Abstract:

A method for the simultaneous determination of 18 pesticide residues in red wine was developed using ultra high performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS) with isotope dilution technique. The red wine samples were extracted with acetonitrile, and the extracts were cleaned up with dispersive solid phase extraction (d-SPE) using the mixture of N-propyl ethylene diamine (PSA) and C18 powder as sorbent. The extracted components were separated on a BEH C₁₈ column by gradient elution. The qualitative and quantitative analyses were operated under full scan/data dependent MS/MS (ddms²) and targeted selective ion monitoring (tSIM) by high resolution mass spectrometry, respectively. Carbendazim-D₄, chlorpyrifos-D₁₀, imidacloprid-D₄, methoxyfenozide-D₉, pyrimethanil-D₅ and tebuconazole-D₆ were used as the internal standards to reduce the matrix effects. The response of each pesticide showed a good linearity in the range of 0.5-50 μg/kg with the correlation coefficient more than 0.999. The limits of detection and quantification for the 18 pesticides in the spiked blank red wine were 0.5 μg/kg and 1.0 μg/kg, respectively. The recovery results with spiked blank red wine samples at the levels of 1 to 40 μg/kg were satisfactory with average recoveries of 85.4%-117.9% and the RSDs of 0.5%-6.1%. The method was applied for the determination of the red wine real samples from the market. Carbendazim, imidacloprid, pyrimethanil, tebuconazole and triadimenol were detected in the samples. The results show that the method is suitable for the rapid screening and quantitative analysis of pesticide residues in red wine.

Key words: dispersive solid phase extraction (d-SPE), high resolution mass spectrometry (HRMS), isotope dilution, pesticide residues, ultra high performance liquid chromatography (UPLC), wine