Dispersive liquid-liquid microextraction using non-chlorinated, lighter than water solvents for gas chromatography mass spectrometry determination of fungicides in wine

作者：Rodriguez Cabo T; Rodriguez I^*; Ramil M; Cela R

来源：Journal of Chromatography A, 2011, 1218(38): 6603-6611.

DOI：10.1016/j.chroma.2011.07.054

• Dispersive liquid-liquid microextraction
• Non-chlorinated extractant
• Fungicides
• Wine analysis
• Gas chromatography-mass spectrometry

A novel and low solvent consumption method for the sensitive determination of fungicide residues in wine samples is proposed. Analytes were extracted by dispersive liquid-liquid microextraction (DLLME) and further determined by gas chromatography-mass spectrometry (GC-MS). Under optimized conditions, a binary mixture of acetone and 1-undecanol (0.5 and 0.05 mL, respectively) was used to extract target compounds from diluted (1:1) wine samples. After centrifugation, the floating phase of 1-undecanol was solidified and separated from the liquid hydro-alcoholic matrix. Thereafter, it was allowed to melt at room temperature and injected in the GC-MS system. The method showed relative standard deviations (RSDs, %) below 13%, limits of quantification (LOQs) between 0.2 and 3.2 ng mL(-1) and linear responses for concentrations up to 300 ng mL(-1). The efficiency of the liquid-phase microextraction process was scarcely affected by the characteristics of wine samples, consequently pseudo-external standard calibration (using matrix matched standards of red and white wine) sufficed to achieve acceptable accuracy values: relative recoveries from 81 to 120%. The applicability of the method was demonstrated with commercial wine samples.

• 出版日期2011-9-23