound has been of great challenge in food safety based on its adverse effect on health. Therefore, the extraction and determination of melamine from milk is necessary. Recently, ionic liquid (ILs) as solvent usage has been noticeable for low melting point, low toxicity, high thermal stability, and high extraction capabilities in a wide range of separation processes. ILs are introduced as organic-inorganic salts and green solvents in microextraction preparation. Therefore, in this study, three ionic liquids ([C6mim][NTF2], [C4mim] [NTF2] and [C2mim][NTF2] ILs) were prepared and employed as an extraction solvent in dispersive liquid--liquid microextraction (DLLME) of melamine from milk samples followed by HPLC-UV. The selected ILs were designed using three types of alkyl-imidazolium (as the short organic cations) and bis (tri fluoro methyl sulfonyl) imide as anion and characterized by ATR-FTIR spectra, carbon, and hydrogen Nuclear Magnetic Resonance spectroscopy (H&C-NMR) and energy-dispersive X-ray spectroscopy (EDX). These techniques confirmed the formation of functional groups, the structure of hydrogen and carbon atoms, and various elements of ionic bond between imidazolium and bis (tri fluoro methyl sulfonyl) imide. In the next step, the effect of significant pa-rameters, including type and volume of ILs, adsorption time, pH of the sample solution, and sample volume, were optimized. Under the optimal conditions, the limits of detection (LOD), limits of quantification (LOQ), and linearity range were obtained 63.64 mu g kg(-1), 210.03 mu g kg(-1), and 210.03-1000 mu g kg(-1), respectively, for as prepared [C6mim][NTF2] as the best ILs. Notably, the achieved LOQ was lower than the maximum residue level (MRL) for the melamine residue in dairy products. Eventually, the proposed method was applied to detect melamine in milk samples, and the relative recoveries were examined as 79.6-105.0 %.

Automated summary

In this study, ionic liquids (ILs) were employed as extraction solvent in the dispersive liquid-liquid microextraction (DLLME) of melamine from milk samples, followed by HPLC-UV analysis. The optimal conditions for the extraction were identified, and the LOD and LOQ were determined to be 63.64 μg/kg and 210.03 μg/kg, respectively. The proposed method was successfully applied to detect melamine in milk samples.