Multiresidue Method for the Determination of Organophosphorus Pesticides in Still Wine and Fortified Wine Using Solid-Phase Microextraction and Gas Chromatography – Tandem Mass Spectrometry

Abstract

A SPME-GC-MS/MS method for the determination of eight organophosphorus pesticides (azinphos-methyl, chlorpyriphos, chlorpyriphos-methyl, diazinon, fenitrothion, fenthion, malathion, and methidathion) in still and fortified wine was developed. The extraction procedure is simple, solvent free, and without any sample pretreatment. Limits of detection (LOD) and quantitation (LOQ) values in the range 0.1–14.3 µg/L and 0.2–43.3 µg/L, respectively, were obtained. The LOQ values are below the maximum residue levels (MRLs) established by European Regulation for grapes, with the exception of methidathion. Coefficients of correlation (R²) higher than 0.99 were obtained for the majority of the pesticides, in all different wines analyzed.

Keywords:

• Fortified wine
• GC-MS/MS
• Organophosphorus pesticides
• SPME
• Still wine

Notes

*Quantifier ions.

*Recovery values for spiked wine blend samples (azinphos-methyl 19.9 µg/L, chlorpyriphos 7.9 µg/L, chlorpyriphos-methyl 0.4 µg/L, diazinon 2.0 µg/L, fenitrothion 1.99 µg/L, fenthion 1.00 µg/L, malathion 9.9 µg/L, methidathion 49.5 µg/L).

*The spiking levels used in the recovery study are described in Table 4.