Novel multiresidue method for determination of pesticides in red wine using gas chromatography–mass spectrometry and solid phase extraction

• New GC–MS multiresidue method for detection of 25 pesticides in red wine.
• New in SPE: methanol and water reduces anthocyanins interference.
• Method is fast with high recoveries and good precision.
• Applicable for most popular pesticides in grape/wine application.
• In 32 wine samples 7 pesticides were present at high concentrations.

A new multiresidue method was developed for determination of 25 pesticide residues in red wine by gas chromatography coupled to mass spectrometry with a single run of 23.63 min. Samples were extracted from wine with solid phase extraction using Oasis HLB. Mixture of methanol and water was used for rinsing, while acetonitrile and n-hexane were used as elution solvents. Method was validated according to SANCO/12571/2013 criteria in wide linearity range (limit of quantification – 400 μg L−1). Limits of quantification (LOQ) were well below 10 μg L−1 for most pesticides and recoveries at 2 × LOQ and 10 × LOQ concentration levels were in range 70–120%. Precision, expressed as a relative standard deviation, was always under 14%. The method was applied to 32 red wine samples from Croatia. Pesticides were detected in 30 samples with a total of 15 pesticides found, 7 of which were at a high concentration.